CN112091228B - Preparation method of large-particle spherical tungsten powder - Google Patents
Preparation method of large-particle spherical tungsten powder Download PDFInfo
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- CN112091228B CN112091228B CN202011011267.2A CN202011011267A CN112091228B CN 112091228 B CN112091228 B CN 112091228B CN 202011011267 A CN202011011267 A CN 202011011267A CN 112091228 B CN112091228 B CN 112091228B
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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
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
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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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- 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
A preparation method of large-particle spherical tungsten powder belongs to the technical field of spherical tungsten powder preparation, and sequentially comprises the following steps: (1) mixing the conventional tungsten powder uniformly; (2) carrying out isostatic pressing on the uniformly mixed conventional tungsten powder to obtain a tungsten billet; (3) pre-sintering the pressed billet to increase the bonding strength between the powder; (4) crushing the pre-sintered billet to obtain tungsten powder blocks, screening according to the requirement of large-particle spherical tungsten powder products, and selecting the tungsten powder blocks with proper particle size range; (5) and spheroidizing the tungsten powder block plasma in the proper granularity range to obtain the large-particle spherical tungsten powder. The invention effectively solves the technical problem of upper, middle and lower layering in the pulping process of the traditional preparation method, and avoids introducing impurity C element; according to the invention, tungsten particles with different particle sizes can be selected for plasma spheroidization, so that spherical tungsten powder with different specifications can be prepared; the invention can fully utilize the tungsten powder blocks with the granularity beyond the proper range, and has high utilization rate of raw materials.
Description
Technical Field
The invention belongs to the technical field of preparation of spherical tungsten powder, relates to a material additive manufacturing technology of refractory metals, and particularly relates to a preparation method of large-particle spherical tungsten powder for 3D printing.
Background
The 3D printing technology breaks through the limitation of machining processes such as traditional cutting, greatly improves the utilization rate and preparation efficiency of materials, and subverts the traditional manufacturing industry. Since the first commercial 3D printing device in the united states of 80 s in the 20 th century, 3D printing technology has been rapidly developed in the last 30 years. With the development of 3D printing technology, materials have become important factors that restrict its development. Tungsten, molybdenum and other refractory metal materials have the advantages of high melting point, high hardness, high strength and the like, so that the tungsten, molybdenum and other refractory metal materials have urgent application requirements in the fields of aerospace, weapons, automobiles and medical treatment. Developed countries such as the America and the Germany have taken the breakthrough of the key technology of 3D printing tungsten-molybdenum parts.
For printing a tungsten alloy product by adopting a 3D printing technology, the most important index is powder fluidity, and the tungsten powder is required to have higher sphericity so as to be beneficial to powder feeding and powder laying in the printing process. Common tungsten and molybdenum refractory metal powder in the market has the particle size of less than or equal to 4 mu m, and spherical tungsten powder particles prepared by a freeze spray drying method, a spray granulation method and the like are all less than 100 mu m. For powders with larger particles (. gtoreq.100 μm) with higher flowability the above-mentioned preparation method cannot be achieved because the above-mentioned method is either granulated with conventional tungsten powders (2-4 μm) or with agglomeration granules (45-90 μm). The conventional tungsten powder granulation is limited by the original powder granularity and can only prepare small-particle-size spherical tungsten powder; the method adopts agglomeration granulation, wherein the agglomeration is carried out by adding polyvinyl alcohol (PVA), then the atomizer disk rotates at high speed, the size of the thrown liquid drop is limited, and only spherical tungsten powder with the particle size of most particles below 100 mu m can be prepared. In addition, the spherical tungsten powder prepared by the traditional spray drying, sintering and plasma spheroidizing process routes has poor effect, more hollow spheres, low sphericity, low spheroidization rate and the like, and the main reason is that in the pulping process, the tungsten powder and polyvinyl alcohol (PVA) are mixed and then have the tungsten powder density of 19.3g/cm due to the larger tungsten powder density 3 Tungsten powder is easy to deposit at the bottom of a slurry barrel, so that the density of the tungsten powder at the upper part, the middle part and the bottom is not uniform, granulation is not uniform in the spray drying process, and the compactness of the manufactured tungsten particles is not high. Because of the non-uniformity of tungsten particles in the granulation process, the spheroidization effect is poor after the subsequent plasma spheroidization, and the phenomena of low sphericity, low spheroidization rate, hollow interior and the like occur. Meanwhile, the element C is introduced after polyvinyl alcohol (PVA) is added, and the element C at the center of the tungsten ball can not be completely removed in the subsequent sintering and plasma spheroidizing processes when the tungsten ball formed after spray drying is larger; the introduction of carbon element causes high content of impurity elements and poor density of the printed finished product, and influences the service performance of the final product. Therefore, the current situation of the preparation technology of the high-purity large-particle spherical tungsten powder restricts the development and progress of the 3D printing technology in China, and people urgently need to prepare the large-particle spherical tungsten powder without introducing impuritiesA method of using a C-rich element.
Disclosure of Invention
The invention aims to provide a preparation method of large-particle (more than or equal to 100 mu m) spherical tungsten powder, the tungsten sphere prepared by the method has good sphericity, no impurity element C is introduced, and the granulation effect is much higher than that of the spherical tungsten powder prepared by the prior art. The purpose of the invention is realized by the following technical scheme.
The preparation method of the large-particle spherical tungsten powder is characterized by sequentially comprising the following steps of:
(1) uniformly mixing the conventional tungsten powder;
(2) carrying out isostatic pressing on the uniformly mixed conventional tungsten powder to obtain a tungsten billet;
(3) pre-sintering the pressed billet to increase the bonding strength between the powder;
(4) crushing the pre-sintered billet to obtain tungsten powder blocks, screening according to the requirement of large-particle spherical tungsten powder products, and selecting the tungsten powder blocks with proper particle size range;
(5) and spheroidizing the tungsten powder block plasma in a proper granularity range to obtain large-particle spherical tungsten powder.
According to the preparation method of the large-particle spherical tungsten powder, the technical route of adding polyvinyl alcohol (PVA) for pulping and then performing spray drying is abandoned, the technical problem that the traditional preparation method is layered in the upper, middle and lower parts in the pulping process is effectively solved, and the addition of C element (the C element is higher after the spheroidization of the polyvinyl alcohol pulping) is avoided; meanwhile, by adopting the method, tungsten particles with different particle sizes can be selected for plasma spheroidization by adjusting the screen mesh of the grading screen, so that spherical tungsten powder with different specifications can be prepared.
Furthermore, the large-particle spherical tungsten powder refers to spherical tungsten powder with the particle size of more than or equal to 100 mu m.
Further, the conventional tungsten powder in the step (1) refers to tungsten powder with a particle size of 2-4 μm.
Further, in the step (1), a V-shaped mixer is adopted to uniformly mix the conventional tungsten powder.
Further, the pressure of the isostatic pressing in the step (2) is 200-240MPa, and the dwell time is 60-120 s.
Further, the temperature of the pre-sintering in the step (3) is 1300-.
Further, in the step (4), the tungsten powder blocks larger than the upper limit of the particle size range are crushed again and then sieved again, and the tungsten powder smaller than the lower limit of the particle size range is reduced by hydrogen and then returns to the step (1).
Further, the plasma spheroidizing in the step (5) uses direct current plasma or radio frequency plasma.
Further, the plasma spheroidizing in the step (5) uses radio frequency plasma, and the process parameters are as follows: hydrogen is used as working gas, argon is used as side gas and carrier gas, the flow of the working gas is 4-8slpm, the flow of the side gas is 40-60slpm, the flow of the carrier gas is 2-6slpm, the powder feeding speed is 5-15g/min, and the output power of the equipment is 80-120 KW.
The preparation method of the large-particle spherical tungsten powder provided by the invention has the following technical effects: the particle size is large, the sphericity is good, no impurity element C is introduced, the particle size range of the product can be adjusted, and the utilization rate of raw materials is high.
Detailed Description
The invention is further illustrated by the following examples.
Example 1
A preparation method of large-particle spherical tungsten powder sequentially comprises the following steps:
(1) mixing tungsten powder with conventional particle size of 2-4 μm with V-type mixer to obtain uniform powder.
(2) And pressing the mixed tungsten powder by using isostatic pressing, wherein the pressing pressure is 220MPa, and the pressure maintaining time is 90 s.
(3) And (3) feeding the pressed blank bar into a presintering furnace for presintering at 1400 ℃ for 30 min.
(4) And crushing the pre-sintered billet into large-particle tungsten powder blocks with the particle size of 120-150 mu m by using a crusher. And continuously crushing the tungsten particles with the particle size of more than 150 mu m by using the crusher, and then continuously sieving by using the grading sieve to obtain the tungsten particles meeting the standard. Reducing the fine tungsten particles with the particle size less than 120 mu m by using hydrogen, continuously pressing and sintering the tungsten particles to form pure tungsten bars, and then crushing the pure tungsten bars.
(5) Spheroidizing the tungsten powder block with the particle size of 120-. The plasma spheroidization adopts radio frequency plasma, and the technological parameters are as follows: the method is characterized in that hydrogen is used as working gas, argon is used as side gas and carrier gas, the flow rate of the working gas is 6slpm, the flow rate of the side gas is 50slpm, the flow rate of the carrier gas is 4slpm, the powder feeding speed is 10g/min, and the output power of equipment is 100 kW.
Example 2
A preparation method of large-particle spherical tungsten powder sequentially comprises the following steps:
(1) mixing tungsten powder with conventional particle size of 2-4 μm with V-type mixer to obtain uniform powder.
(2) And pressing the mixed tungsten powder by using isostatic pressing, wherein the pressing pressure is 200MPa, and the pressure maintaining time is 120 s.
(3) And (3) feeding the pressed blank bar into a presintering furnace for presintering, wherein the sintering temperature is 1300 ℃, and the heat preservation time is 45 min.
(4) And crushing the pre-sintered billet into large-particle tungsten powder blocks with the particle size of 120-150 mu m by using a crusher. And continuously crushing the tungsten particles with the particle size of more than 150 mu m by using a crusher, and then continuously sieving by using a grading sieve to sieve out the tungsten particles meeting the standard. Reducing the tungsten particles with the particle size less than 120 mu m by using hydrogen, continuously pressing and sintering the tungsten particles into pure tungsten bars, and crushing the tungsten bars.
(5) Spheroidizing the tungsten powder block with the particle size of 120-. The plasma spheroidization adopts radio frequency plasma, and the technological parameters are as follows: the method is characterized in that hydrogen is used as working gas, argon is used as side gas and carrier gas, the flow rate of the working gas is 4slpm, the flow rate of the side gas is 40slpm, the flow rate of the carrier gas is 2slpm, the powder feeding speed is 5g/min, and the output power of equipment is 80 kW.
Example 3
A preparation method of large-particle spherical tungsten powder sequentially comprises the following steps:
(1) mixing tungsten powder with conventional particle size of 2-4 μm with V-type mixer to obtain uniform powder.
(2) And pressing the mixed tungsten powder by isostatic pressing, wherein the pressing pressure is 240MPa, and the pressure maintaining time is 60 s.
(3) And (3) feeding the pressed blank bar into a presintering furnace for presintering, wherein the sintering temperature is 1500 ℃, and the heat preservation time is 15 min.
(4) And crushing the pre-sintered billet into large-particle tungsten powder blocks with the particle size of 120-150 mu m by using a crusher. And continuously crushing the tungsten particles with the particle size of more than 150 mu m by using a crusher, and then continuously sieving by using a grading sieve to sieve out the tungsten particles meeting the standard. Reducing the tungsten particles with the particle size less than 120 mu m by using hydrogen, continuously pressing and sintering the tungsten particles into pure tungsten bars, and crushing the tungsten bars.
(5) Spheroidizing the tungsten powder block with the particle size of 120-. The plasma spheroidization adopts radio frequency plasma, and the technological parameters are as follows: the method is characterized in that hydrogen is used as working gas, argon is used as side gas and carrier gas, the flow rate of the working gas is 8slpm, the flow rate of the side gas is 60slpm, the flow rate of the carrier gas is 6slpm, the powder feeding rate is 15g/min, and the output power of equipment is 120 kW.
Claims (3)
1. The preparation method of the large-particle spherical tungsten powder is characterized by sequentially comprising the following steps of:
(1) uniformly mixing conventional tungsten powder, wherein the conventional tungsten powder refers to tungsten powder with the particle size of 2-4 mu m;
(2) carrying out isostatic pressing on the uniformly mixed conventional tungsten powder to obtain a tungsten billet; the pressure of isostatic pressing is 200-240MPa, and the pressure maintaining time is 60-120 s;
(3) pre-sintering the pressed billet to increase the bonding strength between the powder; the pre-sintering temperature is 1300-1500 ℃, and the heat preservation time is 15-45 min;
(4) crushing the pre-sintered billet to obtain tungsten powder blocks, screening according to the requirement of large-particle spherical tungsten powder products, and selecting the tungsten powder blocks with proper particle size range;
(5) spheroidizing the tungsten powder block plasma in a proper granularity range to obtain large-particle spherical tungsten powder; the plasma spheroidizing uses the radio frequency plasma as the plasma, and the technological parameters are as follows: hydrogen is used as working gas, argon is used as side gas and carrier gas, the flow of the working gas is 4-8slpm, the flow of the side gas is 40-60slpm, the flow of the carrier gas is 2-6slpm, the powder feeding speed is 5-15g/min, and the output power of the equipment is 80-120 KW;
the large-particle spherical tungsten powder refers to spherical tungsten powder with the particle size of more than or equal to 100 mu m.
2. The preparation method according to claim 1, wherein the conventional tungsten powder is uniformly mixed in the step (1) by using a V-shaped mixer.
3. The preparation method according to claim 1, wherein in the step (4), the tungsten powder blocks larger than the upper limit of the particle size range are crushed again and then sieved again, and the tungsten powder smaller than the lower limit of the particle size range is reduced by hydrogen and then returned to the step (1).
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| CN101224500A (en) * | 2007-12-17 | 2008-07-23 | 金堆城钼业股份有限公司 | Super particle size molybdenum powder preparing method |
| CN102259186A (en) * | 2011-07-28 | 2011-11-30 | 北京科技大学 | Method for producing thin spherical tungsten powder |
| CN107470639B (en) * | 2017-09-18 | 2019-10-18 | 北京科技大学 | A kind of preparation method of narrow size distribution globular tungsten powder |
| RU2678355C1 (en) * | 2017-11-07 | 2019-01-28 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Нижегородский государственный университет им. Н.И. Лобачевского" | METHOD FOR PRODUCING SPRAYABLE COMPOSITE TARGET CONTAINING Co2MnSi HEUSLER ALLOY PHASE |
| CN109266939B (en) * | 2018-12-05 | 2020-07-24 | 株洲江钨博大硬面材料有限公司 | Preparation method of high-density WC-WB-Co spherical powder hard-face material |
| CN109692965A (en) * | 2019-02-27 | 2019-04-30 | 北京工业大学 | A kind of preparation method of the spherical tungsten-molybdenum alloy powder of 3D printing |
| CN110860686A (en) * | 2019-10-25 | 2020-03-06 | 西安宝德九土新材料有限公司 | Small-particle-size cobalt-chromium-tungsten-molybdenum alloy spherical powder and preparation method thereof |
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