CN111663067A - Hard alloy material for 3D printing and preparation process thereof - Google Patents
Hard alloy material for 3D printing and preparation process thereof Download PDFInfo
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- CN111663067A CN111663067A CN202010501394.4A CN202010501394A CN111663067A CN 111663067 A CN111663067 A CN 111663067A CN 202010501394 A CN202010501394 A CN 202010501394A CN 111663067 A CN111663067 A CN 111663067A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/08—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on tungsten carbide
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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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
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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
Abstract
The invention discloses a hard alloy material for 3D printing and a preparation process thereof, wherein the raw materials for preparing the hard alloy material for 3D printing comprise the following components in parts by weight: 89.5 to 92.4 percent of WC, 4.2 to 5.8 percent of Co, 0.10 to 0.60 percent of Ni, 0.2 to 1.0 percent of TiC, 0.4 to 1.2 percent of TiN, 0.5 to 1.6 percent of Mo, 0.15 to 1.2 percent of Cr and 0.12 to 1.1 percent of TaC; the particle size of Co is 1.0-1.5 microns. The hard alloy material for 3D printing has the advantages of high uniformity of the printed product, stable quality, excellent comprehensive mechanical property, simple preparation process, easy operation of the preparation process, higher economic benefit and suitability for large-scale popularization and application.
Description
Technical Field
The invention relates to the technical field of alloy materials, in particular to a hard alloy material for 3D printing and a preparation process thereof.
Background
The hard alloy is an alloy material prepared from refractory metal carbide (hard phase) and metal binder (binder phase) by a powder metallurgy method. With the rapid development of science and technology, especially in the high-precision technical fields of aerospace, defense military industry and the like, the preparation of hard alloy by applying the traditional powder metallurgy method has the defects of low efficiency, excessive productivity, difficult complex parts, high cost and the like, and the requirements on hard alloy products with complex shapes, fine structures and excellent comprehensive properties are difficult to meet. The 3D printing technology can solve the problem, greatly reduces the consumption of materials and preparation processing procedures, and reduces the processing cost and the processing period of products. However, the common hard alloy material or the metal ceramic is not uniform enough in the structure and the composition of a printed product, and the density of pores is not tight enough, so that the quality and the application of a product are influenced.
Chinese patent CN106367652A discloses a hard alloy particle and a preparation method thereof, and a hard alloy and a preparation method thereof, the hard alloy particle includes: WC-V-Cr-Y-La-Ni3Al-SiC particles; a WC-V-Cr-Y-La-Ni3Al transition layer coated outside the WC-V-Cr-Y-La-Ni3Al-SiC particles. However, the structure and composition uniformity of the cemented carbide in the patent are not good, and the cemented carbide is not suitable for 3D printing.
Chinese patent CN108356260A discloses a 3D printing manufacturing method of a hard alloy special-shaped product, which adopts in-situ synthesized WC-Co-C composite powder as an initial material, and regulates the rheological property and the curing behavior of the prepared slurry by adding an organic forming agent with specific molecular weight, so that spherical particles with ultrahigh sphericity and compactness are obtained after spray drying; and coating a tungsten layer on the surface of the spherical particles by a chemical vapor deposition technology. However, the cemented carbide tungsten layer prepared by the patent has poor cohesiveness and influences the strength of cemented carbide.
Disclosure of Invention
Aiming at the problems, the invention provides a hard alloy material for 3D printing and a preparation process thereof.
The technical scheme adopted by the invention for solving the problems is as follows: the hard alloy material for 3D printing comprises the following raw materials in parts by weight: 89.5 to 92.4 percent of WC, 4.2 to 5.8 percent of Co, 0.10 to 0.60 percent of Ni, 0.2 to 1.0 percent of TiC, 0.4 to 1.2 percent of TiN, 0.5 to 1.6 percent of Mo, 0.15 to 1.2 percent of Cr and 0.12 to 1.1 percent of TaC; the particle size of the Co is 1.0-1.5 microns.
The metal Co is used as a binding phase and can be distributed in gaps, crystal boundaries and phase boundaries formed by WC particles to play a role in binding the WC particles, the amount of pores of the material can be reduced by adding a proper amount of Co, the mechanical property of the material is improved, but the Co can generate an agglomeration phenomenon when the content of the Co is higher, and on the contrary, more pores can be generated to influence the hardness of the alloy, so that the content of the Co is controlled to be 4.2-5.8%; the addition of TiC can ensure that the grain structure of the alloy is more reasonably distributed, the alloy structure is more densified, and the hardness of the alloy material is improved, but the addition of TiC with higher content can influence the fracture toughness of the material, so the content of TiC is controlled to be 0.2-1.0%; the appropriate amount of TiN can improve the bending strength of the material; TaC can inhibit the growth of coarse grains.
Further, the technical indexes of WC are as follows: the granularity of WC is 0.3-0.6 micron, the specific surface area is 2.4m2/g~2.7m2The total content of C in WC is 6.18-6.30%, and the content of Cr3C2 is 0.52-0.66%.
Furthermore, the granularity of TiN is 20 nm-50 nm.
Furthermore, the grain size of TiC is 1.5-3.5 microns, and the content of Ti in the TiC is 78-82%.
Furthermore, the granularity of the TaC is between 1.5 and 2.5 microns, and the total carbon content in the TaC is between 6.0 and 6.4 percent.
Further, the raw materials for preparing the hard alloy material for 3D printing comprise the following components in parts by weight: 90.8 to 91.6 percent of WC, 4.6 to 5.6 percent of Co, 0.30 to 0.50 percent of Ni, 0.4 to 0.6 percent of TiC, 0.6 to 1.0 percent of TiN, 0.7 to 1.2 percent of Mo, 0.3 to 0.9 percent of Cr and 0.12 to 0.9 percent of TaC.
Further, the raw materials for preparing the hard alloy material for 3D printing comprise the following components in parts by weight: 90.8% of WC, 4.6% of Co, 0.20% of Ni, 0.8% of TiC, 0.6% of TiN, 1.2% of Mo, 0.9% of Cr and 0.9% of TaC.
Another object of the present invention is to provide a process for preparing a cemented carbide material for 3D printing, comprising the steps of:
step S10, weighing the raw materials for preparing the hard alloy material for 3D printing according to the parts by weight;
step S20, mixing the WC, Co, Ni, TiC, TiN, Mo, Cr and TaC in parts by weight, adding alcohol, uniformly stirring, placing into a ball mill, and ball-milling for 4-10 hours to obtain a mixed material; wherein, the WC easily has a granular structure, the raw materials with different grain sizes can be subjected to grain size homogenization by wet milling and crushing, which is beneficial to producing high-quality alloy, and the short-time high-speed ball milling can reduce the occurrence of oxygenation and activation in the wet milling process and avoid the phenomenon of coarse inclusion; the ratio of the addition amount of the alcohol to the raw materials is 0.25L/kg-0.38L/kg;
and S30, performing spray drying on the mixed material obtained in the step S20, and screening spherical particles with the particle size of 10-30 microns to obtain the hard alloy material for 3D printing. Wherein the spray drying can separate the raw material powder from the alcohol medium in the slurry to obtain particles of a target particle size, and can also safely recover alcohol.
Further, in step S20, the inner diameter of the ball mill was 680mm, and the rotational speed of the cylinder was 35 rpm. When the ball milling speed is too high, raw material particles fall to a higher position to generate impact milling, and the raw material particles are not suitable for the hard alloy raw material with smaller particle size, so the rotating speed is controlled at 35 revolutions per minute.
The invention has the advantages that:
(1) aiming at the action of each metal element in the hard alloy and the specific requirements of 3D printing, the hardness and the mechanical property of the hard alloy material are improved by adjusting and optimizing the raw material composition, the generation of pores in the alloy is reduced by controlling the content of Co in the hard alloy, the mechanical property of the hard alloy is improved, and the compactness of the hard alloy and the hardness of the hard alloy can be improved by controlling the content of TiC;
(2) according to the invention, through wet grinding of the hard alloy raw material, the uniformity of the particle size of the raw material can be improved, so that the uniformity of the product structure and composition is improved, and the quality of the product is improved;
(3) the hard alloy material for 3D printing has the advantages of high uniformity of the printed product, stable quality, excellent comprehensive mechanical property, simple preparation process, easy operation of the preparation process, higher economic benefit and suitability for large-scale popularization and application.
In addition to the objects, features and advantages described above, other objects, features and advantages of the present invention are also provided. The present invention is described in further detail below.
Detailed Description
The following detailed description of embodiments of the invention, but the invention can be practiced in many different ways, as defined and covered by the claims.
The formulations of examples 1-5 and comparative examples of a cemented carbide material for 3D printing according to the present invention are shown in table 1:
TABLE 1
Example 1
Hard alloy material for 3D printing and preparation process thereof
The hard alloy material for 3D printing is prepared by the following processes:
step S10, weighing the raw materials for preparing the hard alloy material for 3D printing according to the parts by weight, wherein the particle size of Co is 1.0-1.5 microns; the granularity of WC is 0.3-0.6 micron, the specific surface area is 2.4m2/g~2.7m2The total content of C in WC is 6.18-6.20%, and the content of Cr3C2 is 0.52-0.66%; the granularity of TiN is 20-50 nm; the grain size of TiC is 1.5-3.5 microns, and the content of Ti in the TiC is 78-80%; the granularity of TaC is between 1.5 and 2.5 microns, and the total carbon content in TaC is between 6.0 and 6.4 percent;
step S20, mixing the WC, the Co, the Ni, the TiC, the TiN, the Mo, the Cr and the TaC in parts by weight, adding alcohol, uniformly stirring, placing into a ball mill, wherein the inner diameter of the ball mill is 680mm, the rotating speed of a cylinder is 35 r/min, and ball-milling for 8 hours to obtain a mixed material;
and S30, performing spray drying on the mixed material obtained in the step S20, and screening spherical particles with the particle size of 10-30 microns to obtain the hard alloy material for 3D printing.
Example 2
Hard alloy material for 3D printing and preparation process thereof
The hard alloy material for 3D printing is prepared by the following processes:
step S10, weighing the raw materials for preparing the hard alloy material for 3D printing according to the parts by weight, wherein the particle size of Co is 1.0-1.5 microns; the granularity of WC is 0.3-0.6 micron, the specific surface area is 2.4m2/g~2.7m2The total content of C in WC is 6.18-6.30%, and the content of Cr3C2 is 0.52-0.66%; the granularity of TiN is 20-50 nm; the grain size of TiC is 1.5-3.5 microns, and the content of Ti in the TiC is 78-82%; the granularity of TaC is between 1.5 and 2.5 microns, and the total carbon content in TaC is between 6.0 and 6.4 percent;
step S20, mixing the WC, the Co, the Ni, the TiC, the TiN, the Mo, the Cr and the TaC in parts by weight, adding alcohol, uniformly stirring, placing into a ball mill, wherein the inner diameter of the ball mill is 680mm, the rotating speed of a cylinder is 35 r/min, and ball-milling for 4 hours to obtain a mixed material;
and S30, performing spray drying on the mixed material obtained in the step S20, and screening spherical particles with the particle size of 10-30 microns to obtain the hard alloy material for 3D printing.
Example 3
Hard alloy material for 3D printing and preparation process thereof
The hard alloy material for 3D printing is prepared by the following processes:
step S10, weighing the raw materials for preparing the hard alloy material for 3D printing according to the parts by weight, wherein the particle size of Co is 1.0-1.5 microns; the granularity of WC is 0.3-0.6 micron, the specific surface area is 2.4m2/g~2.7m2The total content of C in WC is 6.18-6.30%, and the content of Cr3C2 is 0.52-0.66%; the granularity of TiN is 30-50 nm; the grain size of TiC is 1.5-3.5 microns, and the content of Ti in the TiC is 78-82%; the granularity of TaC is between 1.5 and 2.5 microns, and the total carbon content in TaC is between 6.0 and 6.4 percent;
step S20, mixing the WC, the Co, the Ni, the TiC, the TiN, the Mo, the Cr and the TaC in parts by weight, adding alcohol, uniformly stirring, placing into a ball mill, wherein the inner diameter of the ball mill is 680mm, the rotating speed of a cylinder is 35 r/min, and ball-milling for 10 hours to obtain a mixed material;
and S30, performing spray drying on the mixed material obtained in the step S20, and screening spherical particles with the particle size of 10-30 microns to obtain the hard alloy material for 3D printing.
Example 4
Hard alloy material for 3D printing and preparation process thereof
The hard alloy material for 3D printing is prepared by the following processes:
step S10, weighing the raw materials for preparing the hard alloy material for 3D printing according to the parts by weight, wherein the particle size of Co is 1.0-1.5 microns; the granularity of WC is 0.3-0.6 micron, the specific surface area is 2.4m2/g~2.7m2The total content of C in WC is 6.18-6.30%, and the content of Cr3C2 is 0.52-0.62%; the granularity of TiN is 20-30 nanometers; the grain size of TiC is 1.5-3.5 microns, and the content of Ti in the TiC is 78-82%; the granularity of TaC is between 1.5 and 2.5 microns, and the total carbon content in TaC is between 6.0 and 6.4 percent;
step S20, mixing the WC, the Co, the Ni, the TiC, the TiN, the Mo, the Cr and the TaC in parts by weight, adding alcohol, uniformly stirring, placing into a ball mill, wherein the inner diameter of the ball mill is 680mm, the rotating speed of a cylinder is 20 r/min, and ball-milling for 6 hours to obtain a mixed material;
and S30, performing spray drying on the mixed material obtained in the step S20, and screening spherical particles with the particle size of 10-30 microns to obtain the hard alloy material for 3D printing.
Example 5
Hard alloy material for 3D printing and preparation process thereof
The hard alloy material for 3D printing is prepared by the following processes:
step S10, weighing the raw materials for preparing the hard alloy material for 3D printing according to the parts by weight, wherein the particle size of Co is 1.0-1.5 microns; the granularity of WC is 0.3-0.6 micron, the specific surface area is2.4m2/g~2.7m2The total content of C in WC is 6.18-6.30%, and the content of Cr3C2 is 0.52-0.62%; the granularity of TiN is 20-30 nanometers; the grain size of TiC is 1.5-3.5 microns, and the content of Ti in the TiC is 78-82%; the granularity of TaC is between 1.5 and 2.5 microns, and the total carbon content in TaC is between 6.0 and 6.4 percent;
step S20, mixing the WC, the Co, the Ni, the TiC, the TiN, the Mo, the Cr and the TaC in parts by weight, adding alcohol, uniformly stirring, placing into a ball mill, wherein the inner diameter of the ball mill is 680mm, the rotating speed of a cylinder is 100 revolutions per minute, and ball-milling for 5 hours to obtain a mixed material;
and S30, performing spray drying on the mixed material obtained in the step S20, and screening spherical particles with the particle size of 10-30 microns to obtain the hard alloy material for 3D printing.
Comparative example 1
Hard alloy material for 3D printing and preparation process thereof
The hard alloy material for 3D printing is prepared by the following processes:
step S10, weighing the raw materials for preparing the hard alloy material for 3D printing according to the parts by weight, wherein the particle size of Co is 1.0-1.5 microns; the granularity of WC is 0.3-0.6 micron, the specific surface area is 2.4m2/g~2.7m2The total content of C in WC is 6.18-6.30%, and the content of Cr3C2 is 0.52-0.66%;
step S20, mixing the WC and the Co in parts by weight, adding alcohol, uniformly stirring, placing into a ball mill, wherein the inner diameter of the ball mill is 680mm, the rotating speed of a cylinder body is 35 r/min, and ball milling is carried out for 8 hours to obtain a mixed material;
and S30, performing spray drying on the mixed material obtained in the step S20, and screening spherical particles with the particle size of 10-30 microns to obtain the hard alloy material for 3D printing.
Examples of the experiments
To further illustrate the technological advancement of the present invention, experiments are now taken to further illustrate it.
The experimental method comprises the following steps: the hard alloy material for 3D printing prepared by the invention is used for preparing hard alloy by 3D laser printing under the same conditions, and the wear resistance, fracture toughness and hardness of the alloy are tested, and the results are shown in Table 1.
TABLE 1 Performance test results of cemented carbide materials prepared according to the present invention for 3D printing
Experimental results show that the hard alloy synthesized by the hard alloy material for 3D printing prepared by the invention has higher hardness, good compactness and excellent bending strength performance, and the addition of a proper amount of Ni, TiC, TiN, Mo, Cr and TaC elements is beneficial to improving the strength and density of the hard alloy material and improving the quality of products.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The hard alloy material for 3D printing is characterized in that the raw materials for preparing the hard alloy material for 3D printing comprise the following components in parts by weight: 89.5 to 92.4 percent of WC, 4.2 to 5.8 percent of Co, 0.10 to 0.60 percent of Ni, 0.2 to 1.0 percent of TiC, 0.4 to 1.2 percent of TiN, 0.5 to 1.6 percent of Mo, 0.15 to 1.2 percent of Cr and 0.12 to 1.1 percent of TaC; the particle size of the Co is 1.0-1.5 microns.
2. The cemented carbide material for 3D printing according to claim 1, characterized in that the WC specifications are: the granularity of WC is 0.3-0.6 micron, the specific surface area is 2.4m2/g~2.7m2The total content of C in WC is 6.18-6.30%, and the content of Cr3C2 is 0.52-0.66%.
3. The cemented carbide material for 3-D printing according to claim 1, characterised in that the particle size of the TiN is between 20 nm and 50 nm.
4. The cemented carbide material for 3D printing according to claim 1, characterised in that the grain size of TiC is between 1.5 and 3.5 microns, the Ti content in TiC is between 78 and 82%.
5. The cemented carbide material for 3D printing according to claim 1, characterised in that the TaC has a particle size between 1.5 and 2.5 microns and a total carbon content in the TaC between 6.0 and 6.4%.
6. The cemented carbide material for 3D printing according to claim 1, wherein the raw materials for preparing the cemented carbide material for 3D printing comprise, in parts by weight: 90.8 to 91.6 percent of WC, 4.6 to 5.6 percent of Co, 0.30 to 0.50 percent of Ni, 0.4 to 0.6 percent of TiC, 0.6 to 1.0 percent of TiN, 0.7 to 1.2 percent of Mo, 0.3 to 0.9 percent of Cr and 0.12 to 0.9 percent of TaC.
7. The cemented carbide material for 3D printing according to claim 1, wherein the raw materials for preparing the cemented carbide material for 3D printing comprise, in parts by weight: 90.8% of WC, 4.6% of Co, 0.20% of Ni, 0.8% of TiC, 0.6% of TiN, 1.2% of Mo, 0.9% of Cr and 0.9% of TaC.
8. A process for preparing a cemented carbide material for 3D printing according to any one of claims 1 to 7, characterized by the steps of:
step S10, weighing the raw materials for preparing the hard alloy material for 3D printing according to the weight parts;
step S20, mixing the WC, Co, Ni, TiC, TiN, Mo, Cr and TaC in parts by weight, adding alcohol, uniformly stirring, placing into a ball mill, and ball-milling for 4-10 hours to obtain a mixed material;
and S30, performing spray drying on the mixed material obtained in the step S20, and screening spherical particles with the particle size of 10-30 microns to obtain the hard alloy material for 3D printing.
9. The production process according to claim 8, wherein in step S20, the ball mill has an inner diameter of 680mm and a barrel rotation speed of 35 rpm.
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CN114000085A (en) * | 2021-09-17 | 2022-02-01 | 崇义章源钨业股份有限公司 | Titanium carbonitride-based thermal spraying powder and preparation method and application thereof |
CN116005058A (en) * | 2022-12-09 | 2023-04-25 | 浙江恒成硬质合金有限公司 | Cemented carbide cutter for titanium alloy cutting and preparation method thereof |
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Application publication date: 20200915 |