CN111172428A - High-purity nickel powder and preparation method thereof - Google Patents
High-purity nickel powder and preparation method thereof Download PDFInfo
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- CN111172428A CN111172428A CN202010046537.7A CN202010046537A CN111172428A CN 111172428 A CN111172428 A CN 111172428A CN 202010046537 A CN202010046537 A CN 202010046537A CN 111172428 A CN111172428 A CN 111172428A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
- C23C24/02—Coating starting from inorganic powder by application of pressure only
- C23C24/04—Impact or kinetic deposition of particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0848—Melting process before atomisation
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
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Abstract
The invention relates to high-purity nickel powder and a preparation method thereof. The high-purity nickel powder comprises the following components in percentage by mass: ni: not less than 99.7 percent; o is less than or equal to 0.2 percent; c is less than or equal to 0.05 percent; fe is less than or equal to 0.02 percent; the impurity is less than or equal to 0.03 percent. The high-purity nickel powder has the advantages of small particle diameter and small magnetism by strictly controlling the proportion of the components, so that the coating formed by spraying has better performance in the aspects of density, uniformity, binding force and the like, and other coating materials can be well combined with the high-purity nickel powder coating serving as the intermediate coating.
Description
Technical Field
The invention relates to the field of spraying materials, in particular to high-purity nickel powder and a preparation method thereof.
Background
The thermal spraying technology is a processing method which uses gas, liquid fuel or electric arc, plasma arc, laser and the like as heat sources, heats powdered or filiform metals, alloys, ceramics, oxides, carbides, plastics, nylon and composite materials thereof to a molten or semi-molten state, atomizes the materials by the power of the heat sources or external high-speed airflow, and sprays the atomized materials to the surface of a pretreated workpiece at a certain speed to form a surface layer with firm adhesion.
Cold spray is a technique of forming a coating by allowing a supersonic flow to remain in an original solid state without melting or vaporizing a powder material and causing the powder material to impinge on a substrate, and the powder material is plastically deformed at a particle body exceeding a critical velocity under supersonic impact to form a coating. The material is not affected by heat to cause characteristic change, and the oxidation of the coating film can be controlled to the minimum.
Pure nickel powder is used as a paramagnetic material, and the magnetism of the pure nickel powder can influence the combination of metal particles and a base material in a cold spraying operation environment, so that the problems of poor combination force, uneven coating and the like of the coating are caused; on the other hand, the conventional pure nickel powder has larger particle diameter, which further causes the problems of low density, poor uniformity, poor bonding force and the like of a coating formed by spraying.
In view of the problems in the prior art, it is urgently needed to develop a high-purity nickel powder and a preparation method thereof, so that the prepared high-purity nickel powder has the advantages of small particle size and small magnetism, and the coating formed by spraying has better performance.
Disclosure of Invention
In order to solve the technical problems, the invention provides high-purity nickel powder and a preparation method thereof. The high-purity nickel powder has the advantages of small particle diameter and small magnetism by strictly controlling the proportion of the components, so that the coating formed by spraying has better performance in the aspects of density, uniformity, binding force and the like, and other coating materials can be well combined with the high-purity nickel powder coating serving as the intermediate coating.
In order to achieve the purpose, the invention adopts the following technical scheme:
one purpose of the invention is to provide high-purity nickel powder, which comprises the following components in percentage by mass:
the impurities in the high-purity nickel powder of the present invention include any one or a combination of at least two of P, S, H, Cu, and Mg, and typical but non-limiting examples of such combinations are: combinations of P and S, P and H, H and Cu, Cu and Mg, P, S and H or P, S, H, Cu and Mg, and the like.
The high-purity nickel powder provided by the invention can provide possibility for reducing the particle diameter length and reducing the magnetism from the aspect of product proportion by strictly controlling the proportion of each component, so that the performance of a coating formed by spraying is better in the aspects of compactness, uniformity, binding force and the like, and the high-purity nickel powder coating serving as an intermediate coating can be well combined with other coating materials.
In a preferred embodiment of the present invention, the high purity nickel powder has a particle size of 2 to 10 μm, for example, 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm, or 10 μm, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the high purity nickel powder has a particle hardness of 150 to 180Hv, for example, 150Hv, 155Hv, 160Hv, 165Hv, 170Hv, 175Hv, 180Hv, etc., but is not limited to the recited values, and other values not recited within the range of values are also applicable.
Preferably, the high purity nickel powder has a particle out-of-roundness of 30 to 50%, such as 30%, 32%, 35%, 37%, 40%, 43%, 45%, 48%, or 50%, but not limited to the recited values, and other values not recited within the range of values are equally applicable.
Preferably, the high-purity nickel powder has a relative magnetic permeability of 900 to 1300, such as 900, 950, 1000, 1050, 1100, 1120, 1150, 1170, 1200, 1250, 1270, or 1300, but is not limited to the recited values, and other values not recited within the range of values are equally applicable.
Preferably, the high purity nickel powder has an oxygen content of 0.2% or less, such as 0.03, 0.05%, 0.07%, 0.09%, 0.1%, 0.12%, 0.14%, 0.15%, 0.16%, 0.18%, or 0.2%, but not limited to the recited values, and other values not recited in this range are also applicable.
The second object of the present invention is to provide a method for preparing the high purity nickel powder, which comprises the following steps:
(1) heating and melting the high-purity nickel coarse powder into nickel metal liquid;
(2) atomizing and condensing the nickel metal liquid obtained in the step (1);
(3) screening the product obtained in the step (2);
(4) and (4) drying the screened product obtained in the step (3) to obtain the high-purity nickel powder.
As a preferable technical scheme of the invention, besides the high-purity nickel coarse powder in the step (1), a high-purity nickel ingot, a high-purity nickel bar or a high-purity nickel waste material can be used as a raw material.
As a preferred embodiment of the present invention, the high purity nickel coarse powder in step (1) has a particle size of 30 μm or more, for example, 30 μm, 32 μm, 33 μm, 35 μm, 38 μm, 40 μm, 45 μm, 47 μm, 50 μm, 55 μm or 65 μm, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
As a preferred embodiment of the present invention, the heating temperature in the step (1) is 1500 to 1800 ℃, for example 1500 ℃, 1530 ℃, 1550 ℃, 1600 ℃, 1650 ℃, 1700 ℃, 1750 ℃ or 1800 ℃ and the like, but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
As a preferable technical scheme of the invention, the heating and melting in the step (1) are in a protective gas environment.
Preferably, the shielding gas comprises any one of nitrogen, helium, neon or argon, or a combination of at least two of these, typical but non-limiting examples being: a combination of nitrogen and helium, a combination of nitrogen and neon, a combination of nitrogen and argon, a combination of helium and argon, or a combination of helium and neon, and the like.
As a preferable technical scheme of the invention, the atomization mode in the step (2) is vacuum gas atomization.
As a preferred embodiment of the present invention, the sieve size of the sieve in the step (3) is 2 to 10 μm, for example, 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm or 10 μm, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned numerical range are also applicable.
As a preferable technical scheme of the invention, the drying mode in the step (4) is heating and drying.
Preferably, the temperature for heat drying is 400-700 deg.C, such as 400 deg.C, 450 deg.C, 480 deg.C, 500 deg.C, 520 deg.C, 550 deg.C, 600 deg.C, 630 deg.C, 650 deg.C or 700 deg.C, but is not limited to the recited values, and other values not recited in the range of values are also applicable.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) placing high-purity nickel coarse powder with the particle size diameter being more than or equal to 30 mu m in a protective gas environment, and heating and melting the high-purity nickel coarse powder at 1500-1800 ℃ to obtain nickel metal liquid;
(2) atomizing and condensing the nickel metal liquid obtained in the step (1) in a vacuum gas atomization mode;
(3) screening the product obtained in the step (2); wherein the size of the screened mesh is 2-10 μm;
(4) and (4) heating and drying the screened product obtained in the step (3) at the temperature of 400-700 ℃ to obtain the high-purity nickel powder.
Compared with the prior art, the invention at least has the following beneficial effects:
(1) according to the high-purity nickel powder disclosed by the invention, the proportion of each component is strictly controlled, so that the prepared high-purity nickel powder has the advantages of smaller particle size and smaller magnetism, and the performance of a coating formed by spraying is further better in the aspects of density, uniformity, binding force and the like;
(2) the particle diameter of the high-purity nickel powder is 2-10 mu m, the relative magnetic permeability is 900-1300, and the high-purity nickel powder can be used as an intermediate coating and other coating materials to realize good combination;
(3) the coating obtained by using the high-purity nickel powder disclosed by the invention can maximally retain most of physicochemical characteristics such as the conductivity and corrosion resistance of the high-purity nickel.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides high-purity nickel powder, wherein the mass percent of Ni is 99.75%, and the mass percent of O is 0.18%; the mass percentage content of C is 0.04%; the mass percentage of Fe is 0.01%; the mass percentage content of the impurity consisting of P, S and H is 0.02%; the particle diameter length of the high-purity nickel powder is 8-10 mu m; the particle hardness of the high-purity nickel powder is 170 Hv; the particle out-of-roundness of the high-purity nickel powder is 40%; the relative magnetic permeability of the high-purity nickel powder is 1120; the oxygen content of the high-purity nickel powder is 0.18%.
The preparation method of the high-purity nickel powder comprises the following steps:
(1) placing high-purity nickel coarse powder with the particle size diameter of 47 mu m in an argon environment, and heating and melting the high-purity nickel coarse powder at 1650 ℃ to obtain nickel metal liquid;
(2) atomizing and condensing the nickel metal liquid obtained in the step (1) in a vacuum gas atomization mode;
(3) screening the product obtained in the step (2); wherein the size of the screened mesh is 8-10 μm;
(4) and (4) heating and drying the screened product obtained in the step (3) at 550 ℃ to obtain the high-purity nickel powder.
The high-purity nickel powder is sprayed on an aluminum alloy base material by cold spraying, and the obtained coating is subjected to hardness test, adhesion test and spraying thickness test, and relevant test results are shown in table 2.
Example 2
The embodiment provides high-purity nickel powder, wherein the mass percent of Ni is 99.7%, and the mass percent of O is 0.2%; the mass percentage content of C is 0.05%; the mass percentage of Fe is 0.02%; the mass percentage of the impurity consisting of P, S and H is 0.03%; the particle diameter length of the high-purity nickel powder is 5-8 mu m; the particle hardness of the high-purity nickel powder is 150 Hv; the particle out-of-roundness of the high-purity nickel powder is 30%; the relative magnetic permeability of the high-purity nickel powder is 1300; the oxygen content of the high-purity nickel powder is 0.2%.
The preparation method of the high-purity nickel powder comprises the following steps:
(1) placing high-purity nickel coarse powder with the particle size diameter of 55 mu m in an argon environment, and heating and melting the high-purity nickel coarse powder at 1800 ℃ to obtain nickel metal liquid;
(2) atomizing and condensing the nickel metal liquid obtained in the step (1) in a vacuum gas atomization mode;
(3) screening the product obtained in the step (2); wherein the size of the screened mesh is 5-8 μm;
(4) and (4) heating and drying the screened product obtained in the step (3) at 700 ℃ to obtain the high-purity nickel powder.
The high-purity nickel powder is sprayed on an aluminum alloy base material by cold spraying, and the obtained coating is subjected to hardness test, adhesion test and spraying thickness test, and relevant test results are shown in table 2.
Example 3
The embodiment provides high-purity nickel powder, wherein the mass percent of Ni is 99.84%, and the mass percent of O is 0.1%; the mass percentage content of C is 0.03%; the mass percentage of Fe is 0.013%; the mass percentage content of the impurity consisting of S, H and Cu is 0.017 percent; the particle diameter length of the high-purity nickel powder is 2-5 mu m; the particle hardness of the high-purity nickel powder is 180 Hv; the particle out-of-roundness of the high-purity nickel powder is 50%; the relative magnetic permeability of the high-purity nickel powder is 900; the oxygen content of the high-purity nickel powder is 0.1%.
The preparation method of the high-purity nickel powder comprises the following steps:
(1) placing high-purity nickel coarse powder with the particle size diameter of 65 mu m in an argon environment, and heating and melting the high-purity nickel coarse powder at 1500 ℃ to obtain nickel metal liquid;
(2) atomizing and condensing the nickel metal liquid obtained in the step (1) in a vacuum gas atomization mode;
(3) screening the product obtained in the step (2); wherein the size of the screened mesh is 2-5 μm;
(4) and (4) heating and drying the screened product obtained in the step (3) at the temperature of 400 ℃ to obtain the high-purity nickel powder.
The high-purity nickel powder is sprayed on an aluminum alloy base material by cold spraying, and the obtained coating is subjected to hardness test, adhesion test and spraying thickness test, and relevant test results are shown in table 2.
Example 4
In this example, the high purity nickel coarse powder obtained in step (1) of example 1 was replaced with a high purity nickel ingot, and the other conditions were the same as those in example 1.
The high-purity nickel powder is sprayed on an aluminum alloy base material by cold spraying, and the obtained coating is subjected to hardness test, adhesion test and spraying thickness test, and relevant test results are shown in table 2.
And (3) performance testing:
the hardness test, adhesion test and spray thickness test methods for the coatings prepared in examples 1 to 4 were as follows:
(a) and (3) hardness testing: adopting a micro Vickers hardness tester, selecting a diamond regular rectangular pyramid pressure head by a testing head, keeping the pressure for 10s when the pressure F is 0.3 Kgf;
(b) and (3) testing the adhesive force: cleaning the surface of the coating, and scratching 10 multiplied by 10 small grids of 1mm multiplied by 1mm on the surface of the tested coating by using a sharp blade (the angle of the blade is 25 degrees, and the thickness of the blade is 0.43 mm); each scribing line should be deep to the bottom layer of the coating; brushing fragments in the test area with a brush; firmly sticking the tested small grid with a 10N/25mm adhesive tape (NICIBAN CT405AP-24 gummed paper), pressing the adhesive tape with a nail (the nail cannot damage the adhesive tape), and removing air bubbles between the adhesive tape and the coating to increase the contact area and force between the adhesive tape and the tested area; standing for 90s, grasping one end of the adhesive tape by hand, tearing off the adhesive tape in the 60-degree direction within 0.5-1 s, and then checking the falling-off condition of the coating by using a 5-time magnifier;
and (4) judging the adhesive force: dividing the advantages and disadvantages of the adhesive force into 6 grades, wherein the grades are 5B, 4B, 3B, 2B, 1B and 0B from the advantages to the disadvantages in sequence; the meaning of the above grades is shown in table 1:
TABLE 1
(c) And (3) testing the spraying thickness: the high-purity nickel powder is repeatedly sprayed on the aluminum alloy substrate five times under the same cold spraying condition, and then an electronic film thickness meter (American Filmetrics company, model F10-HC) is used for repeatedly measuring 3 times and averaging to obtain five spraying thicknesses.
The coatings prepared in examples 1 to 4 were subjected to hardness test, adhesion test and spray thickness test, and the results of the tests are shown in table 2.
TABLE 2
| Vickers hardness/Hv | Adhesion test results | Five times of spraying thickness/mum | |
| Example 1 | 168 | 5B | 19.8 |
| Example 2 | 172 | 4B | 19.5 |
| Example 3 | 173 | 4B | 18.8 |
| Example 4 | 156 | 4B | 18.3 |
As can be seen from Table 2, the coatings prepared in the examples 1 to 4 of the present invention have high hardness, and the Vickers hardness thereof is 150 to 175 Hv; the adhesion force of the coating on the surface of the base material is also strong, and the adhesion force test results are all more than 4B; the spraying thickness of the coating on the surface of the base material is also higher, and the results of five times of spraying thickness tests are all more than 18 mu m. In conclusion, the high-purity nickel powder provided by the invention has the advantages of smaller particle diameter and smaller magnetism, so that the performance of the coating formed by spraying is better in the aspects of compactness, uniformity, binding force and the like.
The applicant states that the present invention is illustrated by the above examples to show the detailed process equipment and process flow of the present invention, but the present invention is not limited to the above detailed process equipment and process flow, i.e. it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. The high-purity nickel powder is characterized by comprising the following components in percentage by mass:
2. the high-purity nickel powder according to claim 1, wherein the high-purity nickel powder has a particle size of 2 to 10 μm;
preferably, the particle hardness of the high-purity nickel powder is 150-180 Hv;
preferably, the particle out-of-roundness of the high-purity nickel powder is 30-50%;
preferably, the high-purity nickel powder has the relative magnetic permeability of 900-1300;
preferably, the oxygen content of the high-purity nickel powder is less than or equal to 0.2 percent.
3. A method for producing high purity nickel powder as claimed in any one of claims 1 or 2, comprising the steps of:
(1) heating and melting the high-purity nickel coarse powder into nickel metal liquid;
(2) atomizing and condensing the nickel metal liquid obtained in the step (1);
(3) screening the product obtained in the step (2);
(4) and (4) drying the screened product obtained in the step (3) to obtain the high-purity nickel powder.
4. The preparation method according to claim 3, wherein the high purity nickel coarse powder in the step (1) has a particle size of 30 μm or more.
5. The method according to claim 3 or 4, wherein the heating temperature in the step (1) is 1500 to 1800 ℃.
6. The production method according to any one of claims 3 to 5, wherein the heating and melting of step (1) is in a protective gas atmosphere;
preferably, the shielding gas comprises any one of nitrogen, helium, neon or argon or a combination of at least two thereof.
7. The production method according to any one of claims 3 to 6, wherein the atomization in step (2) is vacuum atomization.
8. The production method according to any one of claims 3 to 7, wherein the mesh size of the screen in the step (3) is 2 to 10 μm.
9. The production method according to any one of claims 3 to 8, wherein the drying manner in the step (4) is heat drying;
preferably, the temperature for heating and drying is 400-700 ℃.
10. The method according to any one of claims 3 to 9, characterized by comprising the steps of:
(1) placing high-purity nickel coarse powder with the particle size diameter being more than or equal to 30 mu m in a protective gas environment, and heating and melting the high-purity nickel coarse powder at 1500-1800 ℃ to obtain nickel metal liquid;
(2) atomizing and condensing the nickel metal liquid obtained in the step (1) in a vacuum gas atomization mode;
(3) screening the product obtained in the step (2); wherein the size of the screened mesh is 2-10 μm;
(4) and (4) heating and drying the screened product obtained in the step (3) at the temperature of 400-700 ℃ to obtain the high-purity nickel powder.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009024198A (en) * | 2007-07-18 | 2009-02-05 | Sanyo Special Steel Co Ltd | Method for manufacturing sputtering target material for nickel-tangsten based interlayer |
| CN103866351A (en) * | 2012-12-14 | 2014-06-18 | 重庆华浩冶炼有限公司 | Electrolytic preparation method of nickel powder |
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2020
- 2020-01-16 CN CN202010046537.7A patent/CN111172428A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009024198A (en) * | 2007-07-18 | 2009-02-05 | Sanyo Special Steel Co Ltd | Method for manufacturing sputtering target material for nickel-tangsten based interlayer |
| CN103866351A (en) * | 2012-12-14 | 2014-06-18 | 重庆华浩冶炼有限公司 | Electrolytic preparation method of nickel powder |
Non-Patent Citations (1)
| Title |
|---|
| 余勇等: ""不同工艺对真空气雾化Ni粉粒度的影响研究"", 《粉末冶全工业》 * |
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Application publication date: 20200519 |