CN113523295B - Preparation method of copper-coated tungsten spherical composite powder for additive manufacturing - Google Patents
Preparation method of copper-coated tungsten spherical composite powder for additive manufacturing Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- B22F9/00—Making metallic powder or suspensions thereof
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- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/10—Copper
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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
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/20—Refractory metals
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Abstract
The invention provides a preparation method of copper-clad tungsten spherical composite powder for additive manufacturing, which comprises the following steps: (1) Dissolving soluble copper nitrate powder in absolute ethyl alcohol or deionized water, and fully dissolving the soluble copper nitrate powder by mechanical stirring and ultrasonic treatment; then adding the spherical tungsten powder, and completely wetting the spherical tungsten powder by mechanical stirring and ultrasonic treatment again; (2) Putting the solid-liquid mixture into a drying box, and completely drying to obtain composite powder; (3) Placing the composite powder in a tubular furnace, and calcining at high temperature in a reducing atmosphere; cooling to room temperature to obtain copper-coated tungsten spherical composite powder; (4) Taking out the spherical copper-coated tungsten composite powder from the tube furnace, and grinding the powder until no blocky particles exist. The invention can lead copper with different proportions to be completely and uniformly coated on the surface of the metal particles, and keeps the sphericity of the metal powder in the preparation method process, thereby ensuring the fluidity of the composite metal powder and laying a good foundation for the subsequent metal additive manufacturing.
Description
Technical Field
The invention belongs to the technical field of powder preparation engineering, and particularly relates to a preparation method of copper-coated tungsten spherical composite powder for additive manufacturing.
Background
Metal Additive Manufacturing (AM), commonly referred to as metal 3D printing, is a technique of manufacturing components of the same structure as in a model by connecting metal materials in a layer-by-layer manner under the action of high energy sources such as laser or electron beams according to a digital file in a 3D model, thereby facilitating the freedom of custom production and design. Metal additive manufacturing technologies have revolutionary potential and can design and construct metal parts in the digital industry era.
W — Cu alloys are widely used for electrical contacts, welding electrodes, and heat dissipating devices (such as heat sinks and heat sinks) due to their excellent mechanical properties, low thermal expansion, and high electrical conductivity. In most of these applications, a W-Cu composite material with a high density and a uniform microstructure is required to achieve high performance. W-Cu alloys are generally produced by means of liquid copper infiltration into a tungsten skeleton or liquid phase sintering of W-Cu powder compacts. The infiltration is a two-step process: first wicking molten copper into the open pores of a pre-sintered tungsten skeleton; the infiltrated part is then machined to final dimensions. This method does not produce a uniform microstructure and requires a large amount of energy and a high cost. The main factors influencing the performance of the liquid phase sintered part include parameters such as the particle size of the original composite powder, the liquid phase sintering temperature and the like, and both the copper infiltration method and the liquid phase sintering method have great limitation and challenge on manufacturing compact W-Cu parts with complex shapes. Compared with the traditional manufacturing technology, the additive manufacturing has the advantages of high design freedom degree and low post-processing complexity (near-net-shape forming), so that the complex-structure formed part can be prepared. Therefore, the material increase manufacturing method can be adopted to prepare compact W-Cu parts with complex shapes, and the limitation brought by the traditional preparation method can be broken. At present, no commercial original powder which can be directly used for additive manufacturing of W-Cu parts exists, and the traditional means such as ball milling or direct powder mixing have the problems of uneven mixing, reduction of the sphericity of the composite powder, reduction of the fluidity of the composite powder and the like.
At present, the preparation of spherical tungsten-clad powder for additive manufacturing based on a chemical method has certain limitations, for example, a pomegranate-type tungsten alloy powder, a preparation method thereof and an application thereof are disclosed in a chinese patent publication of application publication No. CN 109454229A. Although the spherical powder is prepared by chemical plating, spray granulation and fluidized bed roasting reduction, the method proposed by the patent has the problems of complicated process, excessive chemical reactions and required reaction substances, formation of irritant gases such as SO2 during the reaction, pollution and the like. In addition, the composite powder prepared by the patent has uneven components and difficult control of particle size due to agglomeration, and is not beneficial to subsequent additive manufacturing.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides the preparation method of the copper-clad tungsten spherical composite powder for additive manufacturing, which can completely and uniformly coat copper with different proportions on the surface of metal particles, and keeps the sphericity of the metal powder in the preparation method process, thereby ensuring the fluidity of the composite metal powder and laying a good foundation for the subsequent metal additive manufacturing.
The technical scheme adopted by the invention is as follows: a preparation method of copper-clad tungsten spherical composite powder for additive manufacturing comprises the following steps:
(1) Dissolving soluble copper nitrate powder in absolute ethyl alcohol or deionized water, and fully dissolving the soluble copper nitrate powder by mechanical stirring and ultrasonic treatment; then adding spherical tungsten powder, and wetting the spherical tungsten powder completely by mechanical stirring and ultrasonic treatment again to form a solid-liquid mixture;
(2) Putting the solid-liquid mixture into a drying box, and completely drying to obtain composite powder;
(3) Placing the composite powder in a tube furnace, heating to 700-900 ℃, and calcining for 1-10h in reducing atmosphere; cooling to room temperature to obtain copper-coated tungsten spherical composite powder;
(4) Taking the copper-coated tungsten spherical composite powder out of the tube furnace, and grinding the powder until no blocky particles exist to obtain the uniformly dispersed copper-coated tungsten spherical composite powder.
Further, the soluble copper nitrate powder in the step (1) is one or more of copper nitrate, copper nitrate trihydrate, copper nitrate hexahydrate and copper nitrate nonahydrate. The main mechanism of the preparation method is that soluble nitrate is dissolved and precipitated on the surface of the spherical tungsten through evaporation, and is reduced into a final product through subsequent reduction.
Further, the amount of the soluble copper nitrate-based powder added in the step (1) is such that 0.5-90 wt.% of Cu is present in the finally prepared copper-clad tungsten spherical composite powder.
Further, the rotation speed of the mechanical stirring in the step (1) is 100-500rpm, and the power of the ultrasonic treatment is 100-400W.
Further, the reducing atmosphere in the step (3) is hydrogen.
Further, the grinding mode in the step (4) can be selected from manual grinding or other powder dispersing means.
Further, the particle size of the copper-clad tungsten spherical composite powder in the step (4) is micron-sized, and the particle size range is 15-100 μm; simultaneously, the shape is spherical and nearly spherical; simultaneously, the structure is that copper is coated on the surface of tungsten particles; simultaneously, the final powder is suitable for use in additive manufacturing techniques.
Compared with the prior art, the invention has the beneficial effects that:
1. on the basis of ensuring the purity and the uniform doping, the invention can ensure that the copper-clad tungsten spherical composite powder keeps good sphericity and fluidity, and is beneficial to the subsequent additive manufacturing.
2. The method has simple process, does not need to add auxiliary agents, realizes accurate regulation and control on the content and distribution of the added copper powder, and provides excellent original composite powder for the subsequent metal additive manufacturing of W-Cu alloys with different Cu contents.
3. The dispersion mode of mechanical stirring and ultrasonic treatment adopted by the invention can fully disperse copper to the maximum extent and uniformly adhere the copper to the surface of the spherical tungsten particles so as to keep the sphericity of the tungsten particles; on the other hand, the method can reduce the impurity pollution to the powder so as to ensure the purity of the powder.
4. The invention adopts proper temperature to match with pure reducing atmosphere (pure hydrogen), on one hand, the invention can effectively ensure that the copper oxide and the tungsten oxide are completely reduced into copper and tungsten, thereby forming high-purity copper-coated tungsten spherical composite powder; on the other hand, too high reduction temperature and too long reduction time can cause copper crystal grains to grow, so that the sphericity of the composite powder is reduced, and too low reduction temperature cannot effectively and fully reduce copper oxide and tungsten oxide.
5. The method can be realized in the preparation of small-batch or single-batch spherical tungsten composite powder coated with a large amount of copper with different copper contents.
Drawings
FIG. 1: SEM image (a) of W-0.5wt.% Cu composite powder prepared in example 1 and spectral profile (b) of Cu element;
FIG. 2 is a schematic diagram: SEM image (a) and energy spectrum profile (b) of Cu element of W-10wt.% Cu composite powder prepared in example 2;
FIG. 3: SEM image (a) and energy spectrum profile (b) of Cu element of W-10wt.% Cu composite powder prepared in example 3;
FIG. 4 is a schematic view of: SEM image (a) and energy spectrum profile (b) of Cu element of W-20wt.% Cu composite powder prepared in example 4;
FIG. 5 is a schematic view of: SEM image (a) of W-50wt.% Cu composite powder prepared in example 5 and spectral profile (b) of Cu element;
FIG. 6: SEM image (a) and energy spectrum profile (b) of Cu element of W-90wt.% Cu composite powder prepared in example 6.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Example 1
Dissolving 0.0297g of copper nitrate in 20mL of deionized water, mechanically stirring at the rotating speed of 400rpm and carrying out ultrasonic treatment at the power of 200W to fully dissolve the copper nitrate powder, adding 2g of spherical tungsten powder particles into the prepared copper nitrate solution, and mechanically stirring at the rotating speed of 100rpm and carrying out ultrasonic treatment at the power of 100W again to completely wet the tungsten powder particles. And (3) putting the solid-liquid mixture into a vacuum drying oven with the set temperature of 90 ℃ for drying for 18h, and removing redundant liquid to obtain composite powder. Calcining the composite powder in hydrogen flow at 700 ℃ for 5h (the heating rate is 5 ℃/min, and the air flow is 100 mL/min), and then cooling to room temperature in hydrogen atmosphere to obtain composite oxide powder. After the powder is manually ground for 10min, a composite powder of copper-coated spherical tungsten powder particles (W-0.5 wt.% Cu) can be obtained, wherein an SEM image is shown in fig. 1 (a), and an energy spectrum profile of a Cu element is shown in fig. 1 (b).
Example 2
Dissolving 1.689g of copper nitrate trihydrate in 10mL of absolute ethyl alcohol, mechanically stirring at the rotating speed of 400rpm and carrying out ultrasonic treatment at the power of 200W to fully dissolve the copper nitrate trihydrate powder, adding 4g of spherical tungsten powder into the prepared copper nitrate solution, and mechanically stirring at the rotating speed of 100rpm and carrying out ultrasonic treatment at the power of 100W again to completely wet the spherical tungsten powder particles. And (3) putting the solid-liquid mixture into a vacuum drying oven with the set temperature of 70 ℃ for drying for 24 hours, and removing redundant liquid to obtain composite powder. Calcining the composite powder in 900 ℃ hydrogen gas flow for 1h (the heating rate is 5 ℃/min, the gas flow is 100 mL/min), and then cooling to room temperature in hydrogen atmosphere to obtain composite oxide powder. The powder is ball milled at a rotation speed of 250rad/min for 4h to obtain a copper-coated spherical tungsten powder particle (W-10 wt.% Cu) composite powder, wherein an SEM (scanning electron microscope) diagram is shown in a figure 2 (a), and a power spectrum profile of a Cu element is shown in a figure 2 (b).
Example 3
Dissolving 1.034g of copper nitrate hexahydrate in 10mL of deionized water, fully dissolving the copper nitrate hexahydrate by using mechanical stirring at the rotating speed of 400rpm and ultrasonic treatment at the power of 200W, adding 2g of spherical tungsten powder particles into the prepared copper nitrate solution, and completely wetting the tungsten powder particles by using mechanical stirring at the rotating speed of 100rpm and ultrasonic treatment at the power of 100W again. And (3) putting the solid-liquid mixture into a vacuum drying oven with the set temperature of 70 ℃ for drying for 24 hours, and removing redundant liquid to obtain composite powder. Calcining the composite powder in hydrogen gas flow at 800 ℃ for 5h (the heating rate is 5 ℃/min, and the gas flow is 100 mL/min), and then cooling to room temperature in hydrogen atmosphere to obtain the composite powder. The powder was hand ground for 15min to disperse the bond. A copper-coated spherical tungsten powder particle (W-10 wt.% Cu) composite powder was obtained, and the SEM image is shown in fig. 3 (a), and the energy spectrum profile of the Cu element is shown in fig. 3 (b). As can be seen from the energy spectrum of fig. 3, the composite powder of copper-coated spherical tungsten powder particles (W-10 wt.% Cu) can maintain the spherical structure.
Example 4
2.750g of copper nitrate nonahydrate is dissolved in 10mL of absolute ethyl alcohol, and after the copper nitrate nonahydrate powder is fully dissolved by mechanical stirring at the rotating speed of 400rpm and ultrasonic treatment at the power of 200W, 2g of spherical tungsten powder is added into the prepared copper nitrate solution, and the spherical tungsten powder particles are completely wetted by mechanical stirring at the rotating speed of 100rpm and ultrasonic treatment at the power of 100W. And (3) putting the solid-liquid mixture into a vacuum drying oven with the set temperature of 70 ℃ for drying for 24 hours, and removing redundant liquid to obtain composite powder. The composite powder was calcined in a hydrogen gas stream at 750 ℃ for 2.5h (temperature rise rate 5 ℃/min, gas flow rate 100 mL/min), and then cooled to room temperature in a hydrogen atmosphere to obtain a composite powder. The powder was hand milled for 30min to obtain a composite powder (W-20 wt.% Cu) with a fully spherical structure, the SEM is shown in fig. 4 (a), and the energy spectrum profile of the Cu element is shown in fig. 4 (b).
Example 5
After 17.708g of copper nitrate was dissolved in 10mL of deionized water, and copper nitrate powder was sufficiently dissolved by mechanical stirring at 400rpm and ultrasonic treatment at 200W, 6g of spherical tungsten powder particles were added to the prepared copper nitrate solution, and spherical tungsten powder particles were completely wetted by mechanical stirring at 100rpm and ultrasonic treatment at 100W. And (3) putting the solid-liquid mixture into a vacuum drying oven with the set temperature of 70 ℃ for drying for 24 hours, and removing redundant liquid to obtain composite powder. Calcining the composite powder in 850 ℃ hydrogen airflow for 5h (the heating rate is 5 ℃/min, and the airflow is 100 mL/min), and then cooling to room temperature in hydrogen atmosphere to obtain the composite powder. The powder is ball-milled at a rotation speed of 200rad/min for 5h to remove the large bonded bodies to obtain a composite powder of copper-coated spherical tungsten powder particles (W-50 wt.% Cu), wherein an SEM picture is shown in figure 5 (a), and a power spectrum profile of a Cu element is shown in figure 5 (b).
Example 6
79.687g of copper nitrate hexahydrate is dissolved in 10mL of deionized water, the mixture is mechanically stirred at the rotating speed of 500rpm and ultrasonically treated at the power of 400W, after the copper nitrate hexahydrate is fully dissolved, 3g of spherical tungsten powder is added into the prepared copper nitrate solution, and the mechanical stirring at the rotating speed of 100rpm and the ultrasonic treatment at the power of 100W are used again, so that the spherical tungsten metal powder particles are completely wetted. And (3) putting the solid-liquid mixture into a vacuum drying oven with the set temperature of 60 ℃ for drying for 24 hours, and removing redundant liquid to obtain composite powder. The composite powder is calcined in hydrogen gas flow at 800 ℃ for 2.5h (the heating rate is 5 ℃/min, the gas flow is 100 mL/min), and then cooled to room temperature in hydrogen atmosphere to obtain composite oxide powder. After the powder is manually ground for 20min, the copper-coated spherical tungsten powder particle (W-90 wt.% Cu) composite powder can still maintain the spherical structure, the SEM image is shown in fig. 6 (a), and the energy spectrum surface scan of the Cu element is shown in fig. 6 (b).
The present invention has been described in detail with reference to the embodiments, but the description is only illustrative of the present invention and should not be construed as limiting the scope of the invention. The scope of protection of the invention is defined by the claims. The technical solutions of the present invention or those skilled in the art, based on the teaching of the technical solutions of the present invention, should be considered to be within the scope of the present invention, and all equivalent changes and modifications made within the scope of the present invention or equivalent technical solutions designed to achieve the above technical effects are also within the scope of the present invention.
Claims (2)
1. A preparation method of copper-clad tungsten spherical composite powder for additive manufacturing is characterized by comprising the following steps: the method comprises the following steps:
(1) Dissolving soluble copper nitrate powder in absolute ethyl alcohol or deionized water, and fully dissolving the soluble copper nitrate powder by mechanical stirring and ultrasonic treatment; then adding spherical tungsten powder, and wetting the spherical tungsten powder completely by mechanical stirring and ultrasonic treatment again to form a solid-liquid mixture; the soluble copper nitrate powder is one or more of copper nitrate, copper nitrate trihydrate, copper nitrate hexahydrate and copper nitrate nonahydrate; the rotation speed of mechanical stirring is 100-500rpm, and the power of ultrasonic treatment is 100-400W;
(2) Putting the solid-liquid mixture in a drying box, and completely drying to obtain composite powder;
(3) Placing the composite powder in a tube furnace, heating to 700-900 ℃, and calcining for 1-10h in reducing atmosphere; cooling to room temperature to obtain copper-coated tungsten spherical composite powder; the reducing atmosphere is hydrogen;
(4) Taking the copper-clad tungsten spherical composite powder out of the tubular furnace, and grinding the powder until no blocky particles exist to obtain uniformly dispersed copper-clad tungsten spherical composite powder; the particle size of the final powder is micron grade, the shape of the final powder is spherical, and the structure of the final powder is that copper is on the surface of tungsten particles; the final powder is suitable for use in additive manufacturing techniques.
2. The method for preparing the copper-clad tungsten spherical composite powder for additive manufacturing according to claim 1, wherein the method comprises the following steps: the amount of the soluble copper nitrate powder added in the step (1) is such that 0.5-90 wt.% of Cu is present in the finally prepared copper-clad tungsten spherical composite powder.
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| CN111041318A (en) * | 2019-12-28 | 2020-04-21 | 泰州市华诚钨钼制品有限公司 | Tungsten-copper alloy and preparation method thereof |
| CN113102747A (en) * | 2020-01-13 | 2021-07-13 | 天津大学 | Preparation method for doping rare earth oxide in metal powder for additive manufacturing |
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08311509A (en) * | 1995-05-08 | 1996-11-26 | Osram Sylvania Inc | Production of flowing tungsten/copper composite powder |
| WO2000035616A1 (en) * | 1998-12-16 | 2000-06-22 | Celsia S.P.A. | Process for the production of tungsten-copper composite sinterable powders |
| CN101078068A (en) * | 2007-07-05 | 2007-11-28 | 北京科技大学 | Method for preparing ultra-fine crystal grain tungsten-copper alloy and tungsten-copper alloy |
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