METHOD OF PREPARING ALUMINUM-CONTAINING ALLOY POWDER AND APPLICATION THEREOF
20230001481 · 2023-01-05
Inventors
Cpc classification
B33Y70/00
PERFORMING OPERATIONS; TRANSPORTING
C22C1/0458
CHEMISTRY; METALLURGY
B22F2998/10
PERFORMING OPERATIONS; TRANSPORTING
C22C33/0278
CHEMISTRY; METALLURGY
B22F2998/10
PERFORMING OPERATIONS; TRANSPORTING
Y02P10/25
GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
B22F1/05
PERFORMING OPERATIONS; TRANSPORTING
International classification
B33Y70/00
PERFORMING OPERATIONS; TRANSPORTING
Abstract
The present disclosure relates to a method of preparing an aluminum-containing alloy powder and an application thereof. The preparation method includes: by using the characteristic that a solidification structure of an initial alloy includes a matrix phase and a dispersed particle phase, the matrix phase is removed by reaction with an acid solution, so as to separate out the dispersed particle phase and obtain an aluminum-containing alloy powder. The preparation method is simple in process and can prepare different morphologies of aluminum-containing alloy powders of nano-level, sub-micron-level, micron-level and millimeter-level, which can be applied to the fields such as photo-electronic devices, wave absorbing materials, catalysts, 3D metal printing, metal injection molding and corrosion-resistant coating.
Claims
1. A preparation method containing aluminum alloy powder, is characterized in that, comprises the following steps: Step 1, select the initial alloy raw material, and melt the initial alloy raw material according to the initial alloy composition ratio to obtain a uniform initial alloy melt; the main component of the initial alloy melt is REaAlbMcTd; wherein, RE includes Y, La, Ce, At least one of Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, M includes W, Cr, Mo, V, Ta, Nb, Zr, Hf, Ti, at least one of Fe, Co, Ni; T is an impurity element and contains at least one of O, H, N, P, S, F, Cl; a, b, c, d represent the corresponding constituent elements respectively Atomic percentage content, and 35%≤a≤99.7%, 0.1%≤b≤25%, 0.1%≤c≤35%, 0≤d≤10%; Step 2, solidify the initial alloy melt into initial alloy strips; the solidified structure of the initial alloy strips includes a matrix phase and a dispersed particle phase; the melting point of the matrix phase is lower than that of the dispersed particle phase, and the dispersed particles The phase is coated in the matrix phase; the average composition of the matrix phase is mainly REx1Aly1Tz1, the composition of the dispersed particle phase is mainly Mx2Aly2Tz2, x1, y1, z1, x2, y2, z2 represent the corresponding constituent elements, respectively. Atomic percentage content, and 68%≤x1<99.8%, 0.2%≤y1≤30%, 0≤z1≤30%; 77%≤x2≤99.8%, 0.1%≤y2≤22%, 0≤z2≤1.5%, z2≤d≤z1; during the solidification of the initial alloy melt, the impurity element T in the initial alloy melt is redistributed in the dispersed particle phase and the matrix phase, and is enriched in the matrix phase, so that the The disperse particle phase is purified; In step 3, the initial alloy strip is reacted with the acid solution, the matrix phase in the initial alloy strip reacts with the acid to become ions entering the solution, and the dispersed particle phase that does not react with the acid solution is removed from the initial alloy. The strip is separated out to obtain an aluminum alloy-containing powder material whose main component is Mx2Aly2Tz2.
2. The method for preparing an aluminum alloy-containing powder according to claim 1, wherein the source of impurity elements in the initial alloy melt includes: impurities introduced from the initial alloy raw material, and impurities introduced from the atmosphere or the crucible during the smelting process.
3. The method for preparing an aluminum alloy-containing powder according to claim 1, wherein the particle size range of the dispersed particle phase is 2 nm to 3 mm.
4. The method for preparing an aluminum alloy-containing powder according to claim 1, wherein the number of single crystal particles of the dispersed particles in the initial alloy strip accounts for not less than 75% of the total number of dispersed particles.
5. The method for preparing an aluminum alloy-containing powder according to claim 1, wherein y1>y2.
6. The method for preparing an aluminum alloy-containing powder according to claim 1, wherein z2≤d≤z1, and 2z2≤z1.
7. The method for preparing an aluminum alloy-containing powder according to claim 1, wherein the particle size of the aluminum alloy-containing powder material ranges from 2 nm to 3 mm.
8. The method for preparing an aluminum alloy-containing powder according to claim 1, wherein the following step is further performed after the step 3: after sieving the aluminum alloy-containing powder material, a particle size range of 5 μm is selected. ˜200 μm aluminum alloy-containing powder material is subjected to plasma spheroidization to obtain spherical aluminum alloy-containing powder.
9. An application of the aluminum alloy-containing powder or spherical aluminum-alloy-containing powder according to claim 1 in optoelectronic devices, wave absorbing materials, catalysts, powder metallurgy, 3D metal printing, metal injection molding, and coatings.
10. An alloy strip is characterized in that it includes endogenous aluminum alloy powder and a coating body; the solidification structure of the alloy strip includes a matrix phase and a dispersed particle phase, and the matrix phase is the coating body, and the dispersed particle phase is the is the endogenous aluminum alloy powder; the melting point of the coating body is lower than the endogenous aluminum alloy powder, and the endogenous aluminum alloy powder is coated in the coating body; the coating The average composition of the coating is mainly REx1Aly1Tz1, the main composition of the endogenous aluminum alloy powder is Mx2Aly2Tz2, x1, y1, z1, x2, y2, z2 respectively represent the atomic percentage content of the corresponding constituent elements, and 60%≤x1<99.8%, 0.2%≤y1≤30%, 0≤z1≤30%; 80%≤x2≤99.8%, 0.1%≤y2≤22%, 0≤z2≤1.5%, z2≤z1, y1<y2; The RE includes at least one of Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, and M includes W, Cr, Mo, V, At least one of Ta, Nb, Zr, Hf, Ti, Fe, Co, and Ni; T is an impurity element and includes at least one of O, H, N, P, S, F, and Cl.
11. A preparation method containing aluminum alloy powder, is characterized in that, comprises: An initial alloy is provided, the composition of the initial alloy is REaAlbMc, wherein RE is selected from Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu At least one of, M is selected from at least one of W, Cr, Mo, V, Ta, Nb, Zr, Hf, Ti, a, b, c respectively represent the atomic percentage content of the corresponding constituent elements, and 0.1%≤b≤25%, 0.1%≤c≤35%, a+b+c=100%, the solidified structure of the initial alloy includes a matrix phase and a dispersed particle phase, the average composition of the matrix phase is REx1Aly1, the dispersion The composition of the particle phase is Mx2Aly2, x1, y1, x2, and y2 represent the atomic percentage content of the corresponding constituent elements respectively, and 0.5%≤y1≤30%, 0.1%≤y2≤25%, x1+y1=100%, x2+y2=100%; An acid solution is provided, and the initial alloy is mixed with the acid solution, so that the matrix phase in the initial alloy reacts with the acid solution to become metal ions, and the dispersed particle phase in the initial alloy is detached to obtain a mixture containing Aluminum alloy powder, the composition of the aluminum alloy powder-containing powder is Mx2Aly2.
12. The method for preparing an aluminum alloy-containing powder according to claim 11, wherein the initial alloy is obtained by the following method: Weigh the raw materials according to the proportion; Fully melting the raw material to obtain an alloy melt; The initial alloy is obtained by solidifying the alloy melt, wherein the solidification rate is 0.001 K/s.sup.18 107 K/s.
13. The method for preparing an aluminum alloy-containing powder according to claim 11, wherein y1>y2.
14. The method for preparing an aluminum alloy-containing powder according to claim 11, wherein the particle shape of the dispersed particle phase comprises at least one of a dendritic shape, a spherical shape, a near-spherical shape, a square shape, a pie shape, and a rod shape, and the particle size of the dispersed particle phase is 2 nm to 50 mm.
15. The method for preparing an aluminum alloy-containing powder according to claim 11, wherein the acid in the acid solution comprises at least one of sulfuric acid, hydrochloric acid, nitric acid, perchloric acid, phosphoric acid, acetic acid, oxalic acid, formic acid, and carbonic acid One, and the molar concentration of the acid is 0.001 mol/L to 20 mol/L.
16. The method for preparing an aluminum alloy-containing powder according to claim 11, wherein the reaction temperature of the matrix phase and the acid solution is 0° C. to 100° C., and the time is 0.1 min to 24 hours.
17. The method for preparing an aluminum alloy-containing powder according to claim 11, characterized in that, after the step of reacting the matrix phase with the acid solution, the following step is further performed: sieving the separated prefabricated powder, respectively Plasma spheroidizing treatment is performed to obtain aluminum alloy-containing powders with different particle sizes and spherical shapes; Contains aluminum alloy powder.
18. An application of the aluminum alloy-containing powder obtained by the preparation method according to claim 11 in 3D metal printing, wherein the particle size of the aluminum alloy-containing powder is 0.5 μm to 1 mm.
19. An application of the aluminum alloy-containing powder obtained by the preparation method according to claim 11 in metal injection molding, wherein the particle size of the aluminum alloy-containing powder is 0.1 μm to 50 μm.
20. An application of the aluminum alloy-containing powder obtained by the preparation method according to claim 11 in an anti-corrosion coating, wherein the particle size of the aluminum alloy-containing powder is 2 nm to 5 μm.
Description
BRIEF DESCRIPTIONS OF THE DRAWINGS
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[0133]
[0134]
[0135]
[0136]
DETAILED DESCRIPTIONS OF EMBODIMENTS
[0137] A method of preparing an aluminum-containing alloy powder and an application thereof according the present disclosure will be further described below in combination with the accompanying drawings.
EXAMPLE 1
[0138] The example provides a method of preparing a micron-level Ti—V—Cr—Mo—Zr—Al alloy powder. The preparation method includes the following steps.
[0139] (1) Raw materials were weighed according to the formulation of Gd.sub.76A.sub.18(Ti.sub.82V.sub.8Cr.sub.6Mo.sub.2Zr.sub.2).sub.16 alloy (atomic percent), and then subjected to arc melting to obtain a Gd.sub.76Al.sub.8(Ti.sub.82V.sub.8Cr.sub.6Mo.sub.2Zr.sub.2).sub.16 master alloy. The master alloy was reheated and melted into an alloy melt by induction melting, and the alloy melt was prepared into a Gd.sub.76Al.sub.8(Ti.sub.82V.sub.8Cr.sub.6Mo.sub.2Zr.sub.2).sub.16 alloy sheet with a thickness of 1 mm to 20 mm at the solidification rate of 10 K/s to 1000 K/s. The solidification structure of the alloy sheet was formed by a matrix phase with an average ingredient about being Gd.sub.91.5Al.sub.8.5 and a dispersed dendritic particle phase with an ingredient being (Ti.sub.82V.sub.8Cr.sub.6Mo.sub.2Zr.sub.2).sub.94.5Al5.5, and the particle size of the dispersed particle phase was in a range of 1 μm to 200 μm.
[0140] (2) At room temperature, 1 g of Gd.sub.76Al.sub.8(Ti.sub.82V.sub.8Cr.sub.6Mo.sub.2Zr.sub.2).sub.16 alloy sheet prepared at step (1) was added to 150 ml of sulfuric acid aqueous solution with a concentration of 0.25 mol/L for reaction. During the reaction, the matrix phase with an average ingredient about being Gd.sub.91.5Al.sub.8.5 reacted with an acid to change into an ion entering the solution, whereas the micron-level (Ti.sub.82V.sub.8Cr.sub.6Mo.sub.2Zr.sub.2).sub.94.5Al.sub.5.5 dispersed dendritic particle phase difficult to react with the acid was gradually separated from the matrix phase in a dispersion manner. After 20 min, the obtained (Ti.sub.82V.sub.8Cr.sub.6Mo.sub.2Zr.sub.2).sub.94.5Al.sub.5.5 micron-level particles were separated from the solution, and cleaned and dried to obtain a micron-level (Ti.sub.82V.sub.8Cr.sub.6Mo.sub.2Zr.sub.2).sub.94.5Al.sub.5.5 alloy powder, with an average size of a single (Ti.sub.82V.sub.8Cr.sub.6Mo.sub.2Zr.sub.2).sub.94.5Al.sub.5.5 particle being in a range of 1 μm to 200 μm.
EXAMPLE 2
[0141] This example provides a method of preparing a micron-level Ti—Mo—Zr—Al alloy powder. The preparation method includes the following steps.
[0142] (1) Raw materials were weighed according to the formulation of Ce.sub.76Al.sub.8(Ti.sub.98Mo.sub.1Zr.sub.1).sub.16 alloy (atomic percent), and then subjected to arc melting to obtain a Ce.sub.76Al.sub.8(Ti.sub.98Mo.sub.1Zr.sub.1).sub.16 master alloy. The master alloy was reheated and melted into an alloy melt by induction melting, and the alloy melt was prepared into a Ce.sub.76Al.sub.8(Ti.sub.98Mo.sub.1Zr.sub.1).sub.16 alloy sheet with a thickness of 1 mm to 20 mm at the solidification rate of 10 K/s to 1000 K/s. The solidification structure of the alloy sheet was formed by a matrix phase with an average ingredient about being Ce91.5Al8.5 and a dispersed dendritic particle phase with an ingredient being (Ti.sub.98Mo.sub.1Zr.sub.1).sub.94.5Al.sub.5.5, and the particle size of the dispersed particle phase was in a range of 1 μm to 200 μm.
[0143] (2) At room temperature, 1 g of Ce.sub.76Al.sub.8(Ti.sub.98Mo.sub.1Zr.sub.1).sub.16 alloy sheet prepared at step (1) was added to 200 ml of hydrochloric acid aqueous solution with a concentration of 0.4 mol/L for reaction. During the reaction, the matrix phase with an average ingredient of about Ce91.5Al8.5 reacted with an acid to change into an ion entering the solution, whereas the micron-level (Ti.sub.98Mo.sub.1Zr.sub.1).sub.94.5Al.sub.5.5 dispersed dendritic particle phase difficult to react with the acid was gradually separated from the matrix phase in a dispersion manner. After 20 min, the obtained (Ti.sub.98Mo.sub.1Zr.sub.1).sub.94.5Al.sub.5.5 micron-level particles were separated from the solution, and cleaned and dried to obtain a micron-level (Ti.sub.98Mo.sub.1Zr.sub.1).sub.94.5Al.sub.5.5 alloy powder, with an average size of a single (Ti.sub.98Mo.sub.1Zr.sub.1).sub.94.5Al.sub.5.5 particle being in a range of 1 μm to 200 μm.
EXAMPLE 3
[0144] This example provides a method of preparing a nano-level Ti—Cr—Al alloy powder. The preparation method includes the following steps.
[0145] (1) Raw materials were weighed according to the formulation of Ce.sub.72Al.sub.12(Ti.sub.97.5Cr.sub.2.5).sub.16 alloy (atomic percent), and then subjected to induction melting to obtain a molten Ce.sub.72Al.sub.12(Ti.sub.97.5Cr.sub.2.5).sub.16 alloy melt. The alloy melt was prepared into a Ce.sub.72Al.sub.12(Ti.sub.97.5Cr.sub.2.5).sub.16 alloy ribbon with a thickness of 20 μm to 100 μm by using copper roller spinning at the rate of ˜10.sup.5 K/s. The solidification structure of the alloy ribbon was formed by a matrix phase with an average ingredient about being Ce.sub.87Al.sub.13 and a dispersed particle phase with an ingredient being (Ti.sub.97.5Cr.sub.2.5).sub.91.5Al.sub.8.5, and the dispersed particle phase had a particle size of 10 nm to 200 nm and was shaped like sub-spheroid.
[0146] (2) At room temperature, 1 g of Ce.sub.72Al.sub.12(Ti.sub.97.5Cr.sub.2.5).sub.16 alloy ribbon prepared at step (1) was added to 150 ml of hydrochloric acid aqueous solution with a concentration of 0.4 mol/L for reaction. During the reaction, the matrix phase with an average ingredient about being Ce.sub.87Al.sub.13 reacted with an acid to change into an ion entering the solution, whereas the nano-level (Ti.sub.97.5Cr.sub.2.5).sub.91.5Al.sub.8.5 dispersed particle phase difficult to react with the acid was gradually separated from the matrix phase in a dispersion manner. After 10 min, the obtained (Ti.sub.97.5Cr.sub.2.5).sub.91.5Al.sub.8.5 nano-level particles were separated from the solution, and cleaned and dried to obtain a nano-level (Ti.sub.97.5Cr.sub.2.5).sub.91.5Al.sub.8.5 alloy powder, with an average size of a single (Ti.sub.97.5Cr.sub.2.5).sub.91.5Al.sub.8.5 particle being in a range of 10 nm˜200 nm.
EXAMPLE 4
[0147] This example provides a method of preparing a micron-level Ti—Nb—Al alloy powder. The preparation method includes the following steps.
[0148] (1) Raw materials were weighed according to the formulation of Ce.sub.68Al.sub.14(Ti.sub.96Nb.sub.4).sub.18 alloy (atomic percent), and then subjected to induction melting to obtain a molten Ce.sub.68Al.sub.14(Ti.sub.96Nb.sub.4).sub.18 alloy melt. The alloy melt was prepared into a Ce.sub.68Al.sub.14(Ti.sub.96Nb.sub.4).sub.18 alloy sheet with a thickness of 1 mm to 20 mm at the solidification rate of 10 K/s to 1000 K/s. The solidification structure of the alloy sheet was formed by a matrix phase with an average ingredient about being Ce.sub.85Al.sub.15 and a dispersed dendritic particle phase with an ingredient being (Ti.sub.96Cr.sub.4).sub.90Al.sub.10, and the particle size of the dispersed particle phase was 1 μm to 200 μm.
[0149] (2) At room temperature, 1 g of Ce.sub.68Al.sub.14(Ti.sub.96Nb.sub.4).sub.18 alloy sheet prepared at step (1) was added to 200 ml of hydrochloric acid aqueous solution with a concentration of 0.5 mol/L for reaction. During the reaction, the matrix phase with an average ingredient being Ce.sub.85Al.sub.15 reacted with an acid to change into an ion entering the solution, whereas the micron-level (Ti.sub.96Nb.sub.4).sub.90Al.sub.10 dispersed dendritic particle phase difficult to react with the acid was gradually separated from the matrix phase in a dispersion manner. After 20 min, the obtained (Ti.sub.96Nb.sub.4).sub.90Al.sub.10 micron-level dendritic particles were separated from the solution, and cleaned and dried to obtain a micron-level (Ti.sub.96Nb.sub.4).sub.90Al.sub.10 alloy powder, with an average size of a single (Ti.sub.96Nb.sub.4).sub.90Al.sub.10 particle being in a range of 1 μm to 200 μm.
EXAMPLE 5
[0150] This example provides a method of preparing a nano-level Ti—V—Al alloy powder. The preparation method includes the following steps.
[0151] (1) Raw materials were weighed according to the formulation of Ce.sub.72Al.sub.10(Ti.sub.96V.sub.4).sub.18 alloy (atomic percent), and then subjected to induction melting to obtain a molten Ce.sub.72Al.sub.10(Ti.sub.96V.sub.4).sub.18 alloy melt. The alloy melt was prepared into a Ce.sub.72Al.sub.10(Ti.sub.96V.sub.4).sub.18 alloy ribbon with a thickness of 20 μm to 100 μm by using copper roller spinning at the rate of ˜10.sup.5 K/s. The solidification structure of the alloy ribbon was formed by a matrix phase with an average ingredient being Ce.sub.88.5Al.sub.11.5 and a dispersed particle phase with an ingredient being (Ti.sub.96V.sub.4).sub.92.5Al.sub.7.5, and the dispersed particle phase had a particle size of 10 nm to 300 nm and was shaped like sub-spheroid.
[0152] (2) At room temperature, 1 g of Ce.sub.72Al.sub.10(Ti.sub.96V.sub.4).sub.18 alloy ribbon prepared at step (1) was added to 200 ml of hydrochloric acid aqueous solution with a concentration of 0.5 mol/L for reaction. During the reaction, the matrix phase with an average ingredient being Ce.sub.88.5Al.sub.11.5 reacted with an acid to change into an ion entering the solution, whereas the nano-level (Ti.sub.96V.sub.4).sub.92.5Al.sub.7.5 dispersed particle phase difficult to react with the acid was gradually separated from the matrix phase in a dispersion manner. After 10 min, the obtained (Ti.sub.96V.sub.4).sub.92.5Al.sub.7.5 nano-level particles were separated from the solution, and cleaned and dried to obtain a nano-level (Ti.sub.96V.sub.4).sub.92.5Al.sub.7.5 alloy powder, with an average size of a single (Ti.sub.96V.sub.4).sub.92.5Al.sub.7.5 particle being in a range of 10 nm to 300 nm. As shown in
EXAMPLE 6
[0153] This example provides a method of preparing a nano-level Ti—V—Al alloy powder. The preparation method includes the following steps:
[0154] (1) Raw materials were weighed according to the formulation of Ce.sub.68Al.sub.14(Ti.sub.96V.sub.4).sub.18 alloy (atomic percent), and then subjected to induction melting to obtain a molten Ce.sub.68Al.sub.14(Ti.sub.96V.sub.4).sub.18 alloy melt. The alloy melt was prepared into a Ce.sub.68Al.sub.14(Ti.sub.96V.sub.4).sub.18 alloy ribbon with a thickness of 20 μm to 100 μm by using copper roller spinning at the rate of ˜10.sup.5 K/s. The solidification structure of the alloy ribbon was formed by a matrix phase with an average ingredient being Ce.sub.85Al.sub.15 and a dispersed particle phase with an ingredient being (Ti.sub.96V.sub.4).sub.90Al.sub.10, and the dispersed particle phase had a particle size of 10 nm to 300 nm and was shaped like sub-spheroid.
[0155] (2) At room temperature, 1 g Ce.sub.68Al.sub.14(Ti.sub.96Nb.sub.4).sub.18 alloy ribbon prepared at step (1) was added to 200 ml of hydrochloric acid aqueous solution with a concentration of 0.5 mol/L for reaction. During the reaction, the matrix phase with an average ingredient being Ce.sub.85Al.sub.15 reacted with an acid to change into an ion entering the solution, whereas the nano-level (Ti.sub.96V.sub.4).sub.90Al.sub.10 dispersed particle phase difficult to react with the acid was gradually separated from the matrix phase in a dispersion manner. After 10 min, the obtained (Ti.sub.96V.sub.4).sub.90Al.sub.10 nano-level particles were separated from the solution, and cleaned and dried to obtain a nano-level (Ti.sub.96V.sub.4).sub.90Al.sub.10 alloy powder shown in
EXAMPLE 7
[0156] This example provides a method of preparing a sub-micron-level Ti—V—Al alloy powder. The preparation method includes the following steps.
[0157] (1) Raw materials were weighed according to the formulation of (La.sub.50Ce.sub.50).sub.68Al.sub.14(Ti.sub.96V.sub.4).sub.18 alloy (atomic percent), and then subjected to induction melting to obtain a molten (La.sub.50Ce.sub.50).sub.68Al.sub.14(Ti.sub.96V.sub.4).sub.18 alloy melt. The alloy melt was prepared into a (La.sub.50Ce.sub.50).sub.68 (Ti.sub.96V.sub.4).sub.18 alloy ribbon with a thickness of 100 μm to 2 mm by using copper roller spinning at the solidification rate of about 10.sup.3 to 10.sup.4 K/s. The solidification structure of the alloy ribbon was formed by a matrix phase with an average ingredient being (La.sub.50Ce.sub.50).sub.85Al.sub.15 and a dispersed particle phase with an ingredient being (Ti.sub.96V.sub.4).sub.90Al.sub.10, and the dispersed particle phase had a particle size of 100 nm to 1.5 μm.
[0158] (2) At room temperature, 1 g of (La.sub.50Ce.sub.50).sub.68Al.sub.14(Ti.sub.96V.sub.4).sub.18 alloy ribbon prepared at step (1) was added to 200 ml of sulfuric acid aqueous solution with a concentration of 0.4 mol/L for reaction. During the reaction, the matrix phase with an average ingredient being (La.sub.50Ce.sub.50).sub.85Al.sub.15 reacted with an acid to change into an ion entering the solution, whereas the sub-micron-level (Ti.sub.96V.sub.4).sub.90Al.sub.10 dispersed particle phase difficult to react with the acid was gradually separated from the matrix phase in a dispersion manner. After 10 min, the obtained (Ti.sub.96V.sub.4).sub.90Al.sub.10 sub-micron-level particles were separated from the solution, and cleaned and dried to obtain a sub-micron-level (Ti.sub.96V.sub.4).sub.90Al.sub.10 alloy powder shown in
EXAMPLE 8
[0159] This example provides a method of preparing a micron-level Ti—V—Al alloy powder. The preparation method includes the following steps.
[0160] (1) Raw materials were weighed according to the formulation of Ce.sub.68Al.sub.14(Ti.sub.96V.sub.4).sub.18 alloy (atomic percent), and then subjected to induction melting to obtain a molten Ce.sub.68Al.sub.14(Ti.sub.96V.sub.4).sub.18 alloy melt. The alloy melt was prepared into a Ce.sub.68Al.sub.14(Ti.sub.96V.sub.4).sub.18 alloy sheet with a thickness of 2 mm to 6 mm at the solidification rate of 50 K/s to 500 K/s. The solidification structure of the alloy sheet was formed by a matrix phase with an average ingredient being Ce.sub.85Al.sub.15 and a dispersed dendritic particle phase with an ingredient being (Ti.sub.96V.sub.4).sub.90Al.sub.10, and the particle size of the dispersed particle phase was 5 μm to 100 μm.
[0161] (2) At room temperature, 1 g of Ce.sub.68Al.sub.14(Ti.sub.96V.sub.4).sub.18 alloy sheet prepared at step (1) was added to 200 ml of hydrochloric acid aqueous solution with a concentration of 0.5 mol/L for reaction. During the reaction, the matrix phase with an average ingredient being Ce.sub.85Al.sub.15 reacted with an acid to change into an ion entering the solution, whereas the micron-level (Ti.sub.96V.sub.4).sub.90Al.sub.10 dispersed dendritic particle phase difficult to react with the acid was gradually separated from the matrix phase in a dispersion manner. After 20 min, the obtained (Ti.sub.96V.sub.4).sub.90Al.sub.10 micron-level dendritic particles were separated from the solution, and cleaned and dried to obtain a micron-level (Ti.sub.96V.sub.4).sub.90Al.sub.10 alloy powder as shown in
EXAMPLE 9
[0162] This example provides a method of preparing a spheroidal micron-level Ti—V—Al alloy powder. The preparation method includes the following steps.
[0163] (1) Raw materials were weighed according to the formulation of Ce.sub.68Al.sub.14(Ti.sub.96V.sub.4).sub.18 alloy (atomic percent), and then subjected to induction melting to obtain a molten Ce.sub.68Al.sub.14(Ti.sub.96V.sub.4).sub.18 alloy melt. The alloy melt was prepared into a Ce.sub.68Al.sub.14(Ti.sub.96V.sub.4).sub.18 alloy sheet with a thickness of 1 mm to 20 mm at the solidification rate of 10 K/s to 1000 K/s. The solidification structure of the alloy sheet was formed by a matrix phase with an average ingredient being Ce.sub.85Al.sub.15 and a dispersed dendritic particle phase with an ingredient being (Ti.sub.96V.sub.4).sub.90Al.sub.10, and the particle size of the dispersed particle phase was 1 μm to 200 μm.
[0164] (2) At room temperature, 1 g of Ce.sub.68Al.sub.14(Ti.sub.96V.sub.4).sub.18 alloy sheet prepared at step (1) was added to 200 ml of hydrochloric acid aqueous solution with a concentration of 0.5 mol/L for reaction. During the reaction, the matrix phase with an average ingredient being Ce.sub.85Al.sub.15 reacted with an acid to change into an ion entering the solution, whereas the micron-level (Ti.sub.96V.sub.4).sub.90Al.sub.10 dispersed dendritic particle phase difficult to react with the acid was gradually separated from the matrix phase in a dispersion manner. After 20 min, the obtained (Ti.sub.96V.sub.4).sub.90Al.sub.10 micron-level particles were separated from the solution, and cleaned and dried to obtain a micron-level (Ti.sub.96V.sub.4).sub.90Al.sub.10 alloy powder, with an average size of a single (Ti.sub.96V.sub.4).sub.90Al.sub.10 particle being in a range of 1 μm to 200 μm.
[0165] (3) 0.5 kg of micron-level (Ti.sub.96V.sub.4).sub.90Al.sub.10 alloy powder prepared at step (2) was collected and then screened through 100 meshes, 270 meshes, 1000 meshes, 2000 meshes and 8000 meshes to obtain graded (Ti.sub.96V.sub.4).sub.90Al.sub.10 alloy powders with a range of a dendritic particle size being >150 μm, 150 μm to 53 μm, 53 μm to 13 μm, 13 μm to 6.5 μm, 6.5 μm to 1.6 μm and less than 1.6 μm respectively. The (Ti.sub.96V.sub.4).sub.90Al.sub.10 alloy powders with a range of a dendritic particle size being 150 μm to 53 μm, 53 μm to 13 μm and 13 μm to 6.5 μm respectively were selected to further prepare spheroidal (Ti.sub.96V.sub.4).sub.90Al.sub.10 alloy powders with a range of a particle size being 150 μm to 53 μm, 53 μm to 13 μm and 13 μm to 6.5 μm by using a mature plasma spheroidization technique. The spheroidal (Ti.sub.96V.sub.4).sub.90Al.sub.10 alloy powder may be applied to the fields of 3D metal printing and metal injection molding (MIM).
EXAMPLE 10
[0166] The example provides a method of preparing a high purity nano-level Ti—V—Al alloy powder by using low purity raw materials. The preparation method includes the following steps.
[0167] Sponge Ti, Electrolyte V, rare earth Ce and Al raw materials with atomic percent contents of T impurity element (including at least one of O, H, N, P, S, F and Cl) being 3 at. %, 1 at. %, 2.5 at. % and 0.2 at. % were selected. The initial alloy raw materials were melted fully based on a given proportioning ratio to obtain an initial alloy melt with a content of major atomic percent content being Ce.sub.70.5Al.sub.10(T.sub.96V.sub.4).sub.17T.sub.2.5.
[0168] The initial alloy melt was prepared into a Ce.sub.70.5Al.sub.10(T.sub.96V.sub.4).sub.17T.sub.2.5 alloy ribbon with a thickness of ˜20 μm at the solidification rate of ˜10.sup.6 K/s by using copper roller spinning. The solidification structure of the alloy ribbon was formed by a matrix phase with an average ingredient being Ce.sub.86.5Al.sub.10.5T.sub.3 and a dispersed particle phase with an ingredient mainly being (Ti.sub.96V.sub.4).sub.92.25Al.sub.7.5T.sub.0.25. The volume percent of the dispersed particle phase in the alloy ribbon was about 12%, and the dispersed particle phase had a particle size of 5 nm to 100 nm and was shaped like sub-spheroid.
[0169] The alloy ribbon was an alloy ribbon formed by an endogenous aluminum-containing alloy powder and a wrapping body.
[0170] At room temperature, the prepared Ce.sub.70.5Al.sub.10(Ti.sub.96V.sub.4).sub.17T.sub.2.5 alloy ribbon was reacted with a hydrochloric acid aqueous solution with a concentration of 0.5 mol/L. During the reaction, the matrix phase with an average ingredient mainly being Ce.sub.86.5Al.sub.10.5T.sub.3 reacted with an acid to change into an ion entering the solution, and the nano-level (Ti.sub.96.4V.sub.4).sub.92.25Al.sub.7.5T.sub.0.25 dispersed particle phase difficult to react with the acid was gradually separated from the matrix phase by dispersion. After 10 min, the dispersed (Ti.sub.96.4V.sub.4).sub.92.25Al.sub.7.5T.sub.0.25 nano-level particles were separated from the solution and then cleaned and dried under a protective atmosphere to obtain a nano-level (Ti.sub.96.4V.sub.4).sub.92.25Al.sub.7.5T.sub.0.25 alloy powder with a particle size being in a range of 5 nm to 100 nm, where the T impurity content was greatly decreased with respect to the sponge Ti raw material.
[0171] Under the protective atmosphere, the nano-level (Ti.sub.96.4V.sub.4).sub.92.25Al.sub.7.5T.sub.0.25 alloy powder was mixed with epoxy resin and other painting components to prepare a nano-level titanium alloy modified polymer corrosion-resistant painting.
EXAMPLE 11
[0172] The example provides a method of preparing a high purity micron-level Ti—Nb—Al alloy powder by using low purity raw materials. The preparation method includes the following steps.
[0173] Sponge Ti, Nb sheet, rare earth Ce and Al raw materials with atomic percent contents of T impurity element (including at least one of O, H, N, P, S, F and Cl) being 3 at. %, 1 at. %, 2.5 at. % and 0.2 at. % were selected. The initial alloy raw materials were melted fully based on a given proportioning ratio to obtain an initial alloy melt with an ingredient of major atomic percent content being Ce.sub.67.5Al.sub.13(Ti.sub.96Nb.sub.4).sub.17T.sub.2.5.
[0174] The initial alloy melt was prepared into a Ce.sub.67.5Al.sub.13(Ti.sub.96Nb.sub.4).sub.17T.sub.2.5 alloy ribbon with a thickness of ˜1 mm at the solidification rate of 300 K/s by using copper roller spinning The solidification structure of the alloy ribbon was formed by a matrix phase with an average ingredient being Ce.sub.83.2Al.sub.13.7T.sub.3.1 and a dispersed particle phase with an ingredient mainly being (Ti.sub.96Nb.sub.4).sub.89.95Al.sub.10T.sub.0.05. The volume percent of the dispersed particle phase in the alloy ribbon was about 13%, and the dispersed particle phase had a particle size of 0.5 μm to 150 μm and was shaped like dendrite.
[0175] At room temperature, the prepared Ce.sub.67.5Al.sub.13(Ti.sub.96Nb.sub.4).sub.17T.sub.2.5 alloy ribbon was reacted with a hydrochloric acid aqueous solution with a concentration of 0.5 mol/L. During the reaction, the matrix phase with an average ingredient mainly being Ce.sub.83.2Al.sub.13.7T.sub.3.1 reacted with an acid to change into an ion entering the solution, and the micron-level (Ti.sub.96Nb.sub.4).sub.89.95Al.sub.10T.sub.0.05 dispersed particle phase difficult to react with the acid was gradually separated from the matrix phase by dispersion. After 10 min, the dispersed (Ti.sub.96Nb.sub.4).sub.89.95Al.sub.10T.sub.0.05 particles were separated from the solution and then cleaned and dried under a protective atmosphere to obtain a micron-level (Ti.sub.96Nb.sub.4).sub.89.95Al.sub.10T.sub.0.05 alloy powder with a particle size being in a range of 0.5 μm to 150 μm, where the T impurity content was greatly decreased with respect to the sponge Ti raw material.
[0176] The (Ti.sub.96Nb.sub.4).sub.89.95Al.sub.10T.sub.0.05 alloy powder was screened through screens of 270 meshes, 1000 meshes, 2000 meshes and 8000 meshes to obtain graded (Ti.sub.96Nb.sub.4).sub.89.95Al.sub.10T.sub.0.05 alloy powders with a range of a dendritic particle size being 150 μm to 53 μm, 53 μm to 13 μm, 13 μm to 6.5 μm, 6.5 μm to 1.6 μm and less than 1.6 μm respectively. The (Ti.sub.96Nb.sub.4).sub.89.95Al.sub.10T.sub.0.05 alloy powders with a range of a dendritic particle size being 150 μm to 53 μm, 53 μm to 13 μm and 13 μm to 6.5 μm respectively were selected to further prepare sub-spheroidal Ti—Nb—Al alloy powders with a range of a particle size being 150 μm to 53 μm, 53 μm to 13 μm and 13 μm to 6.5 μm by using a plasma spheroidization technique. The spheroidal Ti—Nb—Al alloy powders may be applied to the fields of 3D metal printing and metal injection molding.
EXAMPLE 12
[0177] The example provides a method of preparing a high purity nano-level Ti—Al alloy powder by using low purity raw materials. The preparation method includes the following steps. Sponge Ti, rare earth Ce and Al raw materials with atomic percent contents of T impurity element (including at least one of O, H, N, P, S, F and Cl) being 3 at. %, 2.5 at. %, and 0.2 at. % were selected. The sponge Ti further contained 0.5 at. % of Mn; the rare earth Ce further contained 0.7 at. % of Mg.
[0178] The initial alloy raw materials were melted fully based on a given proportioning ratio to obtain an initial alloy melt with an ingredient of major atomic percent content being (Ce.sub.99.3Mg.sub.0.7).sub.70.5Al.sub.10(Ti.sub.99.5Mn.sub.0.5).sub.17T.sub.2.5. The initial alloy melt was prepared into a (Ce.sub.99.3Mg.sub.0.7).sub.70.5Al.sub.10(Ti.sub.99.5Mn.sub.0.5).sub.17T.sub.2.5 alloy ribbon with a thickness of ˜20 μm at the solidification rate of ˜10.sup.6 K/s by using copper roller spinning The solidification structure of the alloy ribbon was formed by a matrix phase with an average ingredient mainly being (Ce.sub.99.3Mg.sub.0.7)86.5Al.sub.10.5T.sub.3 and a dispersed particle phase with an ingredient mainly being (Ti.sub.99.5Mn.sub.0.5).sub.92.25Al.sub.7.5T.sub.0.25. The volume percent of the dispersed particle phase in the alloy ribbon was about 12%, and the dispersed particle phase had a particle size of 5 nm to 150 nm and was shaped like sub-spheroid. A ratio of a number of its mono-crystalline particles to a total number of dispersed particles was greater than 80%.
[0179] The alloy ribbon was an alloy ribbon formed by the endogenous aluminum-containing alloy powder and the wrapping body.
[0180] At room temperature, the prepared (Ce.sub.99.3Mg.sub.0.7).sub.70.5Al.sub.10(Ti.sub.99.5Mn.sub.0.5).sub.17T.sub.2.5 alloy ribbon was reacted with a hydrochloric acid aqueous solution with a concentration of 1 mol/L. During the reaction, the matrix phase with an average ingredient mainly being (Ce.sub.99.3Mg.sub.0.7)86.5Al.sub.10.5T.sub.3 reacted with an acid to change into an ion entering the solution, and the nano-level (Ti.sub.99.5Mn.sub.0.5).sub.92.25Al.sub.7.5T.sub.0.25 dispersed particle phase difficult to react with the acid was gradually separated from the matrix phase by dispersion. After 10 min, the dispersed (Ti.sub.99.5Mn.sub.0.5).sub.92.25Al.sub.7.5T.sub.0.25 particles were separated from the solution and then cleaned and dried under a protective atmosphere to obtain a nano-level (Ti.sub.99.5Mn.sub.0.5).sub.92.25Al.sub.7.5T.sub.0.25 alloy powder with a particle size being in a range of 5 nm to 150 nm, where the T impurity content was greatly decreased with respect to the sponge Ti raw material. Furthermore, With introduction of Mn and Mg into the alloy melt, no intermetallic compound composed of Ce, Mg and Ti, Mn was generated in the initial alloy ribbon; and structural features of the matrix phase and the dispersed particle phase in the alloy ribbon were not affected and the law of the decreasing content of the impurity of the dispersed particle phase was also not affected.
[0181] Under the protective atmosphere, the nano-level (Ti.sub.99.5Mn.sub.0.5).sub.92.25Al.sub.7.5T.sub.0.25 alloy powder was mixed with epoxy resin and other painting components to prepare a nano-level titanium alloy modified polymer corrosion-resistant painting.
EXAMPLE 13
[0182] The example provides a method of preparing a high purity nano-level Ti—V—Al alloy powder by using low purity raw materials. The preparation method includes the following steps.
[0183] Sponge Ti, V raw material, rare earth Ce raw material and Al raw material with atomic percent contents of T impurity element (including at least one of O, H, N, P, S, F and Cl) being 1.5 at. %, 0.5 at. %, 1.5 at. % and 0.2 at. % were selected. The initial alloy raw materials were melted fully based on a given proportioning ratio to obtain an initial alloy melt with an ingredient of major atomic percent content being Ce.sub.65.6Al.sub.15(Ti.sub.96V.sub.4).sub.18T.sub.1.4.
[0184] The initial alloy melt was prepared into a Ce.sub.65.6Al.sub.15(Ti.sub.96V.sub.4).sub.18T.sub.1.4 initial alloy ribbon with a thickness of about 30 μm to 50 μm at the solidification rate of 10.sup.6 K/s-10.sup.7 K/s by using copper roller spinning. The solidification structure of the alloy ribbon was formed by a matrix phase with an average ingredient about being Ce.sub.81.5Al.sub.16.5T.sub.2 and a dispersed particle phase with an ingredient mainly being (Ti.sub.96V.sub.4).sub.89Al.sub.10.8T.sub.0.2. The dispersed particle phase had a particle size of 5 nm to 250 nm and was shaped like sub-spheroid. The volume percent of the dispersed particle phase in the alloy ribbon was about 12%.
[0185] The alloy ribbon was an alloy ribbon formed by the endogenous aluminum-containing alloy powder and the wrapping body. The (Ti.sub.96V.sub.4).sub.89Al.sub.10.8T.sub.0.2 dispersed particle phase was the endogenous aluminum-containing alloy powder and the Ce.sub.81.5Al.sub.16.5T.sub.2 matrix phase was the wrapping body.
[0186] At room temperature, the prepared initial alloy ribbon with a major ingredient being Ce.sub.65.6Al.sub.15(Ti.sub.96V.sub.4).sub.18T.sub.14 was reacted with a hydrochloric acid aqueous solution with a concentration of 0.5 mol/L. During the reaction, the matrix phase with an average ingredient mainly being Ce.sub.81.5Al.sub.16.5T.sub.2 reacted with an acid to change into an ion entering the solution, and the nano-level (Ti.sub.96V.sub.4).sub.89Al.sub.10.8T.sub.0.2 dispersed particle phase difficult to react with the acid was gradually separated from the matrix phase by dispersion. The dispersed (Ti.sub.96V.sub.4).sub.89Al.sub.10.8T.sub.0.2 nano-particles were separated from the solution and then cleaned and dried under a protective atmosphere to obtain a nano-level (Ti.sub.96V.sub.4).sub.89Al.sub.10.8T.sub.0.2 alloy powder with a particle size being in a range of 5 nm to 250 nm, where the T impurity content was greatly decreased with respect to the Ti raw material.
[0187] Under the protective atmosphere, the nano-level (Ti.sub.96 V.sub.4).sub.89Al.sub.10.8T.sub.0.2 alloy powder was mixed with epoxy resin and other painting components to prepare a nano-level titanium alloy modified polymer corrosion-resistant painting.
EXAMPLE 14
[0188] The example provides a method of preparing a high purity sub-micron-level Fe—Cr—Al alloy powder by using low purity raw materials. The preparation method includes the following steps:
[0189] Fe sheet, Cr sheet, rare earth La and Al raw materials with atomic percent contents of T impurity element (including at least one of O, H, N, P, S, F and Cl) being 0.75 at. %, 0.5 at. %, 2 at. % and 0.2 at. % were selected. The initial alloy raw materials were melted fully based on a given proportioning ratio to obtain an initial alloy melt with an ingredient of major atomic percent content being La.sub.46.5Fe.sub.27Cr.sub.7Al.sub.18T.sub.1.5.
[0190] The initial alloy melt was prepared into a La.sub.46.5Fe.sub.27Cr.sub.7Al.sub.18T.sub.1.5 initial alloy thin ribbon with a thickness of about 100 μm at the solidification rate of about 10.sup.5 K/s by using copper roller spinning The solidification structure of the alloy thin ribbon was formed by a dispersed particle phase with a major ingredient being Fe.sub.73.3Cr.sub.20Al.sub.6.5T.sub.0.2 and a matrix phase with a major ingredient being La.sub.74Al.sub.24T.sub.2. The dispersed particle phase had a particle size of 5 nm to 3 μm and was mainly of sub-micron-level.
[0191] The alloy ribbon was an alloy ribbon formed by the endogenous aluminum-containing alloy powder and the wrapping body. The Fe.sub.73.3Cr.sub.20Al.sub.6.5T.sub.0.2 dispersed particle phase was the endogenous aluminum-containing alloy powder and the La.sub.74Al.sub.24T.sub.2 matrix phase was the wrapping body.
By using 0.5 mol/L dilute hydrochloric acid, the La.sub.74Al.sub.24T.sub.2 matrix phase in the La.sub.46.5Fe.sub.27Cr.sub.7Al.sub.18T.sub.1.5 initial alloy thin ribbon was removed through reaction corrosion to obtain a dispersed aluminum-containing alloy powder material with a major ingredient being Fe.sub.73.3Cr.sub.20Al.sub.6.5T.sub.2, with a particle size being in a range of 5 nm to 3 μm, where the T impurity content was greatly decreased with respect to the Fe raw material.
[0192] The technical features of the above examples may be combined arbitrarily. For clarity of descriptions, all of the possible combinations of the technical features of the above examples are not described. However, as long as the combinations of these technical features are not contradictory, they should be considered as within the scope of protection of the present disclosure.
[0193] The above examples are merely several implementations of the present disclosure. Although the descriptions of the examples are relatively specific, they cannot be understood as limiting of the scope of protection present disclosure. It should be pointed out that several variations and improvements made by persons of ordinary skills in the art without departing from the idea of the present disclosure shall all fall within the scope of protection of the present disclosure. Therefore, the scope of protection of the present disclosure shall be indicated by the appended claims.