Ink comprising encapsulated nanoparticles, method for depositing the ink, and a pattern, particle and optoelectronic device comprising the ink
10822510 ยท 2020-11-03
Assignee
Inventors
- Marc Pousthomis (Deuil-la-Barre, FR)
- Michele D'AMICO (Romainville, FR)
- Alexis Kuntzmann (Paris, FR)
- Yu-Pu Lin (Versailles, FR)
- Edgar Cao (Paris, FR)
- Robin FAIDEAU (Houilles, FR)
Cpc classification
B82Y40/00
PERFORMING OPERATIONS; TRANSPORTING
C01G11/006
CHEMISTRY; METALLURGY
C01B33/12
CHEMISTRY; METALLURGY
C09K11/025
CHEMISTRY; METALLURGY
C09D11/50
CHEMISTRY; METALLURGY
B82Y20/00
PERFORMING OPERATIONS; TRANSPORTING
C01P2004/80
CHEMISTRY; METALLURGY
C01F7/30
CHEMISTRY; METALLURGY
B01J13/18
PERFORMING OPERATIONS; TRANSPORTING
B01J2/02
PERFORMING OPERATIONS; TRANSPORTING
C01P2004/24
CHEMISTRY; METALLURGY
International classification
H01L33/00
ELECTRICITY
B01J13/18
PERFORMING OPERATIONS; TRANSPORTING
C09K11/88
CHEMISTRY; METALLURGY
C09D11/50
CHEMISTRY; METALLURGY
C09K11/02
CHEMISTRY; METALLURGY
C01F7/30
CHEMISTRY; METALLURGY
Abstract
Disclosed is an ink including at least one particle including a first material; and at least one liquid vehicle; wherein the particle includes at least one particle including a second material and at least one nanoparticle dispersed in the second material; wherein the first material and the second material have an extinction coefficient less or equal to 1510.sup.5 at 460 nm. The invention also relates to inks, light emitting materials including at least one ink, patterns including at least one ink, particles deposited on a support, optoelectronic devices including at least one ink and method for depositing an ink on a support.
Claims
1. An ink comprising: (i) at least one first particle comprising a first material and at least one liquid vehicle; wherein the at least one first particle comprises at least one second particle comprising a second material and at least one nanoparticle dispersed in said second material; wherein the at least one nanoparticle is a luminescent nanoparticle and comprises at least 1% of semiconductor nanoplatelets; wherein the first material and the second material have an extinction coefficient less than or equal to 1510.sup.5 at 460 nm; or (ii) at least one particle comprising a plurality of nanoparticles encapsulated in a material and at least one liquid vehicle; wherein said particle has a surface roughness less than or equal to 5% of the largest dimension of said particle; wherein the at least one nanoparticle is a luminescent nanoparticle and comprises at least 1% of semiconductor nanoplatelets; or (iii) at least one first particle comprising a first material and at least one liquid vehicle; wherein the at least one first particle comprises at least one second particle comprising a second material and at least one nanoparticle dispersed in said second material; wherein said at least one first particle has a surface roughness less than or equal to 5% of the largest dimension of said at least one first particle; and wherein the at least one nanoparticle is a luminescent nanoparticle and comprises at least 1% of semiconductor nanoplatelets.
2. The ink according to claim 1, wherein the first material limits or prevents the diffusion of outer molecular species or fluids into said first material.
3. The ink according to claim 1, wherein the first material has a density ranging from 1 to 10.
4. The ink according to claim 1, wherein the first material has a density greater than or equal to that of the second material.
5. The ink according to claim 1, wherein the first material has a thermal conductivity at standard conditions of at least 0.1 W/(m.Math.K).
6. The ink according to claim 1, wherein the at least one nanoparticle is a semiconductor nanocrystal.
7. The ink according to claim 1, wherein the at least one nanoparticle is a semiconductor nanocrystal comprising a core comprising a material of formula MxNyEzAw, wherein: M is selected from the group consisting of Zn, Cd, Hg, Cu, Ag, Au, Ni, Pd, Pt, Co, Fe, Ru, Os, Mn, Tc, Re, Cr, Mo, W, V, Nd, Ta, Ti, Zr, Hf, Be, Mg, Ca, Sr, Ba, Al, Ga, In, Tl, Si, Ge, Sn, Pb, As, Sb, Bi, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Cs and mixtures thereof; N is selected from the group consisting of Zn, Cd, Hg, Cu, Ag, Au, Ni, Pd, Pt, Co, Fe, Ru, Os, Mn, Tc, Re, Cr, Mo, W, V, Nd, Ta, Ti, Zr, Hf, Be, Mg, Ca, Sr, Ba, Al, Ga, In, Tl, Si, Ge, Sn, Pb, As, Sb, Bi, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Cs and mixtures thereof; E is selected from the group consisting of O, S, Se, Te, C, N, P, As, Sb, F, Cl, Br, I, and mixtures thereof; A is selected from the group consisting of O, S, Se, Te, C, N, P, As, Sb, F, Cl, Br, I, and mixtures thereof; and x, y, z and w are each independently a decimal number from 0 to 5; x, y, z and w are not simultaneously equal to 0; x and y are not simultaneously equal to 0; z and w may not be simultaneously equal to 0.
8. The ink according to claim 1, wherein the at least one nanoparticle is a semiconductor nanocrystal comprising at least one shell comprising a material of formula MxNyEzAw, wherein: M is selected from the group consisting of Zn, Cd, Hg, Cu, Ag, Au, Ni, Pd, Pt, Co, Fe, Ru, Os, Mn, Tc, Re, Cr, Mo, W, V, Nd, Ta, Ti, Zr, Hf, Be, Mg, Ca, Sr, Ba, Al, Ga, In, Tl, Si, Ge, Sn, Pb, As, Sb, Bi, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Cs or a mixture thereof; N is selected from the group consisting of Zn, Cd, Hg, Cu, Ag, Au, Ni, Pd, Pt, Co, Fe, Ru, Os, Mn, Tc, Re, Cr, Mo, W, V, Nd, Ta, Ti, Zr, Hf, Be, Mg, Ca, Sr, Ba, Al, Ga, In, Tl, Si, Ge, Sn, Pb, As, Sb, Bi, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Cs and mixtures thereof; E is selected from the group consisting of O, S, Se, Te, C, N, P, As, Sb, F, Cl, Br, I, and mixtures thereof; A is selected from the group consisting of O, S, Se, Te, C, N, P, As, Sb, F, Cl, Br, I, and mixtures thereof; and x, y, z and w are each independently a decimal number from 0 to 5; x, y, z and w are not simultaneously equal to 0; x and y are not simultaneously equal to 0; z and w may not be simultaneously equal to 0.
9. The ink according to claim 1, wherein the at least one nanoparticle is a semiconductor nanocrystal comprising at least one crown comprising a material of formula MxNyEzAw, wherein: M is selected from the group consisting of Zn, Cd, Hg, Cu, Ag, Au, Ni, Pd, Pt, Co, Fe, Ru, Os, Mn, Tc, Re, Cr, Mo, W, V, Nd, Ta, Ti, Zr, Hf, Be, Mg, Ca, Sr, Ba, Al, Ga, In, Tl, Si, Ge, Sn, Pb, As, Sb, Bi, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Cs or a mixture thereof; N is selected from the group consisting of Zn, Cd, Hg, Cu, Ag, Au, Ni, Pd, Pt, Co, Fe, Ru, Os, Mn, Tc, Re, Cr, Mo, W, V, Nd, Ta, Ti, Zr, Hf, Be, Mg, Ca, Sr, Ba, Al, Ga, In, Tl, Si, Ge, Sn, Pb, As, Sb, Bi, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Cs and mixtures thereof; E is selected from the group consisting of O, S, Se, Te, C, N, P, As, Sb, F, Cl, Br, I, and mixtures thereof; A is selected from the group consisting of O, S, Se, Te, C, N, P, As, Sb, F, Cl, Br, I, and mixtures thereof; and x, y, z and w are each independently a decimal number from 0 to 5; x, y, z and w are not simultaneously equal to 0; x and y are not simultaneously equal to 0; z and w may not be simultaneously equal to 0.
10. The ink according to claim 1, wherein the at least one nanoparticle is a semiconductor nanoplatelet.
11. The ink according to claim 1, wherein the at least one liquid vehicle comprises 1-methoxy-2-propanol, 2-pyrrolidinone, C4 to C8 1,2-alkanediol, aliphatic or alicycle ketone, methyl ethyl ketone, C1-C4 alkanol, ketones, esters, ether of ethylene glycol or propylene glycol, acetals, acrylic resin, polyvinyl acetate, polyvinyl alcohol, polyamide resin, polyurethane resin, epoxy resin, alkyd ester, nitrated cellulose, ethyl cellulose, sodium carboxymethyl cellulose, alkyds, maleics, cellulose derivatives, formaldehyde, rubber resin, phenolics, propyl acetate, glycol ether, aliphatic hydrocarbon, acetate, ester, acrylic, cellulose ester, nitrocellulose, modified resin, alkoxylated alcohol, 2-pyrrolidone, a homolog of 2-pyrrolidone, glycol, water, or a mixture thereof.
12. A pattern comprising at least one ink according to claim 1 deposited by inkjet printing on a support.
13. A pattern comprising at least one ink according to claim 1 deposited by inkjet printing on a LED chip or microsized LED.
14. A particle deposited on a support by inkjet printing, wherein the deposited particle comprises: (i) a first material and at least one second particle comprising a second material and at least one nanoparticle dispersed in said second material; wherein the first material and the second material have an extinction coefficient less than or equal to 1510.sup.5 at 460 nm; wherein the at least one nanoparticle is a luminescent nanoparticle and comprises at least 1% of semiconductor nanoplatelets; or (ii) a first material and at least one second particle comprising a second material and at least one nanoparticle dispersed in said second material; wherein said deposited particle has a surface roughness less than or equal to 5% of the largest dimension of said deposited particle; and wherein the at least one nanoparticle is a luminescent nanoparticle and comprises at least 1% of semiconductor nanoplatelets.
15. A particle deposited on a support by inkjet printing; wherein said particle comprises a plurality of nanoparticles encapsulated in a material; wherein said particle has a surface roughness less than or equal to 5% of the largest dimension of said particle; and wherein the at least one nanoparticle is a luminescent nanoparticle and comprises at least 1% of semiconductor nanoplatelets.
16. An optoelectronic device comprising at least one ink according to claim 1.
17. A method for depositing an ink according to claim 1 on a support comprising: printing the ink on a support using inkjet printing; and evaporating the liquid vehicle.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
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EXAMPLES
(48) The present invention is further illustrated by the following examples.
Example 1: Inorganic Nanoparticles Preparation
(49) Nanoparticles used in the examples herein were prepared according to methods of the art (Lhuillier E. et al., Acc. Chem. Res., 2015, 48 (1), pp 22-30; Pedetti S. et al., J. Am. Chem. Soc., 2014, 136 (46), pp 16430-16438; Ithurria S. et al., J. Am. Chem. Soc., 2008, 130, 16504-16505; Nasilowski M. et al., Chem. Rev. 2016, 116, 10934-10982).
(50) Nanoparticles used in the examples herein were selected in the group comprising CdSe/CdZnS, CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots.
Example 2: Particles Preparation from a Basic Aqueous SolutionCdSe/CdZnS@SiO.SUB.2
(51) 100 L of CdSe/CdZnS nanoplatelets suspended in a basic aqueous solution were mixed with a basic aqueous solution of TEOS at 0.13M previously hydrolyzed for 24 hours, then loaded on a spray-drying set-up. The liquid mixture was sprayed towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The particles were collected at the surface of a filter.
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(54) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(55) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
Example 3: Particles Preparation from an Acidic Aqueous SolutionCdSe/CdZnS@SiO.SUB.2
(56) 100 L of CdSe/CdZnS nanoplatelets suspended in an acidic aqueous solution were mixed with an acidic aqueous solution of TEOS at 0.13M previously hydrolyzed for 24 hours, then loaded on a spray-drying set-up. The liquid mixture was sprayed towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The particles were collected at the surface of a filter.
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(58) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(59) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
Example 4: Particles Preparation from a Basic Aqueous Solution with Hetero-ElementsCdSe/CdZnS@Si.SUB.x.Cd.SUB.y.Zn.SUB.z.O.SUB.w
(60) 100 L of CdSe/CdZnS nanoplatelets suspended in an acidic aqueous solution were mixed with an acidic aqueous solution of TEOS at 0.13M previously hydrolyzed for 24 hours in presence of cadmium acetate at 0.01M and zinc oxide at 0.01M, then loaded on a spray-drying set-up. The liquid mixture was sprayed towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The particles were collected at the surface of a filter.
(61) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(62) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
Example 5: Particles Preparation from an Organic Solution and an Aqueous SolutionCdSe/CdZnS@Al.SUB.2.O.SUB.3
(63) 100 L of CdSe/CdZnS nanoplatelets suspended in heptane were mixed with aluminium tri-sec butoxide and 5 mL of pentane, then loaded on a spray-drying set-up. On another side, a basic aqueous solution was prepared and loaded the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The particles were collected at the surface of a filter.
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(66) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(67) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(68) The same procedure was carried out by replacing Al.sub.2O.sub.3 with ZnTe, SiO.sub.2, TiO.sub.2, HfO.sub.2, ZnSe, ZnO, ZnS or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(69) The same procedure was carried out by replacing Al.sub.2O.sub.3 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 6: Particles Preparation from an Organic Solution and an Aqueous SolutionInP/ZnS@Al.SUB.2.O.SUB.3
(70) 4 mL of InP/ZnS nanoparticles suspended in heptane were mixed with aluminium tri-sec butoxide and 400 mL of heptane, then loaded in a spray-drying set-up. On another side, an acidic aqueous solution was prepared and loaded in the same spray-drying set-up, but at a different location than the first hexane solution. The two liquids were sprayed simultaneously with two different means for forming droplets towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The particles were collected at the surface of a filter.
(71) The same procedure was carried out by replacing InP/ZnS nanoparticles with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(72) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(73) The same procedure was carried out by replacing Al.sub.2O.sub.3 with SiO.sub.2, TiO.sub.2, HfO.sub.2, ZnTe, ZnSe, ZnO, ZnS or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(74) The same procedure was carried out by replacing Al.sub.2O.sub.3 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 7: Particles Preparation from an Organic Solution and an Aqueous SolutionCH.SUB.5.N.SUB.2.PbBr.SUB.3.@Al.SUB.2.O.SUB.3
(75) 100 L of CH.sub.5N.sub.2PbBr.sub.3 nanoparticles suspended in hexane were mixed with aluminium tri-sec butoxide and 5 mL of hexane, then loaded in a spray-drying set-up. On another side, an acidic aqueous solution was prepared and loaded in the same spray-drying set-up, but at a different location than the first hexane solution. The two liquids were sprayed simultaneously with two different means for forming droplets towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The particles were collected at the surface of a filter.
(76) The same procedure was carried out by replacing Al.sub.2O.sub.3 with SiO.sub.2, TiO.sub.2, HfO.sub.2, ZnTe, ZnSe, ZnO, ZnS or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(77) The same procedure was carried out by replacing Al.sub.2O.sub.3 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 8: Particles Preparation from an Organic Solution and an Aqueous SolutionCdSe/CdZnSAu@SiO.SUB.2
(78) On one side, 100 L of gold nanoparticles and 100 L of CdSe/CdZnS nanoplatelets suspended in an acidic aqueous solution were mixed with an acidic aqueous solution of TEOS at 0.13M previously hydrolyzed for 24 hours, then loaded in a spray-drying set-up. The suspension was sprayed towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The particles were collected at the surface of a GaN substrate. The GaN substrate with the deposited particles was then cut into pieces of 1 mm1 mm and electrically connected to get a LED emitting a mixture of the blue light and the light emitted by the fluorescent nanoparticles.
(79) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(80) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(81) The same procedure was carried out by replacing SiO.sub.2 with Al.sub.2O.sub.3, TiO.sub.2, HfO.sub.2, ZnTe, ZnSe, ZnO, ZnS or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(82) The same procedure was carried out by replacing SiO.sub.2 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 9: Particles Preparation from an Organic Solution and an Aqueous SolutionFe.SUB.3.O.SUB.4.@Al.SUB.2.O.SUB.3.CdSe/CdZnS@SiO.SUB.2
(83) On one side, 100 L of Fe.sub.3O.sub.4 nanoparticles suspended in an acidic aqueous solution were mixed with an acidic aqueous solution of TEOS at 0.13M previously hydrolyzed for 24 hours. On another side, 100 L of CdSe/CdZnS nanoplatelets suspended in heptane were mixed with aluminium tri-sec butoxide and 5 mL of heptane, then loaded on the same spray-drying set-up, but at a different location than the first aqueous solution. The two liquids were sprayed simultaneously with two different means for forming droplets towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The particles were collected at the surface of a filter. The particles comprise a core of silica containing Fe.sub.3O.sub.4 nanoparticles and a shell of alumina containing CdSe/CdZnS nanoplatelets.
(84) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(85) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(86) The same procedure was carried out by replacing Al.sub.2O.sub.3 and/or SiO.sub.2 with TiO.sub.2, SiO.sub.2, Al.sub.2O.sub.3, HfO.sub.2, ZnTe, ZnSe, ZnO, ZnS or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(87) The same procedure was carried out by replacing Al.sub.2O.sub.3 and/or SiO.sub.2 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 10: Particles Preparation from an Organic Solution and an Aqueous SolutionCdS/ZnS Nanoplatelets@Al.SUB.2.O.SUB.3
(88) 4 mL of CdS/ZnS nanoplatelets suspended in heptane were mixed with aluminium tri-sec butoxide and 400 mL of heptane, then loaded in a spray-drying set-up. On another side, an acidic aqueous solution was prepared and loaded in the same spray-drying set-up, but at a different location than the first hexane solution. The two liquids were sprayed simultaneously with two different means for forming droplets towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The particles were collected at the surface of a filter.
(89) The same procedure was carried out by replacing CdS/ZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/CdZnS, CdTe/ZnS, CdSe/CdZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(90) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(91) The same procedure was carried out by replacing Al.sub.2O.sub.3 with SiO.sub.2, TiO.sub.2, HfO.sub.2, ZnTe, ZnSe, ZnO, ZnS or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(92) The same procedure was carried out by replacing Al.sub.2O.sub.3 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 11: Particles Preparation from an Organic Solution and an Aqueous SolutionInP/ZnS@SiO.SUB.2
(93) 4 mL of InP/ZnS nanoparticles suspended in an acidic aqueous solution were mixed with an acidic aqueous solution of TEOS at 0.13M previously hydrolyzed for 24 hours, then loaded in a spray-drying set-up. The suspension was sprayed for forming droplets towards a tube furnace heated a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The particles were collected at the surface of a filter.
(94) The same procedure was carried out by replacing InP/ZnS nanoparticles with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, CdSe/CdZnS, InP/CdS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(95) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(96) The same procedure was carried out by replacing SiO.sub.2 with TiO.sub.2, Al.sub.2O.sub.3, HfO.sub.2, ZnTe, ZnSe, ZnO, ZnS or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(97) The same procedure was carried out by replacing SiO.sub.2 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 12: Particles Preparation from an Organic Solution and an Aqueous Solution, Followed by a Treatment of Ammonia VaporsCdSe/CdZnS@ZnO
(98) 100 L of CdSe/CdZnS nanoplatelets suspended in heptane were mixed with zinc methoxyethoxide and 5 mL of pentane, then loaded on a spray-drying set-up as described in the invention. On another side, a basic aqueous solution was prepared and loaded on the same spray-drying set-up, but at a different location than the first heptane solution. On another side, an ammonium hydroxide solution was loaded on the same spray-drying system, between the tube furnace and the filter. The two first liquids were sprayed while the third one was heated at 35 C. by an external heating system to produce ammonia vapors, simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The particles were collected at the surface of a filter.
(99) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(100) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(101) The same procedure was carried out by replacing ZnO with TiO.sub.2, SiO.sub.2, HfO.sub.2, Al.sub.2O.sub.3, ZnTe, ZnSe, ZnS or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(102) The same procedure was carried out by replacing ZnO with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 13: Particles Preparation from an Organic Solution and an Aqueous Solution, Followed by an Extra Shell CoatingCdSe/CdZnS@Al.SUB.2.O.SUB.3.@MgO
(103) 100 L of CdSe/CdZnS nanoplatelets suspended in heptane were mixed with zinc methoxyethoxide and 5 mL of pentane, then loaded on a spray-drying set-up as described in the invention. On another side, a basic aqueous solution was prepared and loaded on the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The particles were directed towards a tube where an extra MgO shell was coated at the surface of the particles by an ALD process, said particles being suspended in the gas. The particles were finally collected on the inner wall of the tube where the ALD was performed.
(104) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(105) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
Example 14: Particles Preparation from an Organic Solution and an Aqueous SolutionCdSe/CdZnSFe.SUB.3.O.SUB.4.@SiO.SUB.2
(106) On one side, 100 L of Fe.sub.3O.sub.4 nanoparticles and 100 L of CdSe/CdZnS nanoplatelets suspended in an acidic aqueous solution were mixed with an acidic aqueous solution of TEOS at 0.13M previously hydrolyzed for 24 hours, then loaded in a spray-drying set-up as described in the invention. On another side, an acidic aqueous solution was prepared and loaded on the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The particles were collected at the surface of a filter.
(107) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(108) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
Example 15: Core/Shell Particles Preparation from an Organic Solution and an Aqueous SolutionAu@Al.SUB.2.O.SUB.3 .in the Core and CdSe/CdZnS@SiO.SUB.2 .in the Shell
(109) On one side, 100 L of CdSe/CdZnS nanoplatelets suspended in an acidic aqueous solution were mixed with an acidic aqueous solution of TEOS at 0.13M previously hydrolyzed for 24 hours, then loaded on a spray-drying set-up as described in the invention. On another side, 100 L of Au nanoparticles suspended in heptane were mixed with aluminium tri-sec butoxide and 5 mL of heptane, then loaded on the same spray-drying set-up, but at a different location than the first aqueous solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The particles were collected at the surface of a filter. The particles comprise a core of alumina containing gold nanoparticles and a shell of silica containing CdSe/CdZnS nanoplatelets.
(110) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(111) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
Example 16: Particles PreparationPhosphor Nanoparticles@SiO.SUB.2
(112) Phosphor nanoparticles were suspended in a basic aqueous solution were mixed with a basic aqueous solution of TEOS at 0.13M previously hydrolyzed for 24 hours, then loaded on a spray-drying set-up. The liquid mixture was sprayed towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The particles were collected at the surface of a filter.
(113) Phosphor nanoparticles used for this example were: Yttrium aluminium garnet nanoparticles (YAG, Y.sub.3Al.sub.5O.sub.12), (Ca,Y)--SiAlON:Eu nanoparticles, ((Y,Gd).sub.3(Al,Ga).sub.5O.sub.12:Ce) nanoparticles, CaAlSiN.sub.3:Eu nanoparticles, sulfide-based phosphor nanoparticles, PFS:Mn.sup.4+ nanoparticles (potassium fluorosilicate).
Example 17: Particles PreparationPhosphor Nanoparticles@Al.SUB.2.O.SUB.3
(114) Phosphor nanoparticles were suspended in heptane were mixed with aluminium tri-sec butoxide and 400 mL of heptane, then loaded in a spray-drying set-up. On another side, an acidic aqueous solution was prepared and loaded in the same spray-drying set-up, but at a different location than the first hexane solution. The two liquids were sprayed simultaneously with two different means for forming droplets towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The particles were collected at the surface of a filter.
(115) Phosphor nanoparticles used for this example were: Yttrium aluminium garnet nanoparticles (YAG, Y.sub.3Al.sub.5O.sub.12), (Ca,Y)--SiAlON:Eu nanoparticles, ((Y,Gd).sub.3(Al,Ga).sub.5O.sub.12:Ce) nanoparticles, CaAlSiN.sub.3:Eu nanoparticles, sulfide-based phosphor nanoparticles, PFS:Mn.sup.4+ nanoparticles (potassium fluorosilicate).
Example 18: Particles PreparationCdSe/CdZnS@HfO.SUB.2
(116) 100 L of CdSe/CdZnS nanoplatelets suspended in heptane (10 mg/mL) were mixed with Hafnium n-butoxide and 5 mL of pentane, then loaded on a spray-drying set-up. On another side, a basic aqueous solution was prepared and loaded on the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. Particles were collected at the surface of a filter.
(117) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(118) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
Example 19: Particles PreparationPhosphor Nanoparticles@HfO.SUB.2
(119) 1 m of phosphor nanoparticles (cf. list below) suspended in heptane (10 mg/mL) were mixed with hafnium n-butoxide and 5 mL of pentane, then loaded on a spray-drying set-up. On another side, an aqueous solution was prepared and loaded on the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The resulting particles phosphors particles@HfO.sub.2 were collected at the surface of a filter.
(120) Phosphor nanoparticles used for this example were: Yttrium aluminium garnet nanoparticles (YAG, Y.sub.3Al.sub.5O.sub.12), (Ca,Y)--SiAlON:Eu nanoparticles, ((Y,Gd).sub.3(Al,Ga).sub.5O.sub.12:Ce) nanoparticles, CaAlSiN.sub.3:Eu nanoparticles, sulfide-based phosphor nanoparticles, PFS:Mn.sup.4+ nanoparticles (potassium fluorosilicate).
Example 20: Particles Preparation from an Organometallic Precursor
(121) 100 L of CdSe/CdZnS nanoplatelets suspended in heptane were mixed with an organometallic precursor selected in the group below in pentane under controlled atmosphere, then loaded on a spray-drying set-up. On another side, an aqueous solution was prepared and loaded on the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated from room temperature to 300 C. with a nitrogen flow. The particles were collected at the surface of a filter.
(122) The procedure was carried out with an organometallic precursor selected in the group comprising: Al[N(SiMe.sub.3).sub.2].sub.3, trimethyl aluminium, triisobutylaluminum, trioctylaluminum, triphenylaluminum, dimethyl aluminium, trimethyl zinc, dimethyl zinc, diethylzinc, Zn[(N(TMS).sub.2].sub.2, Zn[(CF.sub.3SO.sub.2).sub.2N].sub.2, Zn(Ph).sub.2, Zn(C.sub.6F.sub.5).sub.2, Zn(TMHD).sub.2 (-diketonate), Hf[C.sub.5H.sub.4(CH.sub.3)].sub.2(CH.sub.3).sub.2, HfCH.sub.3(OCH.sub.3)[C.sub.5H.sub.4(CH.sub.3)].sub.2, [[(CH.sub.3).sub.3Si].sub.2N].sub.2HfCl.sub.2, (C.sub.5H.sub.5).sub.2Hf(CH.sub.3).sub.2, [(CH.sub.2CH.sub.3).sub.2N].sub.4Hf, [(CH.sub.3).sub.2N].sub.4Hf, [(CH.sub.3).sub.2N].sub.4Hf, [(CH.sub.3)(C.sub.2H.sub.5)N].sub.4Hf, [(CH.sub.3)(C.sub.2H.sub.5)N].sub.4Hf, 2,2,6,6-tetramethyl-3,5-heptanedione zirconium (Zr(THD).sub.4), C.sub.10H.sub.12Zr, Zr(CH.sub.3C.sub.5H.sub.4).sub.2CH.sub.3OCH.sub.3, C.sub.22H.sub.36Zr, [(C.sub.2H.sub.5).sub.2N].sub.4Zr, [(CH.sub.3).sub.2N].sub.4Zr, [(CH.sub.3).sub.2N].sub.4Zr, Zr(NCH.sub.3C.sub.2H.sub.5).sub.4, Zr(NCH.sub.3C.sub.2H.sub.5).sub.4, C.sub.18H.sub.32O.sub.6Zr, Zr(C.sub.5H.sub.15O.sub.2).sub.4, Zr(OCC(CH.sub.3).sub.3CHCOC(CH.sub.3).sub.3).sub.4, Mg(C.sub.5H.sub.5).sub.2, or C.sub.20H.sub.30Mg, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the organometallic precursor chosen.
(123) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(124) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(125) The same procedure was carried out by replacing Al.sub.2O.sub.3 with TiO.sub.2, ZnO, MgO, HfO.sub.2 or ZrO.sub.2. The same procedure was carried out by replacing Al.sub.2O.sub.3 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof.
(126) The same procedure was carried out by replacing the aqueous solution with another liquid or vapor source of oxidation.
Example 21: Particles Preparation from an Organometallic PrecursorCdSe/CdZnS@ZnTe
(127) 100 L of CdSe/CdZnS nanoplatelets suspended in heptane were mixed with two organometallic precursors selected in the group below in pentane under inert atmosphere then loaded on a spray-drying set-up. The suspension was sprayed towards a tube furnace heated from RT to 300 C. with a nitrogen flow. The particles were collected at the surface of a filter.
(128) The procedure was carried out by with a first organometallic precursor selected in the group comprising: dimethyl telluride, diethyl telluride, diisopropyl telluride, di-t-butyl telluride, diallyl telluride, methyl allyl telluride, dimethyl selenide, or dimethyl sulfur, or a mixture thereof.
(129) Reaction temperature of the above procedure is adapted according to the organometallic precursor chosen.
(130) The procedure was carried out by with a second organometallic precursor selected in the group comprising: dimethyl zinc, trimethyl zinc, diethylzinc, Zn[(N(TMS).sub.2].sub.2, Zn[(CF.sub.3SO.sub.2).sub.2N].sub.2, Zn(Ph).sub.2, Zn(C.sub.6F.sub.5).sub.2, or Zn(TMHD).sub.2 (-diketonate), or a mixture thereof. Reaction temperature of the above procedure is adapted according to the organometallic precursor chosen.
(131) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(132) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(133) The same procedure was carried out by replacing ZnTe with ZnS or ZnSe, or a mixture thereof.
(134) The same procedure was carried out by replacing ZnTe with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof.
Example 22: Particles Preparation from an Organometallic PrecursorCdSe/CdZnS @ZnS
(135) 100 L of CdSe/CdZnS nanoplatelets suspended in heptane were mixed with an organometallic precursor selected in the group below in pentane under inert atmosphere, then loaded on a spray-drying set-up. On another side, a vapor source of H.sub.2S was inserted in the same spray-drying set-up. The suspension was sprayed towards a tube furnace heated from RT to 300 C. with a nitrogen flow. The particles were collected at the surface of a filter.
(136) The procedure was carried out with an organometallic precursor selected in the group comprising: dimethyl zinc, trimethyl zinc, diethylzinc, Zn[(N(TMS).sub.2].sub.2, Zn[(CF.sub.3SO.sub.2).sub.2N].sub.2, Zn(Ph).sub.2, Zn(C.sub.6F.sub.5).sub.2, Zn(TMHD).sub.2 (-diketonate), or a mixture thereof. Reaction temperature of the above procedure is adapted according to the organometallic precursor chosen.
(137) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(138) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(139) The same procedure was carried out by replacing ZnS with ZnSe or ZnTe, or a mixture thereof.
(140) The same procedure was carried out by replacing ZnS with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof.
(141) The same procedure was carried out by replacing H.sub.2S with H.sub.2Se, H.sub.2Te or other gas.
Example 23: InP/GaP/ZnSe/ZnS@Al.SUB.2.O.SUB.3.@HfO.SUB.2
(142) 1st Step
(143) 100 L of InP/GaP/ZnSe/ZnS nanocrystals suspended in heptane (10 mg/mL) were mixed with aluminium tri-sec butoxide and 5 mL of pentane, then loaded on a spray-drying set-up. On another side, a basic aqueous solution was prepared and loaded the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The resulting particles InP/GaP/ZnSe/ZnS@Al.sub.2O.sub.3 were collected at the surface of a filter.
(144) 2nd Step
(145) 5 mg of InP/GaP/ZnSe/ZnS@Al.sub.2O.sub.3 particles were suspended in 5 mL of pentane and mixed with hafnium n-butoxide, then loaded on a spray-drying set-up. On another side, a basic aqueous solution was prepared and loaded the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The luminescent particles InP/GaP/ZnSe/ZnS@Al.sub.2O.sub.3@HfO.sub.2 were collected at the surface of a filter.
(146) The same procedure was carried out by replacing InP/GaP/ZnSe/ZnS nanocrystals with CdSe/CdZnS, CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(147) The same procedure was carried out by replacing InP/GaP/ZnSe/ZnS nanocrystals with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(148) The same procedure was carried out by replacing Al.sub.2O.sub.3 and/or HfO.sub.2 with TiO.sub.2, ZnTe, Al.sub.2O.sub.3, SiO.sub.2, HfO.sub.2, ZnSe, ZnO, ZnS, SiZrO.sub.2, SiHfO.sub.2 or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(149) The same procedure was carried out by replacing Al.sub.2O.sub.3 and/or HfO.sub.2 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 24: InP/ZnS/ZnSe/ZnS@Al.SUB.2.O.SUB.3.@HfO.SUB.2
(150) 1st Step
(151) 100 L of InP/ZnS/ZnSe/ZnS nanocrystals suspended in heptane (10 mg/mL) were mixed with aluminium tri-sec butoxide and 5 mL of pentane, then loaded on a spray-drying set-up. On another side, a basic aqueous solution was prepared and loaded the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The resulting particles InP/ZnS/ZnSe/ZnS@Al.sub.2O.sub.3 were collected at the surface of a filter.
(152) 2nd Step
(153) 5 mg of InP/ZnS/ZnSe/ZnS @Al.sub.2O.sub.3 particles were suspended in 5 mL of pentane and mixed with hafnium n-butoxide, then loaded on a spray-drying set-up. On another side, a basic aqueous solution was prepared and loaded the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The luminescent particles InP/ZnS/ZnSe/ZnS@Al.sub.2O.sub.3@HfO.sub.2 were collected at the surface of a filter.
(154) The same procedure was carried out by replacing InP/ZnS/ZnSe/ZnS nanocrystals with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(155) The same procedure was carried out by replacing InP/ZnS/ZnSe/ZnS nanocrystals with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(156) The same procedure was carried out by replacing Al.sub.2O.sub.3 and/or HfO.sub.2 with TiO.sub.2, ZnTe, Al.sub.2O.sub.3, SiO.sub.2, HfO.sub.2, ZnSe, ZnO, ZnS, SiZrO.sub.2, SiHfO.sub.2 or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(157) The same procedure was carried out by replacing Al.sub.2O.sub.3 and/or HfO.sub.2 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 25: CdSe/CdZnS@HfO.SUB.2.@Si.SUB.0.8.Hf.SUB.0.2.O.SUB.2
(158) 1st Step
(159) 100 L of CdSe/CdZnS nanoplatelets suspended in heptane (10 mg/mL) were mixed with hafnium n-butoxide and 5 mL of pentane, then loaded on a spray-drying set-up. On another side, an aqueous solution was prepared and loaded the same spray-drying set-up, but at a different location than the first pentane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The resulting particles CdSe/CdZnS@HfO.sub.2 were collected at the surface of a filter.
(160) 2nd Step
(161) 50 mg of CdSe/CdZnS@HfO.sub.2 particles were suspended in 20 mL of ethanol and mixed with TEOS, hafnium oxychloride and water, then loaded on a spray-drying set-up. The liquid was sprayed towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The luminescent particles CdSe/CdZnS@HfO.sub.2@SiHfO.sub.2 were collected at the surface of a filter.
(162) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(163) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(164) The same procedure was carried out by replacing SiHfO.sub.2 and/or HfO.sub.2 with ZnTe, Al.sub.2O.sub.3, SiO.sub.2, HfO.sub.2, ZnSe, TiO.sub.2, ZnO, ZnS, SiZrO.sub.2, SiHfO.sub.2 or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(165) The same procedure was carried out by replacing SiHfO.sub.2 and/or HfO.sub.2 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 26: CdSe/CdZnS@HfO.SUB.2.@Si.SUB.0.8.Zr.SUB.0.2.O.SUB.2
(166) 1st Step
(167) 100 L of CdSe/CdZnS nanoplatelets suspended in heptane (10 mg/mL) were mixed with hafnium n-butoxide and 5 mL of pentane, then loaded on a spray-drying set-up. On another side, an aqueous solution was prepared and loaded the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The resulting particles CdSe/CdZnS@HfO.sub.2 were collected at the surface of a filter.
(168) 2nd Step
(169) 50 mg of CdSe/CdZnS@HfO.sub.2 particles were suspended in 20 mL of ethanol and mixed with TEOS, zirconium oxychloride and water, then loaded on a spray-drying set-up. The liquid was sprayed towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The luminescent particles CdSe/CdZnS @HfO.sub.2@SiZrO.sub.2 were collected at the surface of a filter.
(170) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(171) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(172) The same procedure was carried out by replacing SiZrO.sub.2 and/or HfO.sub.2 with ZnTe, Al.sub.2O.sub.3, SiO.sub.2, HfO.sub.2, ZnSe, TiO.sub.2, ZnO, ZnS, SiZrO.sub.2, SiHfO.sub.2 or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(173) The same procedure was carried out by replacing SiZrO.sub.2 and/or HfO.sub.2 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 27: CdSe/CdZnS@Al.SUB.2.O.SUB.3.@HfO.SUB.2
(174) 1st Step
(175) 100 L of CdSe/CdZnS nanoplatelets suspended in heptane (10 mg/mL) were mixed with aluminium tri-sec butoxide and 5 mL of pentane, then loaded on a spray-drying set-up. On another side, an aqueous solution was prepared and loaded the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The resulting particles CdSe/CdZnS@Al.sub.2O.sub.3 (particles 2) were collected at the surface of a filter.
(176) 2nd Step
(177) 5 mg of CdSe/CdZnS@Al.sub.2O.sub.3 particles were suspended in 5 mL of pentane and mixed with hafnium n-butoxide, then loaded on a spray-drying set-up. On another side, an aqueous solution was prepared and loaded the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The luminescent particles CdSe/CdZnS@Al.sub.2O.sub.3@HfO.sub.2 were collected at the surface of a filter.
(178) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(179) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(180) The same procedure was carried out by replacing Al.sub.2O.sub.3 and/or HfO.sub.2 with ZnTe, TiO.sub.2, Al.sub.2O.sub.3, SiO.sub.2, HfO.sub.2, ZnSe, ZnO, ZnS, SiZrO.sub.2, SiHfO.sub.2 or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(181) The same procedure was carried out by replacing Al.sub.2O.sub.3 and/or HfO.sub.2 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 28: CdSe/CdZnS@Al.SUB.2.O.SUB.3 .and SnO.SUB.2 .Particles Encapsulated in Al.SUB.2.O.SUB.3
(182) 5 mg of a previously prepared CdSe/CdZnS@Al.sub.2O.sub.3 particles (size: 150 nm) were suspended in 5 mL of pentane along with larger particles (SnO.sub.2, 2 m) and mixed with aluminium tri-sec butoxide, then loaded on a spray-drying set-up. On another side, a basic aqueous solution was prepared and loaded the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The luminescent particles, CdSe/CdZnS@Al.sub.2O.sub.3 and SnO.sub.2 particles encapsulated in Al.sub.2O.sub.3, were collected at the surface of a filter.
(183) Note: the amount of aluminium tri-sec butoxide is calculated so that the amount of Al.sub.2O.sub.3 formed would form a layer around the SnO.sub.2 particle so that it is thicker than the solid diameter.
(184) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets and/or SnO.sub.2 particles with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(185) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets and/or SnO.sub.2 particles with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(186) The same procedure was carried out by replacing Al.sub.2O.sub.3 with ZnTe, Al.sub.2O.sub.3, TiO.sub.2, SiO.sub.2, HfO.sub.2, ZnSe, ZnO, ZnS, SiZrO.sub.2, SiHfO.sub.2 or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(187) The same procedure was carried out by replacing Al.sub.2O.sub.3 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 29: Phosphor Particles@Al.SUB.2.O.SUB.3.@HfO.SUB.2
(188) 1st Step
(189) 1 m of phosphor particles (cf. list below) suspended in heptane (10 mg/mL) were mixed with aluminium tri-sec butoxide and 5 mL of pentane, then loaded on a spray-drying set-up. On another side, an aqueous solution was prepared and loaded the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The resulting particles phosphors particles@Al.sub.2O.sub.3 were collected at the surface of a filter.
(190) 2nd Step
(191) 5 mg of phosphors particles@Al.sub.2O.sub.3 were suspended in 5 mL of pentane and mixed with hafnium n-butoxide, then loaded on a spray-drying set-up. On another side, an aqueous solution was prepared and loaded the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The luminescent particles phosphor particles@Al.sub.2O.sub.3@HfO.sub.2 were collected at the surface of a filter.
(192) Phosphor particles used for this example were: Yttrium aluminium garnet particles (YAG, Y.sub.3Al.sub.5O.sub.12), (Ca,Y)--SiAlON:Eu particles, ((Y,Gd).sub.3(Al,Ga).sub.5O.sub.12:Ce) particles, CaAlSiN.sub.3:Eu particles, sulfide-based phosphor particles, PFS:Mn.sup.4+ particles (potassium fluorosilicate).
(193) The same procedure was carried out by replacing Al.sub.2O.sub.3 and/or HfO.sub.2 with TiO.sub.2, ZnTe, Al.sub.2O.sub.3, SiO.sub.2, HfO.sub.2, ZnSe, ZnO, ZnS, SiZrO.sub.2, SiHfO.sub.2 or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(194) The same procedure was carried out by replacing Al.sub.2O.sub.3 and/or HfO.sub.2 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 30: CdSe/CdZnS@HfO.SUB.2.@Al.SUB.2.O.SUB.3
(195) 1st Step
(196) 100 L of CdSe/CdZnS nanoplatelets suspended in heptane (10 mg/mL) were mixed with hafnium n-butoxide and 5 mL of pentane, then loaded on a spray-drying set-up. On another side, a basic aqueous solution was prepared and loaded the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The resulting particles CdSe/CdZnS@HfO.sub.2 were collected at the surface of a filter.
(197) 2nd Step
(198) 5 mg of CdSe/CdZnS@HfO.sub.2 particles were suspended in 5 mL of pentane and mixed with aluminium tri-sec butoxide, then loaded on a spray-drying set-up. On another side, a basic aqueous solution was prepared and loaded the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The luminescent particles CdSe/CdZnS@HfO.sub.2@Al.sub.2O.sub.3 were collected at the surface of a filter.
(199) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(200) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(201) The same procedure was carried out by replacing Al.sub.2O.sub.3 and/or HfO.sub.2 with TiO.sub.2, ZnTe, Al.sub.2O.sub.3, SiO.sub.2, HfO.sub.2, ZnSe, ZnO, ZnS, SiZrO.sub.2, SiHfO.sub.2 or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(202) The same procedure was carried out by replacing Al.sub.2O.sub.3 and/or HfO.sub.2 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 31: CdSe/CdZnS@HfO.SUB.2 .and SnO.SUB.2 .Particles Encapsulated in Al.SUB.2.O.SUB.3
(203) 5 mg of a previously prepared CdSe/CdZnS@HfO.sub.2 particles (size: 150 nm) were suspended in 5 mL of pentane along with larger particles (SnO.sub.2, 2 am) and mixed with aluminium tri-sec butoxide, then loaded on a spray-drying set-up. On another side, an aqueous solution was prepared and loaded the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The luminescent particles, CdSe/CdZnS@HfO.sub.2 and SnO.sub.2 particles encapsulated in Al.sub.2O.sub.3, were collected at the surface of a filter.
(204) Note: the amount of aluminium tri-sec butoxide is calculated so that the amount of Al.sub.2O.sub.3 formed would form a layer around the SnO.sub.2 particle so that it is thicker than the solid diameter.
(205) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets and/or SnO.sub.2 particles with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(206) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets and/or SnO.sub.2 particles with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(207) The same procedure was carried out by replacing Al.sub.2O.sub.3 and/or HfO.sub.2 with TiO.sub.2, ZnTe, Al.sub.2O.sub.3, SiO.sub.2, HfO.sub.2, ZnSe, ZnO, ZnS, SiZrO.sub.2, SiHfO.sub.2 or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(208) The same procedure was carried out by replacing Al.sub.2O.sub.3 and/or HfO.sub.2 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 32: Phosphor Particles@HfO.SUB.2.@Al.SUB.2.O.SUB.3
(209) 1st Step
(210) 1 m of phosphor particles (cf. list below) suspended in heptane (10 mg/mL) were mixed with hafnium n-butoxide and 5 mL of pentane, then loaded on a spray-drying set-up. On another side, an aqueous solution was prepared and loaded the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The resulting particles phosphors particles@HfO.sub.2 were collected at the surface of a filter.
(211) 2nd Step
(212) 5 mg of phosphors particles@HfO.sub.2 were suspended in 5 mL of pentane and mixed with aluminium tri-sec butoxide, then loaded on a spray-drying set-up. On another side, an aqueous solution was prepared and loaded the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The luminescent particles phosphor particles @HfO.sub.2@Al.sub.2O.sub.3 were collected at the surface of a filter.
(213) Phosphor particles used for this example were: Yttrium aluminium garnet particles (YAG, Y.sub.3Al.sub.5O.sub.12), (Ca,Y)--SiAlON:Eu particles, ((Y,Gd).sub.3(Al,Ga).sub.5O.sub.12:Ce) particles, CaAlSiN.sub.3:Eu particles, sulfide-based phosphor particles, PFS:Mn.sup.4+ particles (potassium fluorosilicate).
(214) The same procedure was carried out by replacing Al.sub.2O.sub.3 and/or HfO.sub.2 with TiO.sub.2, ZnTe, Al.sub.2O.sub.3, SiO.sub.2, HfO.sub.2, ZnSe, ZnO, ZnS, SiZrO.sub.2, SiHfO.sub.2 or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(215) The same procedure was carried out by replacing Al.sub.2O.sub.3 and/or HfO.sub.2 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 33: Preparation of CdSe/CdZnS@HfO.SUB.2.@SiO.SUB.2 .Comprising SnO.SUB.2 .Nanoparticles by Microemulsion
(216) CdSe/CdZnS@HfO.sub.2 and SnO.sub.2 nanoparticles (30-40 nm diameter) were coated with SiO.sub.2 using reverse micelles of polyoxyethylene cetylether (Nihon surfactant, C-15) using cyclohexane (purity 99.0%) as the organic phase. The concentration of the surfactant in the organic solvent was 0.5 mol/L. The microemulsion solution was prepared by injecting an aqueous solution (4.0 mL, denoted as aq.) containing 100 mg of CdSe/CdZnS@HfO.sub.2 and SnO.sub.2 nanoparticles (varying proportions) into the organic surfactant solution (100 mL) at 50 C. under magnetic stirring. An oxalic acid solution ((COOH).sub.2 aq., 1 mol/L, 3.0 mL) was used to charge positively the oxides surface. Tetraethylorthosilicate (TEOS, 0.86 mol/L in the microemulsion solution) as a SiO.sub.2 source and diluted NH.sub.4OH solution (2.70 mol/l, 15.0 ml) were charged into the microemulsion containing CdSe/CdZnS @HfO.sub.2 and SnO.sub.2 nanoparticles, and subjected to hydrolysis at 50 C. for 60 min. The molar ratio of water to surfactant in the solution during TEOS hydrolysis was 23. The solid formed was centrifuged, thoroughly washed with propanol, dried at 80 C. overnight, and a thermal treatment at 130 C. for 24 h was performed in air.
(217) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets and/or SnO.sub.2 nanoparticles with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(218) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets and/or SnO.sub.2 nanoparticles with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(219) The same procedure was carried out by replacing SiO.sub.2 and/or HfO.sub.2 with TiO.sub.2, ZnTe, Al.sub.2O.sub.3, SiO.sub.2, HfO.sub.2, ZnSe, ZnO, ZnS, SiZrO.sub.2, SiHfO.sub.2 or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(220) The same procedure was carried out by replacing SiO.sub.2 and/or HfO.sub.2 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 34: Semiconductor Nanoplatelets@Al.SUB.2.O.SUB.3.@SiO.SUB.2
(221) The dry solid 0.05 g, i.e., semiconductor nanoplatelets@Al.sub.2O.sub.3, is weighted under dry atmosphere (glovebox) and is dispersed in 1 mL of pure/dry THF, then 0.07 mL of 2.3 mol.Math.L.sup.1 HCl solution is added. The solution is then heated in a closed vessel to 70 C. A solution (1 mL) containing TEOS (TetraEthyl OrthoSilicate) (0.5 mmol.Math.L.sup.1) in clean THF is added dropwise over a period of 0.1 mol.Math.min.sup.1 under stirring. The mixture is then refluxed for about 1 h. The product is then filtered and washed consecutively with 20/80 water/THF (35 mL), EtOH (35 mL), and Et.sub.2O (35 mL), and dried at 80 C. under vacuum.
(222) The same procedure was carried out by replacing semiconductor nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(223) The same procedure was carried out by replacing Al.sub.2O.sub.3 and/or SiO.sub.2 with TiO.sub.2, ZnTe, Al.sub.2O.sub.3, SiO.sub.2, HfO.sub.2, ZnSe, ZnO, ZnS, SiZrO.sub.2, SiHfO.sub.2 or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(224) The same procedure was carried out by replacing Al.sub.2O.sub.3 and/or SiO.sub.2 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 35: Semiconductor Nanoplatelets@HfO.SUB.2.@SiO.SUB.2
(225) The dry solid 0.05 g, i.e., semiconductor nanoplatelets@HfO.sub.2, is weighted under dry atmosphere (glovebox) and is dispersed in 1 mL of pure/dry THF, then 0.07 mL of 2.3 mol.Math.L.sup.1 HCl solution is added. The solution is then heated in a closed vessel to 70 C. A solution (1 mL) containing TEOS (TetraEthyl OrthoSilicate) (0.5 mmol.Math.L.sup.1) in clean THF is added dropwise over a period of 0.1 mol.Math.min.sup.1 under stirring. The mixture is then refluxed for about 1 h. The product is then filtered and washed consecutively with 20/80 water/THF (35 mL), EtOH (35 mL), and Et.sub.2O (35 mL), and dried at 80 C. under vacuum.
(226) Note 1: Trialkoxy Azidoalkyl silane, Trialkoxy Aminoalkyl silane or Trialkoxy alkylThiol silane can be added to the TEOS solution to add versatile functionalities the solid for further functionalization.
(227) The same procedure was carried out by replacing semiconductor nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(228) The same procedure was carried out by replacing HfO.sub.2 and/or SiO.sub.2 with TiO.sub.2, ZnTe, Al.sub.2O.sub.3, SiO.sub.2, HfO.sub.2, ZnSe, ZnO, ZnS, SiZrO.sub.2, SiHfO.sub.2 or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(229) The same procedure was carried out by replacing HfO.sub.2 and/or SiO.sub.2 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 36: Semiconductor Nanoplatelets@Al.SUB.2.O.SUB.3.@SiO.SUB.2
(230) Semiconductor nanoplatelets@Al.sub.2O.sub.3 particles are dispersed in 16.7 wt % H.sub.2O in an anhydrous ethanol to reach 5 wt. % solid loading and then ultrasonicated to break down agglomerates. A 20 wt. % of TEOS+silane in ethanol solution (quantity varied to tune SiO.sub.2 thickness) was carefully added to the suspension step by step. The amounts of added TEOS were calculated based on the surface area of semiconductor nanoplatelets@Al.sub.2O.sub.3 particle and the desired shell thickness, assuming complete conversion of TEOS to silica. The appropriate pH value of the suspension was adjusted using ammonia to pH=11. Afterward, the suspension was stirred at 50 C. for 6 h to control the thickness of the coating layer through the hydrolysis and condensation of TEOS on the surface of semiconductor nanoplatelets@Al.sub.2O.sub.3 particle. Resulting particles were then collected by centrifuged, washed with anhydrous ethanol and dried in an oven at 80 C.
(231) The same procedure was carried out by replacing semiconductor nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(232) The same procedure was carried out by replacing Al.sub.2O.sub.3 and/or SiO.sub.2 with ZnTe, TiO.sub.2, Al.sub.2O.sub.3, SiO.sub.2, HfO.sub.2, ZnSe, ZnO, ZnS, SiZrO.sub.2, SiHfO.sub.2 or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(233) The same procedure was carried out by replacing Al.sub.2O.sub.3 and/or SiO.sub.2 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 37: CdSe/CdZnS@HfO.SUB.2.@SiO.SUB.2
(234) 1st Step
(235) 100 L of CdSe/CdZnS nanoplatelets suspended in heptane (10 mg/mL) were mixed with Hafnium n-butoxide and 5 mL of pentane, then loaded on a spray-drying set-up. On another side, a basic aqueous solution was prepared and loaded the same spray-drying set-up, but at a different location than the first heptane solution. The two liquids were sprayed simultaneously towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The resulting particles CdSe/CdZnS@HfO.sub.2 were collected at the surface of a filter.
(236) 2nd Step
(237) 50 mg of CdSe/CdZnS@HfO.sub.2 particles were suspended in 20 mL of water and mixed with TEOS and ammonia, then loaded on a spray-drying set-up. The liquid was sprayed towards a tube furnace heated at a temperature ranging from the boiling point of the solvent to 1000 C. with a nitrogen flow. The luminescent particles CdSe/CdZnS@HfO.sub.2@SiO.sub.2 were collected at the surface of a filter.
(238)
(239)
(240) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(241) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(242) The same procedure was carried out by replacing SiO.sub.2 and/or HfO.sub.2 with TiO.sub.2, ZnTe, Al.sub.2O.sub.3, SiO.sub.2, HfO.sub.2, ZnSe, ZnO, ZnS, SiZrO.sub.2, SiHfO.sub.2 or MgO, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
(243) The same procedure was carried out by replacing SiO.sub.2 and/or HfO.sub.2 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the inorganic material chosen.
Example 38: Luminescent Particles Preparation from an Organometallic Precursor
(244) 100 L of CdSe/CdZnS@HfO.sub.2 particles suspended in heptane were mixed with an organometallic precursor selected in the group below in pentane under controlled atmosphere, then loaded on a spray-drying set-up. On another side, an aqueous solution was prepared and loaded on the same spray-drying set-up, but at a different location than the first heptane solution.
(245) The two liquids were sprayed simultaneously towards a tube furnace heated from room temperature to 300 C. with a nitrogen flow. The particles were collected at the surface of a filter.
(246) The procedure was carried out with an organometallic precursor selected in the group comprising: Al[N(SiMe.sub.3).sub.2].sub.3, trimethyl aluminium, triisobutylaluminum, trioctylaluminum, triphenylaluminum, dimethyl aluminium, trimethyl zinc, dimethyl zinc, diethylzinc, Zn[(N(TMS).sub.2].sub.2, Zn[(CF.sub.3SO.sub.2).sub.2N].sub.2, Zn(Ph).sub.2, Zn(C.sub.6F.sub.5).sub.2, Zn(TMHD).sub.2 (-diketonate), Hf[C.sub.5H.sub.4(CH.sub.3)].sub.2(CH.sub.3).sub.2, HfCH.sub.3(OCH.sub.3)[C.sub.5H.sub.4(CH.sub.3)].sub.2, [[(CH.sub.3).sub.3Si].sub.2N].sub.2HfCl.sub.2, (C.sub.5H.sub.5).sub.2Hf(CH.sub.3).sub.2, [(CH.sub.2CH.sub.3).sub.2N].sub.4Hf, [(CH.sub.3).sub.2N].sub.4Hf, [(CH.sub.3).sub.2N].sub.4Hf, [(CH.sub.3)(C.sub.2H.sub.5)N].sub.4Hf, [(CH.sub.3)(C.sub.2H.sub.5)N].sub.4Hf, 2,2,6,6-tetramethyl-3,5-heptanedione zirconium (Zr(THD).sub.4), C.sub.10H.sub.12Zr, Zr(CH.sub.3C.sub.5H.sub.4).sub.2CH.sub.3OCH.sub.3, C.sub.22H.sub.36Zr, [(C.sub.2H.sub.5).sub.2N].sub.4Zr, [(CH.sub.3).sub.2N].sub.4Zr, [(CH.sub.3).sub.2N].sub.4Zr, Zr(NCH.sub.3C.sub.2H.sub.5).sub.4, Zr(NCH.sub.3C.sub.2H.sub.5).sub.4, C.sub.18H.sub.32O.sub.6Zr, Zr(C.sub.5H.sub.15O.sub.2).sub.4, Zr(OCC(CH.sub.3).sub.3CHCOC(CH.sub.3).sub.3).sub.4, Mg(C.sub.5H.sub.5).sub.2, or C.sub.20H.sub.30Mg, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the organometallic precursor chosen.
(247) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(248) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(249) The same procedure was carried out by replacing HfO.sub.2 with ZnTe, TiO.sub.2, Al.sub.2O.sub.3, SiO.sub.2, HfO.sub.2, ZnSe, ZnO, ZnS, SiZrO.sub.2, SiHfO.sub.2 or MgO, or a mixture thereof.
(250) The same procedure was carried out by replacing HfO.sub.2 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof.
(251) The same procedure was carried out by replacing the aqueous solution with another liquid or vapor source of oxidation.
Example 39: Luminescent Particles Preparation from an Organometallic PrecursorCdSe/CdZnS@HfO.SUB.2.@ZnTe
(252) 100 L of CdSe/CdZnS@HfO.sub.2 particles suspended in heptane were mixed with two organometallic precursors selected in the group below in pentane under inert atmosphere then loaded on a spray-drying set-up. The suspension was sprayed towards a tube furnace heated from RT to 300 C. with a nitrogen flow. The particles were collected at the surface of a filter.
(253) The procedure was carried out by with a first organometallic precursor selected in the group comprising: dimethyl telluride, diethyl telluride, diisopropyl telluride, di-t-butyl telluride, diallyl telluride, methyl allyl telluride, dimethyl selenide, or dimethyl sulfur, or a mixture thereof. Reaction temperature of the above procedure is adapted according to the organometallic precursor chosen.
(254) The procedure was carried out by with a second organometallic precursor selected in the group comprising: dimethyl zinc, trimethyl zinc, diethylzinc, Zn[(N(TMS).sub.2].sub.2, Zn[(CF.sub.3SO.sub.2).sub.2N].sub.2, Zn(Ph).sub.2, Zn(C.sub.6F.sub.5).sub.2, or Zn(TMHD).sub.2 (-diketonate), or a mixture thereof. Reaction temperature of the above procedure is adapted according to the organometallic precursor chosen.
(255) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(256) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(257) The same procedure was carried out by replacing ZnTe with ZnS or ZnSe, or a mixture thereof.
(258) The same procedure was carried out by replacing HfO.sub.2 with ZnTe, TiO.sub.2, Al.sub.2O.sub.3, SiO.sub.2, HfO.sub.2, ZnSe, ZnO, ZnS, SiZrO.sub.2, SiHfO.sub.2 or MgO. The same procedure was carried out by replacing HfO.sub.2 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer, or a mixture thereof.
(259) The same procedure was carried out by replacing the aqueous solution with another liquid or vapor source of oxidation.
Example 40: Luminescent Particles Preparation from an Organometallic PrecursorCdSe/CdZnS@HfO.SUB.2.@ZnS
(260) 100 L of CdSe/CdZnS@HfO.sub.2 particles suspended in heptane were mixed with an organometallic precursor selected in the group below in pentane under inert atmosphere, then loaded on a spray-drying set-up. On another side, a vapor source of H.sub.2S was inserted in the same spray-drying set-up. The suspension was sprayed towards a tube furnace heated from RT to 300 C. with a nitrogen flow. The particles were collected at the surface of a filter.
(261) The procedure was carried out with an organometallic precursor selected in the group comprising: dimethyl zinc, trimethyl zinc, diethylzinc, Zn[(N(TMS).sub.2].sub.2, Zn[(CF.sub.3SO.sub.2).sub.2N].sub.2, Zn(Ph).sub.2, Zn(C.sub.6F.sub.5).sub.2, Zn(TMHD).sub.2 (-diketonate), or a mixture thereof. Reaction temperature of the above procedure is adapted according to the organometallic precursor chosen.
(262) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with CdSe, CdS, CdTe, CdSe/CdS, CdSe/ZnS, CdSe/CdZnS, CdS/ZnS, CdS/CdZnS, CdTe/ZnS, CdTe/CdZnS, CdSeS/ZnS, CdSeS/CdS, CdSeS/CdZnS, CuInS.sub.2/ZnS, CuInSe.sub.2/ZnS, InP/CdS, InP/ZnS, InZnP/ZnS, InP/ZnSeS, InP/ZnSe, InP/CdZnS, CdSe/CdZnS/ZnS, CdSe/ZnS/CdZnS, CdSe/CdS/ZnS, CdSe/CdS/CdZnS, CdSe/ZnSe/ZnS, CdSeS/CdS/ZnS, CdSeS/CdS/CdZnS, CdSeS/CdZnS/ZnS, CdSeS/ZnSe/ZnS, CdSeS/ZnSe/CdZnS, CdSeS/ZnS/CdZnS, CdSe/ZnS/CdS, CdSeS/ZnS/CdS, CdSe/ZnSe/CdZnS, InP/ZnSe/ZnS, InP/CdS/ZnSe/ZnS, InP/CdS/ZnS, InP/ZnS/CdS, InP/GaP/ZnS, InP/GaP/ZnSe, InP/CdZnS/ZnS, InP/ZnS/CdZnS, InP/CdS/CdZnS, InP/ZnSe/CdZnS, InP/ZnS/ZnSe, InP/GaP/ZnSe/ZnS, InP/ZnS/ZnSe/ZnS, nanoplatelets or quantum dots, or a mixture thereof.
(263) The same procedure was carried out by replacing CdSe/CdZnS nanoplatelets with organic nanoparticles, inorganic nanoparticles such as metal nanoparticles, halide nanoparticles, chalcogenide nanoparticles, phosphide nanoparticles, sulfide nanoparticles, metalloid nanoparticles, metallic alloy nanoparticles, phosphor nanoparticles, perovskite nanoparticles, ceramic nanoparticles such as for example oxide nanoparticles, carbide nanoparticles, nitride nanoparticles, or a mixture thereof.
(264) The same procedure was carried out by replacing ZnS with ZnSe or ZnTe, or a mixture thereof.
(265) The same procedure was carried out by replacing HfO.sub.2 with ZnTe, TiO.sub.2, Al.sub.2O.sub.3, SiO.sub.2, HfO.sub.2, ZnSe, ZnO, ZnS, SiZrO.sub.2, SiHfO.sub.2 or MgO, or a mixture thereof. The same procedure was carried out by replacing HfO.sub.2 with a metal material, halide material, chalcogenide material, phosphide material, sulfide material, metalloid material, metallic alloy material, ceramic material such as for example oxide, carbide, nitride, glass, enamel, ceramic, stone, precious stone, pigment, cement and/or inorganic polymer
(266) The same procedure was carried out by replacing the aqueous solution with another liquid or vapor source of oxidation.
(267) The same procedure was carried out by replacing H.sub.2S with H.sub.2Se, H.sub.2Te or other gas.
Example 41: Ink
(268) Particles of the invention were prepared, collected and then dispersed in a solvent composed of 40 l of toluene and 20 l of PMMA (10 wt % in toluene). The resulting suspension was homogeneously mixed using ultrasonic bath (37 kHz, 480 W, sweep mode) for 1 minute.
Example 42: Ink
(269) 0.1 g of particles of the invention having an emission peak centered at 620 nm were mixed with a mixed solvent of 70 g of chlorobenzene and 24.9 g of cyclohexane, and 5 g of Ttiton X-100 as an additive was added to the mixture to prepare an ink composition for inkjet printing.
Example 43: Ink
(270) 10 mg of particles of the invention in toluene is added to 1.0 mL of Ebecyl 150 and degassed under reduced pressure to remove the toluene and oxygen. Once the toluene is removed, three purge and N.sub.2 back-fill cycles are completed and then 10 mg of TiO.sub.2 (1% by weight) is added to the formulation and the mixture is degassed under reduced pressure while stirring in order to disperse the TiO.sub.2. The formulation is then ready for ink preparation.
Example 44: Ink
(271) An ink composition was prepared comprising: 40 wt. % to 60 wt. % polyethylene glycol dimethacrylate monomer, or polyethylene glycol diacrylate monomer (number average molecular weights in the range from about 230 g/mole to about 430 g mole); 25 wt. % to 50 wt. % monoacrylate monomer, or monomethacrylate monomer (viscosity in the range from about 10 cps to about 27 cps at 22 C.); 4 wt. % to 10 wt. % multifunctional acrylate crosslinking agent, or a multifunctional methacrylate crosslinking agent; and 0.1 wt. % to 10 wt. % crosslinking photoinitiator; and 0.01 wt. % to 50 wt. % particles of the invention.
(272) The resulting ink composition has a surface tension of between about 32 dynes/cm and about 45 dynes/cm at 22 C.
Example 45: Ink
(273) An ink composition was prepared comprising: from 30 wt. % to 50 wt. % of a polyethylene glycol dimethacrylate monomer, or a polyethylene glycol diacrylate monomer (number average molecular weights in the range from 230 g/mole to 430 g/mole); from 4 wt. % to 10 wt. % of a multifunctional acrylate crosslinking agent, or a multifunctional methacrylate crosslinking agent; from 40 wt. % to 60 wt. % of a spreading modifier comprising an alkoxylated aliphatic diacrylate monomer, or an alkoxylated aliphatic dimethacrylate monomer (viscosity in the range from 14 cps to 18 cps at 22 C. and surface tension in the range from 35 dynes/cm to 39 dynes/cm at 22 C.); and 0.01 wt. % to 50 wt. % particles of the invention.
Example 46: Ink
(274) An ink composition was prepared comprising: from 30 wt. % to 50 wt. % of a monomer selected from the group consisting of a polyethylene glycol dimethacrylate monomer, a polyethylene glycol diacrylate monomer (number average molecular weights in the range from 230 g/mole to 430 g/mole); from 4 wt. % to 10 wt. % of a crosslinking agent selected from the group consisting of a multifunctional acrylate crosslinking agent, a multifunctional methacrylate crosslinking agent; from 40 wt. % to 60 wt. % of a spreading modifier selected from the group consisting of an alkoxylated aliphatic diacrylate monomer, an alkoxylated aliphatic dimethacrylate monomer; and 0.01 wt. % to 50 wt. % particles of the invention.
(275) The resulting ink composition has a viscosity in the range from 14 cps to 18 cps at 22 C. and a surface tension in the range from 35 dynes/cm to 39 dynes/cm at 22 C.
Example 47: Ink
(276) An ink composition was prepared comprising: 75-95 wt. % of a polyethylene glycol dimethacrylate monomer, or a polyethylene glycol diacrylate monomer (number average molecular weights in the range from about 230 g/mole to about 430 g/mole); 4-10 wt. % of pentaerythritol tetraacrylate, or pentaerythritol tetramethacrylate; 1-15 wt. % of a spreading modifier (viscosity in the range from about 14 to about 18 cps at 22 C. and surface tension in the range from about 35 to about 39 dynes/cm at 22 C.); and 0.01 wt. % to 50 wt. % particles of the invention.
Example 48: Ink
(277) An ink composition was prepared comprising: 70 wt. % to 96 wt. % di(meth)acrylate monomers or a combination of di(meth)acrylate monomers and mono(meth)acrylate monomers; 4 wt. % to 10 wt. % multifunctional (meth)acrylate crosslinking agent; and 0.1 wt. % to 5 wt. % particles of the invention; wherein said particles are particles 1 as prepared in the examples hereabove; or particles 2 as prepared in the examples hereabove;
(278) The resulting ink composition has a viscosity in the range from 2 cps to 30 cps and a surface tension at 22 C. in the range from 25 dyne/cm to 45 dyne/cm at a temperature in the range from 22 C. to 40 C.
REFERENCES
(279) 1Particle 11First material 12Core of the particle 13Shell of the particle 14Inorganic material 15Ink 2Particle 21Second material 22Core of the particle 2 23Shell of the particle 2 3Nanoparticle 31Spherical Nanoparticle 322D nanoparticle 33Core of a nanoparticle 34First shell of a nanoparticle 35Second shell of a nanoparticle 36Insulator shell of a nanoparticle 37Crown of a nanoparticle 4LED support 5LED chip 6Microsized LED 7Light emitting material 71Host material 8Bead 81Third material 9Dense particle DPixel pitch