PREPARATIONS OF NOBLE METAL COMPLEXES
20230243038 · 2023-08-03
Inventors
Cpc classification
C23C18/08
CHEMISTRY; METALLURGY
International classification
Abstract
A preparation containing: (A) 30 to 90 wt. % of at least one organic solvent, (B) 10 to 70 wt. % of at least one noble metal complex comprising diolefin and C6-C18 monocarboxylate ligands selected from the group consisting of noble metal complexes of the type [LPd[O(CO)R1]X].sub.n, [LRh[O(CO)R1]].sub.m, and [LIr[O(CO)R1]].sub.m, wherein L represents a compound acting as diolefin ligand, wherein X is selected among bromide, chloride, iodide, and —O(CO)R2, wherein —O(CO)R1 and —O(CO)R2 represent identical or different non-aromatic C6-C18 monocarboxylic acid residues, and wherein n is an integral number 1, and m is an integral number 2, and (C) 0 to 10 wt. % of at least one additive.
Claims
1. A preparation containing or consisting of: (A) 30 to 90 wt. % of at least one organic solvent, (B) 10 to 70 wt. % of at least one noble metal complex comprising diolefin and C6-C18 monocarboxylate ligands selected from the group consisting of noble metal complexes of the type [LPd[O(CO)R1]X].sub.n, [LRh[O(CO)R1]].sub.m and [LIr[O(CO)R1]].sub.m, wherein L represents a compound acting as diolefin ligand, wherein X is selected among bromide, chloride, iodide, and —O(CO)R2, wherein —O(CO)R1 and —O(CO)R2 represent identical or different non-aromatic C6-C18 monocarboxylic acid residues, and wherein n is an integral number ≥1, and m is an integral number ≥2, and (C) 0 to 10 wt. % of at least one additive.
2. The preparation according to claim 1, wherein integral n>1 and integral m lies in the range of 2 to 5.
3. The preparation according to claim 1 in the form of a non-colloidal organic solution.
4. The preparation according to claim 1 comprising a noble metal content originating from the at least one mobile metal complex in the range of 2.5 to 25 wt. %.
5. The preparation according to claim 1, wherein the at least one noble metal complex is selected among noble metal complexes of the type [(COD)Pd[O(CO)R1].sub.2].sub.n, [(NBD)Pd[O(CO)R1].sub.2].sub.n, [(COD)Rh[O(CO)R1]].sub.m, [(NBD)Rh[O(CO)R1]].sub.m, [(COD)Ir[O(CO)R1]].sub.m, and [(NBD)Ir[O(CO)R1]].sub.m, wherein n is equal to 1 or 2, wherein m is equal to 2, and wherein R1 stands for a non-aromatic C5-C17 hydrocarbon residue.
6. The preparation according to claim 1, wherein the decomposition temperature of the at least one noble metal complex lies in the range of 150 to 200° C. or of 150 to 250° C.
7. The preparation according to claim 1, wherein the at least one additive (C) is selected from the group consisting of wetting additives, rheology additives, defoamers, deaerators, additives for influencing the surface tension, and odorants.
8. A method for the production of a noble metal-comprising layer on a substrate, comprising the steps of: (1) application of a covering layer of a preparation according to claim 1, and (2) thermal decomposition of the covering layer by forming the noble metal-comprising layer.
9. The method according to claim 8, wherein the substrate comprises one or several materials selected from the group consisting of glass, carbide substrates, nitride substrates, boride substrates, ceramic substrates, semiconductor substrates, metal, plastics, modified or unmodified polymers of natural origin, carbon substrates, wood, cardboard and paper.
10. The method according to claim 8, wherein the substrate is provided with the coating layer on inner and/or outer surfaces and/or on inner and/or outer surface portions.
11. The method according to claim 8, wherein the application method used for the production of the covering layer is selected from the group consisting of immersion, spray application, printing, application by means of paint brush, application by means of brush, application by means of felt, and application by means of cloth.
12. The method according to claim 8, wherein the covering layer applied in step (1) is initially dried and is thereby partially or completely freed from the organic solvent (A), before it is subjected to the thermal decomposition in step (2).
13. The method according to claim 8, wherein the thermal decomposition according to step (2) takes place by means of thermal treatment, which comprises a heating to an object temperature above the decomposition temperature of the at least one noble metal complex.
14. The method according to claim 8, wherein the noble metal-comprising layer has a thickness of 50 nm to 5 μm.
15. The method according to claim 8, wherein the noble metal-comprising layer is a layer comprising metallic palladium, rhodium oxide, or iridium oxide or consisting thereof.
Description
EXAMPLES
Example 1 (Equipping of a Polyimide Film with a Palladium Layer):
[0059] A solution of 35 mmol (COD)PdCl.sub.2 in 200 ml of dichloromethane was stirred, and a solution of 140 mmol of sodium-2-ethylhexanoate in 150 ml of water was added. The two-phase mixture was emulsified for 24 h at 20° C. by means of intensive stirring. The dichloromethane phase turned yellow thereby.
[0060] The dichloromethane phase was separated, and the solvent was distilled off. The viscous, yellow residue was received in petroleum benzine (40-60) and the solution was dried and filtered with magnesium sulphate. The petroleum benzine was then distilled off completely. What remained was a viscous yellow residue of (COD)Pd[O(CO)CH(C.sub.2H.sub.5)C.sub.4H.sub.9].sub.2.
[0061] 5 g of the yellow residue were dissolved in 5.60 g of a solvent mixture (50 wt. % of ethanol, 50 wt. % of propylene glycol monopropylether). This solution was sprayed onto a Kapton® film (polyimide) by means of an airbrush spray gun. The coated film was heated to an object temperature of 200° C. in a laboratory furnace and was kept at this temperature for 5 minutes. A glossy electrically conductive layer of palladium had formed on the film.
Example 2 (Equipping of a Polyimide Film with a Patterned Palladium Layer):
[0062] A Kapton® film was imprinted with the solution from Example 1 with the help of an inkjet printer at a resolution of 1270 dpi in a meander design. The film imprinted in this way was heated to an object temperature of 200° C. in a laboratory furnace and was kept at this temperature for 5 minutes. A glossy electrically conductive layer of palladium in the form of the meander design with a width of the conductor paths of 2.5 mm had formed on the film.
Example 3 (Equipping of a Polyimide Film with a Palladium Layer):
[0063] Example 1 was repeated completely analogously with the sole difference that (NBD)PdCl.sub.2 was used instead of (COD)PdCl.sub.2, so that a yellow residue of (NBD)Pd[O(CO)CH(C.sub.2H.sub.5)C.sub.4H.sub.9].sub.2 and finally a polyimide film, which was provided with a palladium layer and which corresponded to the coated film obtained in Example 1, was obtained as result of the synthesis.
Example 4 (Equipping of a Polyimide Film with a Patterned Palladium Layer):
[0064] Example 2 was repeated completely analogously, with the sole difference that (NBD)PdCl.sub.2 was used instead of (COD)PdCl.sub.2, so that a yellow residue of (NBD)Pd[O(CO)CH(C.sub.2H.sub.5)C.sub.4H.sub.9].sub.2 and finally a polyimide film, which was provided with a patterned palladium layer and which corresponded to the film obtained in Example 2, which was provided with a patterned palladium layer, was obtained as result of the synthesis.
Example 5 (Equipping of a Polyimide Film with a Rhodium Oxide Layer):
[0065] A solution of 16.3 mmol [(COD)RhCl].sub.2 in 200 ml of dichloromethane was stirred, and a solution of 65.3 mmol of sodium-2-ethylhexanoate in 100 ml of water was added. The two-phase mixture was emulsified for 24 h at 20° C. by intensive stirring. The dichloromethane phase turned yellow thereby.
[0066] The dichloromethane phase was separated, and the solvent was distilled off. The viscous, yellow residue was received in petroleum benzine (40-60) and the solution was dried and filtered with magnesium sulphate. The petroleum benzine was then distilled off completely. What remained was a viscous yellow residue of
[(COD)Rh[O(CO)CH(C.sub.2H.sub.5)C.sub.4H.sub.9]].sub.m.
[0067] 5 g of the yellow residue were dissolved in 5 g of petroleum benzine. This solution was sprayed onto a Kapton® film by means of an airbrush spray gun. The coated film was heated to an object temperature of 250° C. in a laboratory furnace and was kept at this temperature for 3 minutes. A matte layer of essentially rhodium oxide had formed on the film.
Example 6 (Equipping of a Polyimide Film with a Patterned Rhodium Oxide Layer):
[0068] A Kapton® film was imprinted with the solution from Example 5 with the help of an inkjet printer at a resolution of 1270 dpi in a meander design. The film imprinted in this way was heated to an object temperature of 250° C. in a laboratory furnace and was kept at this temperature for 5 minutes. A matte layer of essentially rhodium oxide in the form of the meander design with a width of the conductor paths of 2.5 mm had formed on the film.
Example 7 (Equipping of a Polyimide Film with a Rhodium Oxide Layer):
[0069] Example 5 was repeated completely analogously, with the sole difference that [(NBD)RhCl].sub.2 was used instead of [(COD)RhCl].sub.2, so that a yellow residue of [(NBD)Rh[O(CO)CH(C.sub.2H.sub.5)C.sub.4H.sub.9]].sub.m and finally a polyimide film, which was provided with a matte layer of essentially rhodium oxide and which corresponded to the coated film obtained in Example 5, was obtained as result of the synthesis.
Example 8 (Equipping of a Polyimide Film with a Patterned Rhodium Oxide Layer):
[0070] Example 6 was repeated completely analogously, with the sole difference that [(NBD)RhCl].sub.2 was used instead of [(COD)RhCl].sub.2, so that a yellow residue of [(NBD)Rh[O(CO)CH(C.sub.2H.sub.5)C.sub.4H.sub.9]].sub.m and finally a polyimide film, which was provided with a patterned layer of essentially rhodium oxide and which corresponded to the film obtained in Example 6, which was provided with a patterned layer of essentially rhodium oxide, was obtained as result of the synthesis.
Example 9 (Equipping a Polyimide Film with an Iridium Oxide Layer):
[0071] A solution of 16.3 mmol [(COD)IrCl].sub.2 in 200 ml of dichloromethane was stirred, and a solution of 65.3 mmol of sodium neodecanoate in 100 ml of water was added. The two-phase mixture was emulsified for 24 h at 20° C. by intensive stirring. The dichloromethane phase turned yellow thereby.
[0072] The dichloromethane phase was separated, and the solvent was distilled off. The viscous, yellow residue was received in petroleum benzine (40-60) and the solution was dried and filtered with magnesium sulphate. The petroleum benzine was then completely distilled off. What remained was a viscous yellow residue of
[(COD)Ir[O(CO)(CH.sub.2).sub.5C(CH.sub.3).sub.3]].sub.m.
[0073] 5 g of the yellow residue were dissolved in 5 g of petroleum benzine. This solution was sprayed onto a Kapton® film by means of an airbrush spray gun. The coated film was heated to an object temperature of 250° C. in a laboratory furnace and was kept at this temperature for 3 minutes. A matte layer of essentially iridium oxide had formed on the film.
Example 10 (Equipping of a Polyimide Film with a Patterned Iridium Oxide Layer):
[0074] A Kapton® film was imprinted with the solution from Example 9 with the help of an inkjet printer at a resolution of 1270 dpi in a meander design. The film imprinted in this way was heated to an object temperature of 250° C. in a laboratory furnace and was kept at this temperature for 5 minutes. A matte layer of essentially iridium oxide in the form of the meander design with a width of the conductor paths of 2.5 mm had formed on the film.