CN113523295A - 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
- 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
- B22F9/16—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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- 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
- B22F9/04—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
- 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
- B22F9/04—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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- 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
- B22F2301/10—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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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 wetting the spherical tungsten powder completely by mechanical stirring and ultrasonic treatment again; (2) putting the solid-liquid mixture in 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 industrial 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. The W — Cu alloy is generally produced by a method such as liquid copper infiltration of a tungsten skeleton or liquid phase sintering of a W — Cu powder compact. 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 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. As no commercial original powder which can be directly used for additive manufacturing of W-Cu parts exists at present, and the traditional ball milling or direct powder mixing and other means have the problems of uneven mixing, reduction of the sphericity of the composite powder, reduction of the flowability of the composite powder and the like.
At present, the preparation of spherical powder of tungsten coated with copper 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 this patent prepares spherical powder by electroless plating, spray granulation, fluidized bed roasting reduction, the method proposed in this patent has problems of complicated process, excessive chemical reactions involved and necessary reaction substances, formation of irritating gases such as SO2 during the reaction, contamination, 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 in a drying box, and completely drying to obtain composite powder;
(3) placing the composite powder in a tubular furnace, heating to the temperature of 700-900 ℃, and calcining for 1-10h by using a reducing atmosphere; cooling to room temperature to obtain copper-coated tungsten spherical composite powder;
(4) and taking the copper-clad tungsten spherical composite powder out of the tubular furnace, and grinding the powder until no blocky particles exist to obtain the uniformly dispersed copper-clad 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 wt.% to 90 wt.% of Cu is present in the finally produced copper-clad tungsten spherical composite powder.
Further, the rotation speed of the mechanical stirring in the step (1) is 100-.
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 is adopted, on one hand, copper can be completely dispersed to the maximum extent and can be uniformly attached to the surface of spherical tungsten particles, so that the sphericity of the particles is kept; on the other hand, the impurity pollution of the powder can be reduced, so that the purity of the powder is ensured.
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 small-batch or single-batch preparation of a large amount of spherical tungsten composite powder coated with different copper contents.
Drawings
FIG. 1: SEM image (a) and energy spectrum profile (b) of Cu element of W-0.5 wt.% Cu composite powder prepared in example 1;
FIG. 2: SEM image (a) and energy spectrum profile (b) of Cu element of W-10 wt.% Cu composite powder prepared in example 2;
FIG. 3: SEM image (a) and energy spectrum profile (b) of Cu element of W-10 wt.% Cu composite powder prepared in example 3;
FIG. 4: SEM image (a) and energy spectrum profile (b) of Cu element of W-20 wt.% Cu composite powder prepared in example 4;
FIG. 5: SEM image (a) and energy spectrum profile (b) of Cu element of W-50 wt.% Cu composite powder prepared in example 5;
FIG. 6: SEM image (a) and energy spectrum profile (b) of Cu element of W-90 wt.% 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, and performing mechanical stirring at the rotating speed of 400rpm and 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 performing mechanical stirring at the rotating speed of 100rpm and 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 gas flow at 700 ℃ for 5h (the heating rate is 5 ℃/min, the gas flow is 100mL/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, using mechanical stirring at the rotating speed of 400rpm and 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 using mechanical stirring at the rotating speed of 100rpm and 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 a hydrogen gas flow at 900 ℃ for 1h (the heating rate is 5 ℃/min, the gas flow is 100mL/min), and then cooling to room temperature in a 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, and using mechanical stirring at the rotating speed of 400rpm and ultrasonic treatment at the power of 200W to fully dissolve the copper nitrate hexahydrate, adding 2g of spherical tungsten powder particles into the prepared copper nitrate solution, and using mechanical stirring at the rotating speed of 100rpm and 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 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, the gas flow is 100mL/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 copper-coated spherical tungsten powder particle composite powder (W-10 wt.% Cu) obtained by the above operation can still maintain the spherical structure.
Example 4
2.750g of copper nitrate nonahydrate is dissolved in 10mL of absolute ethyl alcohol, mechanical stirring is carried out at the rotating speed of 400rpm and ultrasonic treatment with the power of 200W is carried out to fully dissolve the copper nitrate nonahydrate powder, 2g of spherical tungsten powder is added into the prepared copper nitrate solution, and mechanical stirring at the rotating speed of 100rpm and ultrasonic treatment with the power of 100W are carried out 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. The composite powder is calcined in hydrogen gas flow at 750 ℃ for 2.5h (the heating rate is 5 ℃/min, the gas flow is 100mL/min), and then cooled to room temperature in hydrogen atmosphere to obtain the composite powder. The powder was manually ground for 30min to obtain a composite powder (W-20 wt.% Cu) with a complete 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
17.708g of copper nitrate is dissolved in 10mL of deionized water, and after copper nitrate powder is fully dissolved by mechanical stirring at the rotating speed of 400rpm and ultrasonic treatment at the power of 200W, 6g of spherical tungsten powder particles are 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. Calcining the composite powder in a hydrogen gas flow at 850 ℃ for 5h (the heating rate is 5 ℃/min, the gas flow is 100mL/min), and then cooling to room temperature in a 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, mechanical stirring is carried out at the rotating speed of 500rpm, ultrasonic treatment with the power of 400W is carried out, after the copper nitrate hexahydrate powder is fully dissolved, 3g of spherical tungsten powder is added into the prepared copper nitrate solution, mechanical stirring is carried out at the rotating speed of 100rpm, ultrasonic treatment with the power of 100W is carried out again, and 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 100mL/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 present invention. The scope 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 (6)
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;
(2) putting the solid-liquid mixture in a drying box, and completely drying to obtain composite powder;
(3) placing the composite powder in a tubular furnace, heating to the temperature of 700-900 ℃, and calcining for 1-10h by using a reducing atmosphere; cooling to room temperature to obtain copper-coated tungsten spherical composite powder;
(4) and taking the copper-clad tungsten spherical composite powder out of the tubular furnace, and grinding the powder until no blocky particles exist to obtain the uniformly dispersed copper-clad tungsten spherical composite powder.
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 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.
3. 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-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.
4. 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 rotation speed of the mechanical stirring in the step (1) is 100-.
5. 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: and (3) the reducing atmosphere is hydrogen.
6. 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 particle size of the final powder obtained in the step (4) is micron grade, the final powder is spherical, and the structure of the final powder is that copper is arranged on the surface of tungsten particles.
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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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- 2021-07-20 CN CN202110810454.5A patent/CN113523295B/en active Active
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| 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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