METHOD FOR PREPARING HIGH-PURITY POWDER MATERIAL, APPLICATION THEREOF, AND DOUBLE-PHASE POWDER MATERIAL
20240033822 ยท 2024-02-01
Inventors
Cpc classification
B22F2301/30
PERFORMING OPERATIONS; TRANSPORTING
C22C28/00
CHEMISTRY; METALLURGY
C22C30/00
CHEMISTRY; METALLURGY
C22C38/005
CHEMISTRY; METALLURGY
B22F1/142
PERFORMING OPERATIONS; TRANSPORTING
B22F2301/205
PERFORMING OPERATIONS; TRANSPORTING
C22C27/02
CHEMISTRY; METALLURGY
B22F2998/10
PERFORMING OPERATIONS; TRANSPORTING
B22F2304/054
PERFORMING OPERATIONS; TRANSPORTING
B22F2999/00
PERFORMING OPERATIONS; TRANSPORTING
B22F2304/10
PERFORMING OPERATIONS; TRANSPORTING
B22F1/056
PERFORMING OPERATIONS; TRANSPORTING
B22F1/145
PERFORMING OPERATIONS; TRANSPORTING
B22F1/05
PERFORMING OPERATIONS; TRANSPORTING
International classification
B22F9/08
PERFORMING OPERATIONS; TRANSPORTING
B22F1/142
PERFORMING OPERATIONS; TRANSPORTING
B22F1/145
PERFORMING OPERATIONS; TRANSPORTING
C22C27/02
CHEMISTRY; METALLURGY
C22C30/00
CHEMISTRY; METALLURGY
B22F1/05
PERFORMING OPERATIONS; TRANSPORTING
C22C28/00
CHEMISTRY; METALLURGY
Abstract
The present disclosure provides a method for preparing a high-purity powder material, an application thereof, and a double-phase powder material. The high-purity powder material is prepared through an atomization comminuting process and de-phasing method. The preparation method comprises the following steps: firstly preparing intermediate alloy powders with first-phase particles wrapped by a second-phase matrix through an atomization comminuting process. Impurity elements are enriched into the second-phase matrix and the first-phase particles are purified during the solidification of the intermediate alloy powders; By removing the second-phase matrix in the intermediate alloy powders, a high-purity target powder material originated from the original first-phase particles can be obtained. The preparation method of the present disclosure has the characteristics of a simple process, easy operation, and low cost, and can be used to prepare nano-level, sub-micron-level, and micro-level multiple high-purity powder materials, which has a good application prospect in catalytic materials, powder metallurgy
Claims
1. A method for preparing a high-purity powder material, comprising the following steps: at step 1, selecting initial alloy raw materials and melting the initial alloy raw materials based on an ingredient ratio of the initial alloy to obtain a homogeneous initial alloy melt; at step 2, atomizing and solidifying the initial alloy melt through an atomization comminuting process to obtain an intermediate alloy powder; wherein the intermediate alloy powder comprises a first phase and a second phase, the first phase is granular, the second phase is a matrix phase with a melting point lower than that of the first phase, and the first-phase particle is wrapped in the second-phase matrix; wherein during the atomization comminuting process, impurity elements in the initial alloy melt and introduced during an atomizing solidification process are enriched in the second-phase matrix such that the first-phase particles are purified; at step 3, removing the second-phase matrix in the intermediate alloy powder, and retaining the first-phase particles, wherein the impurity elements enriched in the second-phase matrix are removed together with the second-phase matrix such that a high-purity target metal power material composed of the first-phase particles is obtained.
2. The method for preparing a high-purity powder material according to claim 1, wherein the impurity element in the initial alloy melt is T, and T includes at least one of O, H, N, P, S, F, Cl, I, and Br.
3. The method for preparing a high-purity powder material according to claim 2, wherein the average ingredient of the initial alloy melt comprises any one of the following combinations (1)-(4) according to different proportions of the initial alloy raw materials: combination (1): the major average ingredient of the initial alloy melt is A.sub.a(M.sub.xD.sub.y).sub.bT.sub.d, A includes at least one of Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu, M includes at least one of W, Cr, Mo, V, Ta, Nb, Zr, Hf, and Ti, D includes at least one of Fe, Co, and Ni, x, y; a, b, and c represent the atomic percent contents of corresponding constituent elements respectively, and 0.5%a99.5%, 0.5%b99.5% and 0d10%; 5%x55% and 45%y95%; combination (2): the major average ingredient of the initial alloy melt is A.sub.aM.sub.bT.sub.d, A includes at least one of Mg, Ca, Li, Na, K, Cu, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu, M includes at least one of W, Cr, Mo, V, Ta, Nb, Zr, Hf, and Ti, a, b, and c represent the atomic percent contents of corresponding constituent elements respectively, and 0.5%a99.5%, 0.5%b99.5% and 0d10%; combination (3): the major average ingredient of the initial alloy melt is A.sub.aM.sub.bT.sub.d, A includes at least one of Zn, Mg, Sn, Pb, Ga, In, Al, La, Ge, Cu, K, Na, and Li, M includes at least one of Be, B, Bi, Fe, Ni, Cu, Ag, Si, Ge, Cr, and V, and the proportion of the atomic percent contents of Be, B, Si, and Ge in M to M is smaller than 50%; a, b, and c represent the atomic percent contents of corresponding constituent elements respectively, and 0.5%a99.5%, 0.5%b99.5%, and 0d10%; combination (4): when the major average ingredient of the initial alloy melt is A.sub.aM.sub.bAl.sub.cT.sub.d, A includes at least one of Y, La, Ge, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu; M includes at least one of W, Cr, Mo, V, Ta, Nb, Zr, Hf, and Ti; Al is aluminum; a, b, c, and d represent the atomic percent contents of corresponding constituent elements respectively, and 0.5%a99.4%, 0.5%b99.4%, 0.1%c25%, and 0d10%.
4. The method for preparing a high-purity powder material according to claim 3, wherein when the average ingredient of the initial alloy melt is the combination (1) of step 1, the initial alloy powder comprises the first-phase particles with the major ingredient of (M.sub.xD.sub.y).sub.x1T.sub.z1, and the second-phase matrix with the major ingredient of A.sub.x2T.sub.z2; 98%x1100% and 0z12%; 70%x2100% and 0z230%; z1dz2 and 2z1z2; and x1, z1, x2, and z2 represent the atomic percent contents of corresponding constituent elements respectively; when the average ingredient of the initial alloy melt is the combination (2) or combination (3) of step 1, the initial alloy powder comprises the first-phase particles with the major ingredient of M.sub.x1T.sub.z1 and the second-phase matrix with the major ingredient of A.sub.x2T.sub.z2; 98%x1100% and 0z12%; 70%x2100% and 0z230%; z1dz2 and 2z1z2; and x1, z1, x2, and z2 represent the atomic percent contents of corresponding constituent elements respectively; when the average ingredient of the initial alloy melt is the combination (4) of step 1, the initial alloy powder comprises the first-phase particles with the major ingredient of M.sub.x1Al.sub.y1T.sub.z1 and the second-phase matrix with the major ingredient of A.sub.x2Al.sub.y2T.sub.z2, 78%x199.9%, 0.1%y122% and 0z12%; 70%x299.8%, 0.2%y230%, 0z230%, z1dz2, and 2z1z2, and x1, y1, z1, x2, y2, and z2 represent the atomic percent contents of corresponding constituent elements respectively.
5. The method for preparing a high-purity powder material according to claim 1, wherein the atomization comminuting process includes at least one of gas atomization, water atomization, water and gas combined atomization, vacuum atomization, plasma atomization, centrifugal atomization, rotating disk atomization, and rotating electrode atomization.
6. The method for preparing a high-purity powder material according to claim 1, wherein the structure in which the first-phase particle is wrapped in the second-phase matrix includes: a mosaic structure in which a plurality of the first-phase particles are distributed in the second-phase matrix in a dispersed manner, or a core-shell structure in which a single first-phase particle is inside and the second-phase matrix is outside.
7. The method for preparing a high-purity powder material according to claim 1, wherein the method for removing the second-phase matrix in the intermediate alloy powders includes at least one of an acid reaction for removal, an alkali reaction for removal, a vacuum volatilization for removal, and a second-phase matrix natural oxidation-powdering peeling removal.
8. The method for preparing a high-purity powder material according to claim 1, wherein the particle size of the high-purity target powder material is in a range of 3 nm to 7.9 mm.
9. An application of the high-purity powder material according to claim 1 in the fields such as catalytic materials, powder metallurgy, composite materials, wave-absorbing materials, sterilization materials, metal injection molding, 3D printing additive manufacturing, and coating.
10. A double-phase powder material, wherein the double-phase powder material is powdery, and a single double-phase particle thereof further comprises an endogenous powder and a wrapping body; the solidification structure of the double-phase powder material comprises a matrix phase and a particle phase, the matrix phase is the wrapping body, and the particle phase is the endogenous powder in the double-phase powder material; the melting point of the wrapping body is lower than that of the endogenous powder, and the endogenous powder is wrapped in the wrapping body; the structure in which the endogenous powder in the double-phase powder material is wrapped in the wrapping body includes: a mosaic structure in which a plurality of the endogenous powder is distributed in the wrapping body in a dispersed manner, or a core-shell structure in which a single endogenous powder is inside and the wrapping body is outside; the chemical constitutions and structures of the double-phase powder material comprise any one of the following four combinations: 1) the major ingredient of the endogenous powder in the double-phase powder material is (M.sub.xD.sub.y).sub.x1T.sub.z1, and the major average ingredient of the wrapping body is A.sub.x2T.sub.z2; 98%x1100% and 0<z12%; 70%x2100% and 0z230%; z1dz2 and 2z1z2; x1, z1, x2, and z2 represent the atomic percent contents of corresponding constituent elements respectively; A includes at least one of Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu, M includes at least one of W, Cr, Mo, V, Ta, Nb, Zr, Hf, and Ti, and D includes at least one of Fe, Co and Ni; T includes at least one of O, H, N, P, S, F, Cl, I, and Br; x and y represent the atomic percent contents of corresponding constituent elements respectively, and 5%x55% and 45%y95%; 2) the major ingredient of the endogenous powder in the double-phase powder material is M.sub.x1T.sub.z1T.sub.z1, and the major average ingredient of the wrapping body is A.sub.x2T.sub.z2; 98%x1100% and 0z12%; 70%x2100% and 0z230%; z1dz2 and 2z1z2; x1, z1, x2 and z2 represent the atomic percent contents of corresponding constituent elements respectively; A includes at least one of Mg, Ca, Li, Na, K, Cu, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu, and M includes at least one of W, Cr, Mo, V, Ta, Nb, Zr, Hf, and Ti; T includes at least one of O, H, N, P, S, F, Cl, I, and Br; 3) the major ingredient of the endogenous powder in the double-phase powder material is M.sub.x1T.sub.z1, and the major average ingredient of the wrapping body is A.sub.x2T.sub.z2; 98%x1100% and 0z12%; 70%x2100% and 0z230%; z1dz2 and 2z1z2; x1, z1, x2, and z2 represent the atomic percent contents of corresponding constituent elements respectively; A includes at least one of Zn, Mg, Sn, Pb, Ga, In, Al, La, Ge, Cu, K, Na, and Li, M includes at least one of Be, B, Bi, Fe, Ni, Cu, Ag, Si, Ge, Cr, and V, and the proportion of the atomic percent contents of Be, B, Si and Ge in M to M is smaller than 50%; T includes at least one of O, H, N, P, S, F, Cl, I, and Br; 4) the major ingredient of the endogenous powder in the double-phase powder material is M.sub.x1Al.sub.y1T.sub.z1, and the major average ingredient of the wrapping body is A.sub.x2Al.sub.y2T.sub.z2; 78%x199.9%, 0.1%y122% and 0z12%; 70%x299.8%, 0.2%y230%, 0z230%, z1dz2 and 2z1z2, and x1, y1, z1, x2, y2, and z2 represent the atomic percent contents of corresponding constituent elements respectively; A includes at least one of Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu; M includes at least one of W, Cr, Mo, V, Ta, Nb, Zr, Hf, and Ti; Al is aluminum; and T includes at least one of O, H, N, P, S, F, Cl, I, and Br.
11. A method for preparing a high-purity powder material, comprising the following steps: at step 1, selecting initial alloy raw materials, melting the initial alloy raw materials based on an ingredient ratio of the initial alloy to obtain a homogeneous initial alloy melt; at step 2, atomizing and solidifying the initial alloy melt through an atomization comminuting process, to obtain an intermediate alloy powder; wherein the intermediate alloy powder comprises a first phase and a second phase, the first phase is granular, the second phase is a matrix phase with a melting point lower than that of the first phase, and the first-phase particle is wrapped in the second-phase matrix; during the atomization comminuting process, impurity elements in the initial alloy melt and introduced during an atomizing solidification process are enriched in the second-phase matrix, so that the first-phase particles are purified; at step 3, removing the second-phase matrix in the intermediate alloy powder, and retaining the first-phase particles, wherein the impurity elements enriched in the second-phase matrix are removed together with the second-phase matrix, so that a high-purity target power material composed of the first-phase particles is obtained; wherein the impurity element in the initial alloy melt is T, and T includes at least one of O, H, N, P, S, F, Cl, I, and Br; the major average ingredient of the initial alloy melt is A.sub.aM.sub.bT.sub.d, A includes at least one of Zn, Sn, Pb, Ga, In, Al, Ge, and Cu; M includes at least one of Be, Si, Ge, and B, and the proportion of the atomic percent contents of Be, Si, Ge, and B in M to M is greater than or equal to 50%, a, b and c represent the atomic percent contents of corresponding constituent elements respectively, and 0.5%a99.5%, 0.5%b99.5%, and 0d10%; the initial alloy powder comprises the first-phase particles with the major ingredient of M.sub.x1T.sub.z1 and the second-phase matrix with the major ingredient of A.sub.x2T.sub.z2; 98%x1100% and 0z12%; 70%x2100% and 0z230%; z1dz2 and 2z1z2; x1, z1, x2, and z2 represent the atomic percent contents of corresponding constituent elements respectively.
12. (canceled)
13. The method for preparing a high-purity metal powder material according to claim 1, wherein when the ingredient ratio of the initial alloy is A.sub.aM.sub.b, A is selected from at least one of Mg, Ca, Li, Na, K, Zn, In, Sn, Pb, Ga, Cu, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu, and M is selected from at least one of W, Cr, Mo, V, Ta, Nb, Zr, Hf, Ti, Fe, Co, Ni, Mn, Cu, Ag, Si, Ge, B, Be, and C; a and b represent the atomic percent contents of corresponding constituent elements respectively, and 0.5%b98% and a+b=100%; the A.sub.aM.sub.b alloy melt does not form an intermetallic compound composed of A and M during atomizing solidification, but forms a first-phase particle with the ingredient of M and a second-phase matrix with the ingredient of A. when the ingredient ratio of the initial alloy is A.sub.aM.sub.bAl.sub.c, A is selected from at least one of Mg, Ca, Li, Na, K, Zn, In, Sn, Pb, Ga, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu, Al is aluminum, and M is selected from at least one of W, Cr, Mo, V, Ta, Nb, Zr, Hf, Ti, Fe, Co, Ni, Mn, Cu, Ag, Si, Ge, B, Be, and C; a, b, and c represent the atomic percent contents of corresponding constituent elements respectively, and 0.5%b98%, 0.1%c30%, and a+b+c=100%; the A.sub.aM.sub.bAl.sub.c alloy melt does not form an intermetallic compound composed of A and M during atomizing solidification, but forms a first-phase particle with the ingredient of M.sub.x1Al.sub.y1 and a second-phase matrix with the ingredient of A.sub.x2Al.sub.y2, x1, y1, x2, and y2 represent atomic percent contents of corresponding constituent elements respectively, and 0.1%y125%, 0.1%y235%, x1+y1=100%, and x2+y2=100%.
Description
DETAILED DESCRIPTION
[0259] A method for preparing a high-purity powder material according to the present disclosure will be further described below in combination with the examples.
Example 1
[0260] This example provides a preparation method for nanometer CrV powders, which includes the following steps:
[0261] An alloy with the atomic percentage formula of Zn.sub.58(Cr.sub.50V.sub.50).sub.42 is selected, raw materials are weighed according to the formulation, after the initial alloy raw material is uniformly molten, the alloy melt is solidified and atomized through a gas atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 3 m to 150 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix with an ingredient of Zn and multiple high-melting-point first-phase particles with an ingredient of Cr.sub.50V.sub.50, the Cr.sub.50V.sub.50 particles are embedded in the Zn matrix in a dispersed manner, wherein the shape of the Cr.sub.50V.sub.50 particles is sub-spheroidal, and the particle size of the Cr.sub.50V.sub.50 particles is in a range of 3 nm to 300 nm. The volume content of the Cr.sub.50V.sub.50 particles in the intermediate alloy powder is about 38%; the impurities are enriched in the Zn matrix during the solidification process.
[0262] The Zn matrix in the intermediate alloy powder is volatilized and removed by vacuum heat treatment, so that the Cr.sub.50V.sub.50 particles which are difficult to be volatilized in the intermediate alloy powder can be separated, then nanometer Cr.sub.50V.sub.50 powders with a particle size being in a range of 3 nm to 300 nm are obtained, and the total content of H, O, N, S, P, F, Cl, I and Br in the Cr.sub.50V.sub.50 powders is lower than 1500 ppm.
Example 2
[0263] This example provides a preparation method for nanometer CrV powders, which includes the following steps:
[0264] An alloy with the atomic percentage formula of Zn.sub.80(Cr.sub.50V.sub.50).sub.20 is selected, raw materials are weighed according to the formulation, after the initial alloy raw material is uniformly molten, the alloy melt is solidified and atomized through a gas atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 1 m to 100 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix with an ingredient of Zn and multiple high-melting-point first-phase particles with an ingredient of Cr.sub.50V.sub.50, the Cr.sub.50V.sub.50 particles are embedded in the Zn matrix in a dispersed manner, wherein the shape of the Cr.sub.50V.sub.50 particles is sub-spheroidal, and the particle size of the Cr.sub.50V.sub.50 particles is in a range of 3 nm to 200 nm. The volume content of the Cr.sub.50V.sub.50 particles in the intermediate alloy powder is about 17.5%; the impurities are enriched in the Zn matrix during the solidification process.
[0265] The Zn matrix in the intermediate alloy powder is reacted and removed by sodium hydroxide solution, so that the Cr.sub.50V.sub.50 particles which do not react with alkali in the intermediate alloy powder can be separated, then nanometer Cr.sub.50V.sub.50 powders with a particle size in a range of 3 nm to 200 nm are obtained, and the total content of H, O, N, S, P, F, Cl, I and Br in the Cr.sub.50V.sub.50 powders is lower than 1600 ppm.
Example 3
[0266] This example provides a preparation method for sub-micron-level and micron-level Nb powders, which includes the following steps:
[0267] An alloy with the atomic percentage formula of Cu.sub.54Nb.sub.46 is selected, raw materials are weighed according to the formulation, after the initial alloy raw material is uniformly molten, the alloy melt is solidified and atomized through a gas atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 5 m to 500 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix with an ingredient of Cu and multiple high-melting-point first-phase particles with an ingredient of Nb, the Nb particles are embedded in the Cu matrix in a dispersed manner, wherein the shape of the Nb particles is sub-spheroidal, and the particle size of the Nb particles is in a range of 50 nm to 5 m. The volume content of the Nb particles in the intermediate alloy powder is about 46%; the impurities are enriched in the Cu matrix during the solidification process.
[0268] The Cu matrix in the intermediate alloy powder is removed by hydrochloric acid, so that the Nb particles which are difficult to react with the hydrochloric acid can be separated, then Nb powders with a particle size in a range of 50 nm to 5 m are obtained, and the total content of H, O, N, S, P, F, Cl, I and Br in the Nb powders is lower than 1400 ppm.
Example 4
[0269] This example provides a preparation method for nanometer FeNi powders, which includes the following steps:
[0270] An alloy with the atomic percentage formula of Li.sub.10(Fe.sub.50Ni.sub.50).sub.90 is selected, raw materials are weighed according to the formulation, after the initial alloy raw material is uniformly molten, the alloy melt is solidified and atomized through a gas atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 3 m to 120 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix shell with an ingredient of Li and high-melting-point first-phase particles with an ingredient of Fe.sub.50Ni.sub.50, the Fe.sub.50Ni.sub.50 core particles are embedded in the Li matrix shell, wherein the shape of the Fe.sub.50Ni.sub.50 particles is sub-spheroidal, and the particle size of the Fe.sub.50Ni.sub.50 particles is in a range of 2 m to 110 m. The volume content of the FeNi particles in the intermediate alloy powder is about 82%; the impurities are enriched in the Li matrix shell during the solidification process.
[0271] The Fe.sub.50Ni.sub.50 particles and the oxidized Li matrix (Lithium oxide powder) are separated from each other by an autoxidation-powdering process, in which the Li matrix shell can be autoxidated and the Fe.sub.50Ni.sub.50 particles can be separated by their magnetic property, then nanometer Fe.sub.50Ni.sub.50 powders with a particle size being in a range of 2 m to 110 m are obtained, and the total content of H, O, N, S, P, F, Cl, I and Br in the Fe.sub.50Ni.sub.50 powders is lower than 1800 ppm.
Example 5
[0272] This example provides a preparation method for micrometer FeCrVTiMo powders, which includes the following steps:
[0273] An alloy with the atomic percentage formula of La.sub.10(Fe.sub.20Cr.sub.20V.sub.20Ti.sub.20Mo.sub.20).sub.90 is selected, raw materials are weighed according to the formulation, after the initial alloy raw material is uniformly molten, the alloy melt is solidified and atomized through a water atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 3 m to 150 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix shell with an ingredient of La and high-melting-point first-phase particles with an ingredient of Fe.sub.20Cr.sub.20V.sub.20Ti.sub.20Mo.sub.20, the Fe.sub.20Cr.sub.20V.sub.20Ti.sub.20Mo.sub.20 core particles are embedded in the La matrix shell, wherein the shape of the Fe.sub.20Cr.sub.20V.sub.20Ti.sub.20Mo.sub.20 particles is sub-spheroidal, and the particle size of the Fe.sub.20Cr.sub.20V.sub.20Ti.sub.20Mo.sub.20 particles is in a range of 2 m to 144 m. The volume content of the Fe.sub.20Cr.sub.20V.sub.20Ti.sub.20Mo.sub.20 particles in the intermediate alloy powder is about 78%; the impurities are enriched in the La matrix shell during the solidification process.
[0274] The La matrix in the intermediate alloy powder is removed by dilute hydrochloric acid, so that the Fe.sub.20Cr.sub.20V.sub.20Ti.sub.20Mo.sub.20 particles which are difficult to react with the dilute hydrochloric acid can be separated, then Fe.sub.20Cr.sub.20V.sub.20Ti.sub.20Mo.sub.20 powders with a particle size being in a range of 2 m to 144 m are obtained, and the total content of H, O, N, S, P, F, Cl, I and Br in the Fe.sub.20Cr.sub.20V.sub.20Ti.sub.20Mo.sub.20 powders is lower than 1800 ppm.
Example 6
[0275] This example provides a preparation method for micrometer Ti powders, which includes the following steps:
[0276] An alloy with the atomic percentage formula of Ce.sub.25Ti.sub.75 is selected, raw materials are weighed according to the formulation, after the initial alloy raw material is uniformly molten, the alloy melt is solidified and atomized through a gas atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 5 m to 100 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix with an ingredient of Ce and multiple high-melting-point first-phase particles with an ingredient of Ti, the Ti particles are embedded in the Ce matrix, wherein the shape of the Ti particles is sub-spheroidal or dendritic, and the particle size of the Ti particles is in a range of 2 m to 50 m. The volume content of the Ti particles in the intermediate alloy powder is about 61%; the impurities are enriched in the Ce matrix during the solidification process.
[0277] The Ce matrix in the intermediate alloy powder is removed by dilute acid solution, so that the Ti particles which are difficult to react with the dilute acid solution can be separated, then Ti powders with a particle size in a range of 2 m to 50 m are obtained, and the total content of H, O, N, S, P, F, Cl, I and Br in the Ti powders is lower than 1500 ppm.
Example 7
[0278] This example provides a preparation method for micron-level TiZrHfNbTa high-Entropy powders, which includes the following steps:
[0279] An alloy with the atomic percentage formula of Ce.sub.10(Ti.sub.20Zr.sub.20Hf.sub.20Nb.sub.20Ta.sub.20).sub.90 is selected, raw materials are weighed according to the formulation, after the initial alloy raw material is uniformly molten, the alloy melt is solidified and atomized through a water atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 3 m to 150 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix with an ingredient of Ce and a single high-melting-point first-phase particle with an ingredient of Ti.sub.20Zr.sub.20Hf.sub.20Nb.sub.20Ta.sub.20, the Ti.sub.20Zr.sub.20Hf.sub.20Nb.sub.20Ta.sub.20 core particle is embedded in the Ce matrix shell, wherein the shape of the Ti.sub.20Zr.sub.20Hf.sub.20Nb.sub.20Ta.sub.20 particle is sub-spheroidal, and the particle size of the Ti.sub.20Zr.sub.20Hf.sub.20Nb.sub.20Ta.sub.20 particle is in a range of 2 m to 142 m. The volume content of the Ti.sub.20Zr.sub.20Hf.sub.20Nb.sub.20Ta.sub.20 particle in the intermediate alloy powder is about 84%; the impurities are enriched in the Ce matrix shell during the solidification process.
[0280] The Ce matrix shell in the intermediate alloy powder is removed by dilute acid, so that the Ti.sub.20Zr.sub.20Hf.sub.20Nb.sub.20Ta.sub.20 particle which is difficult to react with the dilute acid can be separated, then Ti.sub.20Zr.sub.20Hf.sub.20Nb.sub.20Ta.sub.20 powders with a particle size being in a range of 2 m to 142 m are obtained, and the total content of H, O, N, S, P, F, Cl, I and Br in the Ti.sub.20Zr.sub.20Hf.sub.20Nb.sub.20Ta.sub.20 powders is lower than 1500 ppm.
Example 8
[0281] This example provides a preparation method for micron-level TiN powders, which includes the following steps:
[0282] An alloy with the atomic percentage formula of Gd.sub.25(Ti.sub.50Ni.sub.50).sub.75 is selected, raw materials are weighed according to the formulation, after the initial alloy raw material is uniformly molten, the alloy melt is solidified and atomized through a gas atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 5 m to 100 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix with an ingredient of Gd and multiple high-melting-point first-phase particles with an ingredient of Ti.sub.50Ni.sub.50, the Ti.sub.50Ni.sub.50 particles are embedded in the Gd matrix, wherein the shape of the Ti.sub.50Ni.sub.50 particle is sub-spheroidal or dendritic, and the particle size of the Ti.sub.50Ni.sub.50 particle is in a range of 2 m to 50 m. The volume content of the Ti.sub.50Ni.sub.50 particle in the intermediate alloy powder is about 56%; the impurities are enriched in the Gd matrix during the solidification process.
[0283] The Gd matrix in the intermediate alloy powder is removed by dilute acid, so that the Ti.sub.50Ni.sub.50 particle which is difficult to react with the dilute acid can be separated, then Ti.sub.50Ni.sub.50 powders with a particle size in a range of 2 m to 50 m are obtained, and the total content of H, O, N, S, P, F, Cl, I and Br in the Ti.sub.50Ni.sub.50 powders is lower than 1400 ppm.
Example 9
[0284] This example provides a preparation method for micrometer FeCrTi powders, which includes the following steps:
[0285] An alloy with the atomic percentage formula of La.sub.2(Fe.sub.79Cr.sub.20Ti.sub.1).sub.98 is selected, raw materials are weighed according to the formulation, after the initial alloy raw material is uniformly molten, the alloy melt is solidified and atomized through a water atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 3 m to 150 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix shell with an ingredient of La and a single high-melting-point first-phase particle with an ingredient of Fe.sub.79Cr.sub.20Ti.sub.1, the single Fe.sub.79Cr.sub.20Ti.sub.1 core particle is embedded in the La matrix shell, wherein the shape of the Fe.sub.79Cr.sub.20Ti.sub.1 particle is sub-spheroidal, and the particle size of the Fe.sub.79Cr.sub.20Ti.sub.1 particle is in a range of 2.9 m to 147 m. The volume content of the Fe.sub.79Cr.sub.20Ti.sub.1 particle in the intermediate alloy powder is about 94%; the impurities are enriched in the La matrix shell during the solidification process.
[0286] The La matrix shell in the intermediate alloy powder is removed by dilute hydrochloric acid, so that the Fe.sub.79Cr.sub.20Ti.sub.1 particle which is difficult to react with the dilute hydrochloric acid can be separated, then Fe.sub.79Cr.sub.20Ti.sub.1 powders with a particle size in a range of 2.9 m to 147 m are obtained, and the total content of H, O, N, S, P, F, Cl, I and Br in the Fe.sub.79Cr.sub.20Ti.sub.1 powders is lower than 1800 ppm.
Example 10
[0287] This example provides a preparation method for micron-level TiAlV powders, which includes the following steps:
[0288] An alloy with the atomic percentage formula of Ce.sub.30Al.sub.12(Ti.sub.96V.sub.4).sub.58 is selected, raw materials are weighed according to the formulation, after the initial alloy raw material is uniformly molten, the alloy melt is solidified and atomized through a gas atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 3 m to 150 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix with an ingredient of Ce.sub.85Al.sub.15 and multiple high-melting-point first-phase particles with an ingredient of (Ti.sub.96V.sub.4).sub.90Al.sub.10, the (Ti.sub.96V.sub.4).sub.90Al.sub.10 particles are embedded in the Ce.sub.85Al.sub.15 matrix, wherein the shape of the (Ti.sub.96V.sub.4).sub.90Al.sub.10 particle is sub-spheroidal or dendritic, and the particle size of the (Ti.sub.96V.sub.4).sub.90Al.sub.10 particle is in a range of 1 m to 50 m. The volume content of the (Ti.sub.96V.sub.4).sub.90Al.sub.10 particle in the intermediate alloy powder is about 52%; the impurities are enriched in the Ce.sub.85Al.sub.15 matrix during the solidification process.
[0289] The Ce.sub.85Al.sub.15 matrix in the intermediate alloy powder is removed by dilute hydrochloric acid, so that the (Ti.sub.96V.sub.4).sub.90Al.sub.10 particle which is difficult to react with the dilute hydrochloric acid can be separated, then (Ti.sub.96V.sub.4).sub.90Al.sub.10 powders with a particle size being in a range of 1 m to 50 m are obtained, and the total content of H, O, N, S, P, F, Cl, I and Br in the Ti.sub.50Ni.sub.50 powders is lower than 1400 ppm.
Example 11
[0290] This example provides a preparation method for micron-level FeCrNbMoTiV powders, which includes the following steps:
[0291] An alloy with the atomic percentage formula of La.sub.25(Fe.sub.76Cr.sub.16Nb.sub.2Mo.sub.2Ti.sub.2V.sub.2).sub.75 is selected, raw materials are weighed according to the formulation, after the initial alloy raw material is uniformly molten, the alloy melt is solidified and atomized through a gas atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 2 m to 150 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix with an ingredient of La and multiple high-melting-point first-phase particles with an ingredient of Fe.sub.76Cr.sub.16Nb.sub.2Mo.sub.2Ti.sub.2V.sub.2, the Fe.sub.76Cr.sub.16Nb.sub.2Mo.sub.2Ti.sub.2V.sub.2 particles are embedded in the La matrix, wherein the shape of the Fe.sub.76Cr.sub.16Nb.sub.2Mo.sub.2Ti.sub.2V.sub.2 particle is sub-spheroidal or dendritic, and the particle size of the (Ti.sub.96V.sub.4).sub.90Al.sub.10 particle is in a range of 1 m to 50 m. The volume content of the Fe.sub.76Cr.sub.16Nb.sub.2Mo.sub.2Ti.sub.2V.sub.2 particle in the intermediate alloy powder is about 50%; the impurities are enriched in the La matrix during the solidification process.
[0292] The La matrix in the intermediate alloy powder is removed by dilute hydrochloric acid, so that the high Cr content of Fe.sub.76Cr.sub.16Nb.sub.2Mo.sub.2Ti.sub.2V.sub.2 particle which is difficult to react with the dilute hydrochloric acid can be separated, then Fe.sub.76Cr.sub.16Nb.sub.2Mo.sub.2Ti.sub.2V.sub.2 powders with a particle size in a range of 1 m to 50 m are obtained, the Fe.sub.76Cr.sub.16Nb.sub.2Mo.sub.2Ti.sub.2V.sub.2 powders are finer than the intermediate alloy powder, and the total content of H, O, N, S, P, F, Cl, I and Br in the Fe.sub.76Cr.sub.16Nb.sub.2Mo.sub.2Ti.sub.2V.sub.2 powders is lower than 1400 ppm.
Example 12
[0293] This example provides a preparation method for micron-level FeCrMoTi powders, which includes the following steps:
[0294] An alloy with the atomic percentage formula of La.sub.5(Fe.sub.76Cr.sub.20Mo.sub.2Ti.sub.2).sub.95 is selected, raw materials are weighed according to the formulation, after the initial alloy raw material is uniformly molten, the alloy melt is solidified and atomized through a water atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 3 m to 120 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix shell with an ingredient of La and a single high-melting-point first-phase particle with an ingredient of Fe.sub.76Cr.sub.20Mo.sub.2Ti.sub.2, the single Fe.sub.76Cr.sub.20Mo.sub.2Ti.sub.2 core particle is embedded in the La matrix shell, wherein the shape of the Fe.sub.76Cr.sub.20Mo.sub.2Ti.sub.2 particle is sub-spheroidal, and the particle size of the Fe.sub.79Cr.sub.20Ti.sub.1 particle is in a range of 2 m to 113 m. The volume content of the Fe.sub.76Cr.sub.20Mo.sub.2Ti.sub.2 particle in the intermediate alloy powder is about 86%; the impurities are enriched in the La matrix shell during the solidification process.
[0295] The La matrix shell in the intermediate alloy powder is removed by dilute acid, so that the high Cr content of Fe.sub.76Cr.sub.20Mo.sub.2Ti.sub.2 particle which is difficult to react with the dilute acid can be separated, then the micron Fe.sub.76Cr.sub.20Mo.sub.2Ti.sub.2 powders with a particle size being in a range of 2 m to 50 m are obtained, the Fe.sub.76Cr.sub.20Mo.sub.2Ti.sub.2 powders are finer than the intermediate alloy powder, and the total content of H, O, N, S, P, F, Cl, I and Br in the micron Fe.sub.76Cr.sub.20Mo.sub.2Ti.sub.2 powders is lower than 1800 ppm.
Example 13
[0296] This example provides a preparation method for micron-level FeCrC powders, which includes the following steps:
[0297] An alloy with the atomic percentage formula of La.sub.2.5(Fe.sub.84.9Cr.sub.15C.sub.0.1).sub.97.5 is selected, raw materials are weighed according to the formulation, after the initial alloy raw material is uniformly molten, the alloy melt is solidified and atomized through a water atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 3 m to 150 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix shell with an ingredient of La and a single high-melting-point first-phase particle with an ingredient of Fe.sub.84.9Cr.sub.15C.sub.0.1, the single Fe.sub.84.9Cr.sub.15C.sub.0.1 core particle is embedded in the La matrix shell, wherein the shape of the Fe.sub.84.9Cr.sub.15C.sub.0.1 particle is sub-spheroidal, and the particle size of the Fe.sub.84.9Cr.sub.15C.sub.0.1 particle is in a range of 2.9 m to 146 m. The volume content of the Fe.sub.84.9Cr.sub.15C.sub.0.1 particle in the intermediate alloy powder is about 92%; the impurities are enriched in the La matrix shell during the solidification process.
[0298] The Fe.sub.84.9Cr.sub.15C.sub.0.1 particles and the oxidized La matrix (Lanthanum oxide powder) are separated from each other by an autoxidation-powdering process, in which the La matrix shell can be autoxidated and the Fe.sub.84.9Cr.sub.15C.sub.0.1 particles can be separated by their magnetic property, then micrometer Fe.sub.84.9Cr.sub.15C.sub.0.1 powders with a particle size being in a range of 2 m to 50 m are obtained, and the total content of H, O, N, S, P, F, Cl, I and Br in the Fe.sub.50Ni.sub.50 powders is lower than 1600 ppm.
Example 14
[0299] This example provides a preparation method for nanometer Fe powders, which includes the following steps:
[0300] An alloy with the atomic percentage formula of La.sub.59Fe.sub.41 is selected, raw materials are weighed according to the formulation, after the initial alloy raw material is uniformly molten, the alloy melt is solidified and atomized through a water atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 3 m to 150 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix with an ingredient of La and multiple high-melting-point first-phase particles with an ingredient of Fe, the Fe particles are embedded in the La matrix, wherein the shape of the Fe particle is sub-spheroidal, and the particle size of the Fe particle is in a range of 3 nm to 300 nm. The volume content of the Fe particles in the intermediate alloy powder is about 18%; the impurities are enriched in the La matrix during the solidification process.
[0301] The Fe particles and the oxidized La matrix (Lanthanum oxide powder) are separated from each other by an autoxidation-powdering process, in which the La matrix can be autoxidated and the Fe particles can be separated by their magnetic property, then nanometer Fe powders with a particle size being in a range of 2 m to 50 m are obtained, and the total content of H, O, N, S, P, F, Cl, I and Br in the Fe.sub.50Ni.sub.50 powders is lower than 1900 ppm.
Example 15
[0302] This example provides a preparation method for sub-micron-level and micron-level Fe powders, which includes the following steps:
[0303] An alloy with the atomic percentage formula of La.sub.40Fe.sub.60 is selected, raw materials are weighed according to the formulation, after the initial alloy raw material is uniformly molten, the alloy melt is solidified and atomized through a water atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 100 m to 8 mm are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix with an ingredient of La and multiple high-melting-point first-phase particles with an ingredient of Fe, the Fe particles are embedded in the La matrix, wherein the shape of the Fe particle is sub-spheroidal or dendritic, and the particle size of the Fe particle is in a range of 100 nm to 10 m. The volume content of the Fe particles in the intermediate alloy powder is about 32%; the impurities are enriched in the La matrix during the solidification process.
[0304] The Fe particles and the oxidized La matrix (Lanthanum oxide powder) are separated from each other by an autoxidation-powdering process, in which the La matrix can be autoxidated and the Fe particles can be separated by their magnetic property, then Fe powders with a particle size being in a range of 100 nm to 10 m are obtained, and the total content of H, O, N, S, P, F, Cl, I and Br in the Fe powders is lower than 1600 ppm.
[0305] The obtained Fe powders are further graded, to obtain the sub-micron Fe powders with a particle size in a range of 100 nm to 1 m, and the ultrafine micron-level Fe powders with a particle size in a range of 1 m to 10 m.
Example 16
[0306] This example provides a preparation method for nanometer Ti powders and application thereof. The preparation method includes the following steps:
[0307] Sponge Ti and rare earth Ce raw material with the atomic percent contents of an impurity element T (including O, H, N, P, S, F, Cl, Br, and I) being 3 at. % and 2.5 at. % are selected respectively. The sponge Ti and rare earth Ce are sufficiently molten according to an approximate molar ratio of Ce:Ti being 2:1, so as to obtain a homogeneous initial alloy melt with the major atomic percent content being Ce.sub.64.9Ti.sub.32.5T.sub.2.6.
[0308] The initial alloy melt is solidified and atomized through a water atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 5 m to 80 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix with a major ingredient of Ce.sub.96.3T.sub.3.7 and multiple first-phase particles with a major ingredient of Ti.sub.99.7T.sub.0.3, the Ti.sub.99.7T.sub.0.3 particles are embedded in the Ce.sub.96.3T.sub.3.7 matrix, wherein the shape of the Ce.sub.96.3T.sub.3.7 particle is sub-spheroidal, and the particle size of the Ti.sub.99.7T.sub.0.3 particle is in a range of 5 nm to 150 nm. The volume content of the Ti.sub.99.7T.sub.0.3 particles in the intermediate alloy powder is about 19.5%; The Ce.sub.96.3T.sub.3.7 matrix in the intermediate alloy powder is removed by a dilute acid, so that the Ti.sub.99.7T.sub.0.3 particle which is difficult to react with the dilute acid can be separated, then the nanometer Ti.sub.99.7T.sub.0.3 powders with a particle size being in a range of 5 nm to 150 nm are obtained, the nanometer Ti.sub.99.7T.sub.0.3 powders are finer than the intermediate alloy powder, and the total content of H, O, N, S, P, F, Cl, I and Br in the Ti.sub.99.7T.sub.0.3 powders is 0.3 at. %.
[0309] Under the protective atmosphere, the nanometer powder with the major ingredient being Ti.sub.99.7T.sub.0.3 and epoxy resin and other painting components are mixed to prepare a nanometer Ti-modified polymer corrosion-resistant painting.
Example 17
[0310] This example provides a preparation method for sub-micron TiNb powders, which includes the following steps:
[0311] Sponge Ti, Nb sheets, and rare earth Gd raw material with the atomic percent contents of an impurity element T (including O, H, N, P, S, F, Cl, Br, and I) being 3 at. %, 1 at. % and 2.5 at. % are selected respectively. The sponge Ti, Nb sheets, and rare earth Gd are sufficiently molten according to an approximate molar ratio of Gd:Ti:Nb being 3:1:1, so as to obtain a homogeneous initial alloy melt with the major atomic percent content being Gd.sub.58.7Ti.sub.19.5Nb.sub.19.5T.sub.2.3.
[0312] The initial alloy melt is solidified and atomized through a gas atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 15 m to 150 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix with a major ingredient of Gd.sub.96.4T.sub.3.6 and multiple first-phase particles with a major ingredient of Ti.sub.49.88Nb.sub.49.88T.sub.0.24, the Ti.sub.49.88Nb.sub.49.88T.sub.0.24 particles are embedded in the Gd.sub.96.4T.sub.3.6 matrix, wherein the shape of the Ti.sub.49.88Nb.sub.49.88T.sub.0.24 particle is sub-spheroidal, and the particle size of the Ti.sub.49.88Nb.sub.49.88T.sub.0.24 particle is in a range of 50 nm to 500 nm. The volume content of the Ti.sub.49.88Nb.sub.49.88T.sub.0.24 particles in the intermediate alloy powder is about 26%; The Gd.sub.96.4T.sub.3.6 matrix in the intermediate alloy powder is removed by dilute acid, so that the Ti.sub.49.88Nb.sub.49.88T.sub.0.24 particle which is difficult to react with the dilute acid can be separated, then the sub-micron Ti.sub.49.88Nb.sub.49.88T.sub.0.24 powders with a particle size being in a range of 50 nm to 500 nm are obtained, the sub-micron Ti.sub.49.88Nb.sub.49.88T.sub.0.24 powders are finer than the intermediate alloy powder, and the total content of H, O, N, S, P, F, Cl, I and Br in the Ti.sub.49.88Nb.sub.49.88T.sub.0.24 powders is 0.24 at. %.
Example 18
[0313] This example provides a preparation method for micron Ti powders, which includes the following steps:
[0314] Ti and rare earth Ce raw material with the atomic percent contents of an impurity element T (including O, H, N, P, S, F, Cl, Br, and I) being 1 at. % and 2.5 at. % are selected respectively.
[0315] The Ti and rare earth Ce are sufficiently molten according to an approximate molar ratio of Ce:Ti being 5:95, so as to obtain a homogeneous initial alloy melt with the major atomic percent content being Ce.sub.4.9Ti.sub.94T.sub.1.1.
[0316] The initial alloy melt is solidified and atomized through a gas atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 15 m to 100 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix shell with a major ingredient of Ce.sub.86T.sub.14 and a single first-phase particle with a major ingredient of Ti.sub.99.7T.sub.0.3, the core Ti.sub.99.7T.sub.0.3 particle is embedded in the Ce.sub.86T.sub.14 matrix shell, wherein the particle size of the core Ti.sub.99.7T.sub.0.3 particle is in a range of 14.5 m to 97 m. The volume content of the Ti.sub.99.7T.sub.0.3 particle in the intermediate alloy powder is about 91%; The Ce.sub.86T.sub.14 matrix shell in the intermediate alloy powder is removed by a dilute acid, so that the Ti.sub.99.7T.sub.0.3 particle which is difficult to react with the dilute acid can be separated, then the micron Ti.sub.99.7T.sub.0.3 powders with a particle size being in a range of 14.5 m to 97 m are obtained, and the total content of H, O, N, S, P, F, Cl, I and Br in the Ti.sub.99.7T.sub.0.3 powders is 0.3 at. %.
Example 19
[0317] This example provides a preparation method for nano or sub-micron Fe powders, which includes the following steps:
[0318] Fe sheets and La raw material with the atomic percent contents of an impurity element T (including O, H, N, P, S, F, Cl, Br, and I) being 1 at. % and 2.5 at. % are selected respectively.
[0319] The Fe sheets and La raw materials are sufficiently molten according to an approximate molar ratio of La:Fe being 3:2, so as to obtain a homogeneous initial alloy melt with the major atomic percent content being La.sub.58.5Fe.sub.39.6T.sub.1.9.
[0320] The initial alloy melt is solidified and atomized through a gas atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 15 m to 150 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix with a major ingredient of La.sub.97T.sub.3 and multiple dispersed first-phase particles with a major ingredient of Fe.sub.99.75T.sub.0.25. Wherein the shape of the first-phase Fe.sub.99.75T.sub.0.25 particles is sub-spheroidal or dendritic, and the particle size of the Fe.sub.99.75T.sub.0.25 particles is in a range of 50 nm to 600 nm. The volume percent content of the first-phase Fe.sub.99.75T.sub.0.25 particles in the intermediate alloy powder is about 18%; The Fe.sub.99.75T.sub.0.25 particles and the oxidized La.sub.97T.sub.3 matrix (Lanthanum oxide powder) are separated from each other by an autoxidation-powdering process, in which the La.sub.97T.sub.3 matrix can be autoxidated and the Fe.sub.99.75T.sub.0.25 particles can be separated by their magnetic property, then nano or sub-micron Fe.sub.99.75T.sub.0.25 powders with a particle size being in a range of 50 nm to 600 nm are obtained, and the total content of H, O, N, S, P, F, Cl, I and Br in the Fe.sub.99.75T.sub.0.25 powders is 0.25 at. %.
Example 20
[0321] This example provides a preparation method for micron-level spheroidal TiNi powders, which includes the following steps:
[0322] Ti raw material, Ni sheets, and rear earth Gd raw material with the atomic percent contents of an impurity element T (including O, H, N, P, S, F, Cl, Br, and I) being 1 at. %, 0.5 at. % and 2.5 at. % are selected respectively. The initial raw materials are sufficiently molten according to an approximate molar ratio of Gd:Ti:Ni being 5:47.5:47.5, so as to obtain a homogeneous initial alloy melt with the major atomic percent content being Gd.sub.4.9Ti.sub.47.1Ni.sub.47.1T.sub.0.9.
[0323] The initial alloy melt is solidified and atomized through a gas atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 15 m to 100 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix shell with a major ingredient of Gd.sub.87.5T.sub.12.5 and a single first-phase particle with a major ingredient of Ti.sub.49.9Ni.sub.49.9T.sub.0.2, the core Ti.sub.49.9Ni.sub.49.9T.sub.0.2 particle is embedded in the Gd.sub.87.5T.sub.12.5 matrix shell, wherein the particle size of the core Ti.sub.49.9Ni.sub.49.9T.sub.0.2 particle is in a range of 14.5 m to 97 m. The volume content of the first-phase Ti.sub.49.9Ni.sub.49.9T.sub.0.2 particle in the intermediate alloy powder is about 89%; The Gd.sub.87.5T.sub.12.5 matrix shell in the intermediate alloy powder is removed by a dilute acid, so that the Ti.sub.49.9Ni.sub.49.9T.sub.0.2 particle which is difficult to react with the dilute acid can be separated, then the micrometer Ti.sub.49.9Ni.sub.49.9T.sub.0.2 powders and with a particle size being in a range of 14.5 m to 97 m are obtained, and the total content of H, O, N, S, P, F, Cl, I and Br in the Ti.sub.49.9Ni.sub.49.9T.sub.0.2 powders is 0.2 at. %.
Example 21
[0324] This example provides a preparation method for nanometer TiVAl alloy powders, which includes the following steps:
[0325] Sponge Ti, V sheets, rare earth Ce and Al raw material with the atomic percent contents of an impurity element T (including O, H, N, P, S, F, Cl, Br, and I) being 3 at. %, 1 at. %, 2.5 at. % and 0.2 at. % are selected respectively. The initial raw materials are sufficiently molten according to a calculated molar ratio so as to obtain a homogeneous initial alloy melt with the major atomic percent content being Ce.sub.70.5Al.sub.10(Ti.sub.96V.sub.4).sub.17T.sub.2.5.
[0326] The initial alloy melt is solidified and atomized through a water atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 5 m to 100 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix with a major ingredient of Ce.sub.86.5Al.sub.10.5T.sub.3 and multiple dispersed first-phase particles with a major ingredient of (Ti.sub.96V.sub.4).sub.92.25Al.sub.7.5T.sub.0.25, the (Ti.sub.96V.sub.4).sub.92.25Al.sub.7.5T.sub.0.25 particles are embedded in the Ce.sub.86.5Al.sub.10.5T.sub.3 matrix, wherein the shape of the (Ti.sub.96V.sub.4).sub.92.25Al.sub.7.5T.sub.0.25 particle is sub-spheroidal, and the particle size of the (Ti.sub.96V.sub.4).sub.92.25Al.sub.7.5T.sub.0.25 particle is in a range of 10 nm to 200 nm. The volume content of the (Ti.sub.96V.sub.4).sub.92.25Al.sub.7.5T.sub.0.25 particles in the intermediate alloy powder is about 12%; The Ce.sub.86.5Al.sub.10.5T.sub.3 matrix in the intermediate alloy powder is removed by a dilute acid, so that the (Ti.sub.96V.sub.4).sub.92.25Al.sub.7.5T.sub.0.25 particle which is difficult to react with the dilute acid can be separated, then the nano (Ti.sub.96V.sub.4).sub.92.25Al.sub.7.5T.sub.0.25 powders with a particle size being in a range of 50 nm to 200 nm are obtained, the nano (Ti.sub.96V.sub.4).sub.92.25Al.sub.7.5T.sub.0.25 powders are finer than the intermediate alloy powder, and the total content of H, O, N, S, P, F, Cl, I and Br in the (Ti.sub.96V.sub.4).sub.92.25Al.sub.7.5T.sub.0.25 powders is 0.25 at. %.
[0327] Under the protective atmosphere, the nanometer powder with the major ingredient being (Ti.sub.96V.sub.4).sub.92.25Al.sub.7.5T.sub.0.25 and epoxy resin and other painting components are mixed to prepare a nanometer Ti alloy modified polymer corrosion-resistant painting.
Example 22
[0328] This example provides a preparation method for micrometer TiVAl alloy powders, which includes the following steps:
[0329] Sponge Ti, V sheets, rare earth Ce and Al raw material with the atomic percent contents of an impurity element T (including O, H, N, P, S, F, Cl, Br, and I) being 1 at. %, 1 at. %, 1 at. % and 1 at. % are selected respectively. The initial raw materials are sufficiently molten according to a calculated molar ratio so as to obtain a homogeneous initial alloy melt with the major atomic percent content being Ce.sub.4.5Al.sub.0.5(Ti.sub.96V.sub.4).sub.94T.sub.1.
[0330] The initial alloy melt is solidified and atomized through a gas atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 5 m to 80 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix with a major ingredient of Ce.sub.8.2Al.sub.1.8T.sub.16.2 and a first-phase particle with a major ingredient of (Ti.sub.96V.sub.4).sub.99.5Al.sub.0.4T.sub.0.1. The particle size of the (Ti.sub.96V.sub.4).sub.99.5Al.sub.0.4T.sub.0.1 particle is in a range of 4.85 m to 78 m, and the shape of the (Ti.sub.96V.sub.4).sub.99.5Al.sub.0.4T.sub.0.1 particle is sub-spheroidal; The structure of the intermediate alloy powder is a shell-core structure, a single first-phase particle is wrapped in the second-phase matrix shell, and the volume percent content of the (Ti.sub.96V.sub.4).sub.99.5Al.sub.0.4T.sub.0.1 particle in the intermediate alloy powder is about 90%; The Ce.sub.82Al.sub.1.8Ti.sub.6.2 matrix in the intermediate alloy powder is removed by a dilute acid, so that the (Ti.sub.96V.sub.4).sub.99.5Al.sub.0.4T.sub.0.1 particle which is difficult to react with the dilute acid can be separated, then the (Ti.sub.96V.sub.4).sub.99.5Al.sub.0.4T.sub.0.1 powders and with a particle size being in a range of 4.85 m to 78 m are obtained, and the total content of H, O, N, S, P, F, Cl, I and Br in the (Ti.sub.96V.sub.4).sub.99.5Al.sub.0.4T.sub.0.1 powders is 0.1 at. %.
[0331] The obtained spheroidal (Ti.sub.96V.sub.4).sub.99.5Al.sub.0.4T.sub.0.1 alloy powder can be applied in fields of powder metallurgy, injection molding, or metal 3D printing.
Example 23
[0332] This example provides a preparation method for micrometer Nb powders, which includes the following steps:
[0333] Nb and Cu raw materials with the atomic percent contents of an impurity element T (including O, H, N, P, S, F, Cl, Br, and I) being 0.5 at. % and 0.5 at. % are selected respectively.
[0334] The Nb and Cu raw materials are sufficiently molten according to an approximate molar ratio of Cu:Nb being 12:88, so as to obtain a homogeneous initial alloy melt with the major atomic percent content being Cu.sub.11.9Nb.sub.87.6T.sub.0.5.
[0335] The initial alloy melt is solidified and atomized through a gas atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 15 m to 100 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix shell with a major ingredient of Cu.sub.97.7T.sub.2.3 and a single first-phase particle with a major ingredient of Nb.sub.99.8T.sub.0.2, the core Nb.sub.99.8T.sub.0.2 particle is embedded in the Cu.sub.97.7T.sub.2.3 matrix shell, wherein the particle size of the core Cu.sub.97.7T.sub.2.3 particle is in a range of 14.5 m to 97 m and the shape of the Nb.sub.99.8T.sub.0.2 particle is sub-spheroidal; The volume content of the Nb.sub.99.8T.sub.0.2 particle in the intermediate alloy powder is about 92%;
[0336] The Cu.sub.97.7T.sub.2.3 matrix shell in the intermediate alloy powder is removed by a concentrated hydrochloric acid solution, so that the core Nb.sub.99.8T.sub.0.2 particle which is difficult to react with the concentrated hydrochloric acid solution can be separated, then the micron Nb.sub.99.8T.sub.0.2 powders with a particle size being in a range of 14.5 m to 97 m are obtained, and the total content of H, O, N, S, P, F, Cl, I and Br in the Nb.sub.99.8T.sub.0.2 powders is 0.2 at. %.
Example 24
[0337] This example provides a preparation method for sub-micron Si powders, which includes the following steps:
[0338] Si and Zn raw materials with the atomic percent contents of an impurity element T (including O, H, N, P, S, F, Cl, Br, and I) being 0.5 at. % and 0.5 at. % are selected respectively. The initial raw materials are sufficiently molten according to an approximate molar ratio of Si:Zn being 30:70, so as to obtain a homogeneous initial alloy melt with the major atomic percent content being Si.sub.29.85Zn.sub.69.65T.sub.0.5.
[0339] The initial alloy melt is solidified and atomized through a gas atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 15 m to 100 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix with a major ingredient of Zn.sub.99.35T.sub.0.65 and multiple dispersed first-phase particles with a major ingredient of Si.sub.97.83T.sub.0.17, the Si.sub.97.83T.sub.0.17 particles are embedded in the Zn.sub.99.35T.sub.0.65 matrix, wherein the shape of the Si.sub.97.83T.sub.0.17 particle is sub-spheroidal, and the particle size of the Si.sub.97.83T.sub.0.17 particle is in a range of 100 nm to 2 m. The volume content of the Si.sub.97.83T.sub.0.17 particles in the intermediate alloy powder is about 36%;
[0340] The Zn.sub.99.35T.sub.0.65 matrix in the intermediate alloy powder is removed by hydrochloric acid solution, so that the Si.sub.97.83T.sub.0.17 particle which is difficult to react with the hydrochloric acid solution can be separated, then the sub-micron Si.sub.97.83T.sub.0.17 powders with a particle size being in a range of 100 nm to 2 m are obtained, and the total content of H, O, N, S, P, F, Cl, I and Br in the Si.sub.97.83T.sub.0.17 powders is 0.17 at. %.
Example 25
[0341] This example provides a preparation method for micrometer Si powders, which includes the following steps:
[0342] Si and Zn raw materials with the atomic percent contents of an impurity element T (including O, H, N, P, S, F, Cl, Br, and I) being 0.5 at. % and 0.5 at. % are selected respectively.
[0343] The initial raw materials are sufficiently molten according to an approximate molar ratio of Si:Zn being 90:10, so as to obtain a homogeneous initial alloy melt with the major atomic percent content being Si.sub.89.55Zn.sub.9.95T.sub.0.5.
[0344] The initial alloy melt is solidified and atomized through a gas atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 15 m to 100 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix with a major ingredient of Zn.sub.96.1T.sub.3.9 and a first-phase particle with a major ingredient of Si.sub.99.1T.sub.0.1. The structure of the intermediate alloy powder is a shell-core structure, in which a single first-phase particle is inside, and the second-phase matrix is outside and wraps the first-phase particle. The particle size of the Si.sub.99.1T.sub.0.1 particle is in a range of 14.5 m to 97 m, the shape of the Si.sub.99.1T.sub.0.1 particle is sub-spheroidal, and the volume percent content of the Si.sub.99.1T.sub.0.1 particle in the intermediate alloy powder is about 92%;
[0345] The Zn.sub.96.1T.sub.3.9 matrix in the intermediate alloy powder is removed by hydrochloric acid solution, so that the Si.sub.97.83T.sub.0.17 particle which is difficult to react with the hydrochloric acid solution can be separated, then the micrometer Si.sub.99.1T.sub.0.1 powders and with a particle size being in a range of 14.5 m to 97 m are obtained, and the total content of H, O, N, S, P, F, Cl, I and Br in the Si.sub.99.1T.sub.0.1 powders is 0.1 at. %.
Example 26
[0346] This example provides a preparation method for nanometer CuSi powders, which includes the following steps:
[0347] Si raw material, Cu raw material, and Pb raw material with the atomic percent contents of an impurity element T (including O, H, N, P, S, F, Cl, Br, and I) being 0.5 at. %, 0.5 at. % and 0.5 at. % are selected respectively. The initial raw materials are sufficiently molten, wherein the approximate molar ratio of Cu:Si is 90:10, so as to obtain a homogeneous initial alloy melt with the major atomic percent content being Pb.sub.74.5(Cu.sub.90Si.sub.10).sub.25T.sub.0.5.
[0348] The initial alloy melt is solidified and atomized through a water atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 5 m to 80 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix with a major ingredient of Pb.sub.99.4T.sub.0.6 and multiple dispersed first-phase particles with a major ingredient of (Cu.sub.90Si.sub.10).sub.99.8T.sub.0.2, the (Cu.sub.90Si.sub.10).sub.99.8T.sub.0.2 particles are embedded in the Pb.sub.99.4T.sub.0.6 matrix, wherein the shape of the (Cu.sub.90Si.sub.10).sub.99.8T.sub.0.2 particle is sub-spheroidal, and the particle size of the (Cu.sub.90Si.sub.10).sub.99.8T.sub.0.2 particle is in a range of 5 nm to 150 m. The volume content of the (Cu.sub.90Si.sub.10).sub.99.8T.sub.0.2 particles in the intermediate alloy powder is about 12%;
[0349] The Pb.sub.99.4T.sub.0.6 matrix in the intermediate alloy powder is removed by a dilute hydrochloric acid-acetic acid mixed solution, so that the (Cu.sub.90Si.sub.10).sub.99.8T.sub.0.2 particle which is difficult to react with the diluted hydrochloric acid-acetic acid mixed solution can be separated, then the nano (Cu.sub.90Si.sub.10).sub.99.8T.sub.0.2 powders and with a particle size being in a range of 5 nm to 150 m are obtained, and the total content of H, O, N, S, P, F, Cl, I and Br in the (Cu.sub.90Si.sub.10).sub.99.8T.sub.0.2 powders is 0.2 at. %.
Example 27
[0350] This example provides a preparation method for nanometer Ti powders and application thereof. The preparation method includes the following steps:
[0351] Sponge Ti and rare earth Ce raw materials with the atomic percent contents of an impurity element T (including O, H, N, P, S, F, Cl, Br, and I) being 3 at. % and 2.5 at. % are selected respectively. The sponge Ti further contains 0.5 at. % of Mn; the rare earth Ce further contains 0.7 at. % of Mg. The sponge Ti and rare earth Ce are sufficiently molten according to an approximate molar ratio of Ce:Ti being 2:1, so as to obtain a homogeneous initial alloy melt with the major atomic percent content being (Ce.sub.99.3Mg.sub.0.7).sub.64.9(Ti.sub.99.5Mn.sub.0.5).sub.32.5T.sub.2.6.
[0352] The initial alloy melt is solidified and atomized through a water atomization process, then sub-spheroidal intermediate alloy powders with a particle size of 5 m to 80 m are obtained. The solidification structure of the intermediate alloy powder is composed of a second-phase matrix with a major ingredient of (Ce.sub.99.3Mg.sub.0.7).sub.96.3T.sub.3.7 and multiple dispersed first-phase particles with a major ingredient of (Ti.sub.99.5Mn.sub.0.5).sub.99.7T.sub.0.3, the (Ti.sub.99.5Mn.sub.0.5).sub.99.7T.sub.0.3 particles are embedded in the (Ce.sub.99.3Mg.sub.0.7).sub.96.3T.sub.3.7 matrix, wherein the shape of the (Ti.sub.99.5Mn.sub.0.5).sub.99.7T.sub.0.3 particle is sub-spheroidal, and the particle size of the (Ti.sub.99.5Mn.sub.0.5).sub.99.7T.sub.0.3 particle is in a range of 5 nm to 150 m. The volume content of the (Ti.sub.99.5Mn.sub.0.5).sub.99.7T.sub.0.3 particles in the intermediate alloy powder is about 19.5%;
[0353] The (Ce.sub.99.3Mg.sub.0.7).sub.96.3T.sub.3.7 matrix in the intermediate alloy powder is removed by a dilute acid solution, so that the (Ti.sub.99.5Mn.sub.0.5).sub.99.7T.sub.0.3 particle which is difficult to react with the diluted acid solution can be separated, then the nano (Ti.sub.99.5Mn.sub.0.5).sub.99.7T.sub.0.3 powders and with a particle size being in a range of 5 nm to 150 m are obtained, the nano (Ti.sub.99.5Mn.sub.0.5).sub.99.7T.sub.0.3 powders are finer than the intermediate alloy powder, and the total content of H, O, N, S, P, F, Cl, I and Br in the (Ti.sub.99.5Mn.sub.0.5).sub.99.7T.sub.0.3 powders is 0.3 at. %.
[0354] Under the protective atmosphere, the nanometer powder with the major ingredient being (Ti.sub.99.5Mn.sub.0.5).sub.99.7T.sub.0.3 and epoxy resin and other painting components are mixed to prepare a nanometer Ti-modified polymer corrosion-resistant painting.
[0355] The technical features of the above examples may be arbitrarily combined. For conciseness, all possible combinations of the technical features of the above embodiments have not been completely described. However, as long as there is no contradiction between the combinations of these technical features, they shall be considered to be within the scope of the present disclosure.
[0356] The above examples only express several embodiments of the disclosure, and their descriptions are more specific and detailed, but they cannot be interpreted as a limitation on the scope of the present disclosure. It should be noted that for one of ordinary skill in the art, several variations and improvements may be made without deviating from the concept of the disclosure, which all fall within the scope of protection of the disclosure. Therefore, the scope of protection of the present disclosure shall be subject to the attached claims.