CN114289722B - A kind of preparation method of fine-grained spherical tungsten powder - Google Patents
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims description 7
- 239000000843 powder Substances 0.000 claims abstract description 82
- 238000011282 treatment Methods 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000002245 particle Substances 0.000 claims abstract description 22
- 239000006185 dispersion Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000005516 engineering process Methods 0.000 claims abstract description 12
- 239000007789 gas Substances 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 15
- 230000001681 protective effect Effects 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 11
- 238000001354 calcination Methods 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000005243 fluidization Methods 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 5
- 238000009826 distribution Methods 0.000 abstract description 8
- 229910052721 tungsten Inorganic materials 0.000 abstract description 7
- 239000010937 tungsten Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 4
- 238000004663 powder metallurgy Methods 0.000 abstract description 3
- 230000001788 irregular Effects 0.000 abstract description 2
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000010146 3D printing Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000003870 refractory metal Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000026030 halogenation Effects 0.000 description 1
- -1 halogenation method Chemical compound 0.000 description 1
- 238000005658 halogenation reaction Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
一种细粒度球形钨粉的制备方法，属于粉末冶金技术领域。针对目前由于原料细粒度钨粉形貌不规则，且易团聚而导致球化过程球化后颗粒长大、粉末粒度分布宽、收得率低的问题，本发明首先采用流化床处理改善钨粉的粉末状态，提高粉末的分散性并改变其表面形貌。然后将处理后的粉末送入送粉装置，施加压力形成等离子炬，对粉末进行球化处理。最后得到了表面光滑，球化率高的球形钨粉。本发明采用对流化分散技术与等离子球化技术相结合来制备细粒度球形钨粉，球化后钨粉活性低，没有污染，球形度好，球化充分且收得率高。
The invention discloses a method for preparing fine-grained spherical tungsten powder, which belongs to the technical field of powder metallurgy. Aiming at the current problem that the raw material fine-grained tungsten powder has irregular shape and is easy to agglomerate, resulting in particle growth after spheroidization, wide powder particle size distribution, and low yield, the present invention first adopts fluidized bed treatment to improve tungsten The powder state of the powder, improve the dispersibility of the powder and change its surface morphology. Then the processed powder is sent to the powder feeding device, and the pressure is applied to form a plasma torch, and the powder is spheroidized. Finally, spherical tungsten powder with smooth surface and high spheroidization rate was obtained. The present invention adopts the combination of convective dispersion technology and plasma spheroidization technology to prepare fine-grained spherical tungsten powder. After spheroidization, the tungsten powder has low activity, no pollution, good sphericity, sufficient spheroidization and high yield.
Description
技术领域technical field
本发明属于粉末冶金技术领域，具体涉及了一种细粒度球形钨粉的制备方法。The invention belongs to the technical field of powder metallurgy, and in particular relates to a preparation method of fine-grained spherical tungsten powder.
背景技术Background technique
钨及其合金具有熔点高、高温强度高、耐热耐腐蚀性好等优良性能，广泛应用于航空航天、核电及医疗等领域。传统粉末冶金的方法难以制备结构复杂的钨及其合金制品。随着材料成形技术的不断发展，3D打印和粉末注射成形技术成为制备小型钨及其合金制品的有效方法。作为3D打印和粉末注射成形制备复杂结构钨制品件的原材料，球形钨粉的制备是新型钨及其合金制品开发的重要环节。制备球形钨粉的方法层出不穷，如卤化法、旋转电极法、部分优先氧化碱洗、仲钨酸铵循环氧化还原法、喷雾干燥法等，这些方法各有各的弊端，未能实现工业化。因此发展一种工艺简单,成本低的球形钨粉制备工艺十分必要。Tungsten and its alloys have excellent properties such as high melting point, high temperature strength, and good heat and corrosion resistance, and are widely used in aerospace, nuclear power, and medical fields. Traditional powder metallurgy methods are difficult to prepare tungsten and its alloy products with complex structures. With the continuous development of material forming technology, 3D printing and powder injection molding technology have become effective methods for preparing small tungsten and its alloy products. As a raw material for 3D printing and powder injection molding to prepare tungsten products with complex structures, the preparation of spherical tungsten powder is an important link in the development of new tungsten and its alloy products. There are endless methods for preparing spherical tungsten powder, such as halogenation method, rotating electrode method, partial preferential oxidation alkali washing, ammonium paratungstate cyclic redox method, spray drying method, etc. These methods have their own disadvantages and have not been industrialized. Therefore, it is necessary to develop a simple and low-cost spherical tungsten powder preparation process.
等离子球化有能量密度高，加热强度大，且不存在污染等优点，在对钨等难熔金属粉末处理有着良好的效果，能得到球形度好，球化率高，纯度高的球形粉末。由于市售细粒度钨粉团聚严重，而经射频等离子球化处理后收得的粉末的粒度及粒度分布主要由喂料粉末的粒度及粒度分布决定，在这种情况下通过提高功率的来提高粉末的球化率，必然导致在这个过程中细粒度球形钨粉气化消失，粉末的中位径增大，表现为等离子球化处理得到的粉末粒度分布宽，粉末易聚集长大。而流化分散处理可实现对粉末的解团聚、破碎细化、表面整形，提高粉末的松装、振实密度等，且具有能耗低、磨损小等优点。中国专利(CN104070173B)公开了一种球形钨粉的制备方法，将粒度为5-27μm原料钨粉末送入气流磨中研磨后通过氩等离子体炬球化后得到球形钨粉，其球化后的粉末粒度较大、分布不均匀且仍有团聚体的存在球化率过低。中国专利(CN104174862B)公开了一种供一种低成本、易于大规模生产，参数控制容易的球形钨粉的制备方法，但其制备的粉末粒度大小不均匀，球形度较差且易受到污染，很难得到细的球形钨粉。因此，本发明采用对流化分散技术与等离子球化技术相结合来制备细粒度球形钨粉，球化后钨粉活性低，没有污染，球形度好，球化充分且收得率高。Plasma spheroidization has the advantages of high energy density, high heating intensity, and no pollution. It has a good effect on the treatment of refractory metal powders such as tungsten, and can obtain spherical powders with good sphericity, high spheroidization rate, and high purity. Due to serious agglomeration of fine-grained tungsten powder in the market, the particle size and particle size distribution of the powder obtained after radio frequency plasma spheroidization are mainly determined by the particle size and particle size distribution of the feed powder. The spheroidization rate of the powder will inevitably lead to the gasification and disappearance of the fine-grained spherical tungsten powder in this process, and the median diameter of the powder will increase. The fluidized dispersion treatment can realize the deagglomeration, crushing and refinement of the powder, surface shaping, and improve the loose packing and tap density of the powder, and has the advantages of low energy consumption and small wear. Chinese patent (CN104070173B) discloses a preparation method of spherical tungsten powder. The raw material tungsten powder with a particle size of 5-27 μm is sent into a jet mill for grinding and then spheroidized by an argon plasma torch to obtain spherical tungsten powder. The spheroidized tungsten powder The particle size of the powder is large, the distribution is uneven and there are still aggregates, and the spheroidization rate is too low. Chinese patent (CN104174862B) discloses a method for preparing spherical tungsten powder with low cost, easy large-scale production, and easy parameter control, but the prepared powder has uneven particle size, poor sphericity and is easily polluted. It is difficult to obtain fine spherical tungsten powder. Therefore, the present invention adopts the combination of convective dispersion technology and plasma spheroidization technology to prepare fine-grained spherical tungsten powder. After spheroidization, the tungsten powder has low activity, no pollution, good sphericity, sufficient spheroidization and high yield.
发明内容Contents of the invention
本发明的目的在于针对目前由于细粒度钨粉不规则且易团聚，而导致球化过程球化后颗粒长大、粉末粒度分布宽、收得率低的问题，采取流化分散技术与等离子球化技术相结合来制备球形钨粉。The purpose of the present invention is to solve the current problem that the fine-grained tungsten powder is irregular and easy to agglomerate, resulting in particle growth after spheroidization, wide powder particle size distribution, and low yield, and adopts fluidized dispersion technology and plasma ball Combination of chemical technology to prepare spherical tungsten powder.
一种球形钨粉的制备方法，其特征在于采取对喷式气流磨分散技术与等离子球化技术相结合来制备球形钨粉；A method for preparing spherical tungsten powder, which is characterized in that spherical tungsten powder is prepared by combining counter-jet jet mill dispersion technology and plasma spheroidization technology;
具体步骤如下：Specific steps are as follows:
1)原料粉末为纯度大于99.9％，粒度小于3μm的钨粉；1) The raw material powder is tungsten powder with a purity greater than 99.9% and a particle size less than 3 μm;
2)将原料粉末加入到流化床中，分散处理前应先自下而上地向设备中充入高纯惰性气体除去空气，为粉末提供气体保护环境，并对设备进行充气清洗；待流化床腔体内的空气排完之后，将其转移到加热装置中，在流化床处理过程中连续通入稳定流量的高纯氢气气体，在恒流恒温下流化处理一定时间；2) Put the raw material powder into the fluidized bed, and before dispersing, fill the equipment with high-purity inert gas from bottom to top to remove the air, provide a gas protection environment for the powder, and inflate and clean the equipment; After the air in the fluidized bed cavity is exhausted, it is transferred to the heating device, and a stable flow of high-purity hydrogen gas is continuously introduced during the fluidized bed treatment process, and the fluidized treatment is performed at a constant flow and constant temperature for a certain period of time;
3)流化床分散处理之后，将流化床腔体从加热装置移出，并持续通入高纯惰性保护气体，待冷却至室温后，停止通保护气体，得到处理后的粉末；3) After the dispersion treatment of the fluidized bed, remove the fluidized bed cavity from the heating device, and continuously feed high-purity inert protective gas, and after cooling to room temperature, stop the protective gas to obtain the processed powder;
4)在纯度大于99.9％的高纯氢气为保护气氛下，将步骤3)处理后的粉末在200℃～450℃的温度范围内进行一次或者多次的煅烧处理；4) Under the protective atmosphere of high-purity hydrogen with a purity greater than 99.9%, the powder treated in step 3) is subjected to one or more calcination treatments in the temperature range of 200°C to 450°C;
5)将处理后的粉末送入送粉装置，以氩气为工作气体，施加压力形成等离子炬，对粉末进行球化处理；5) Send the processed powder into the powder feeding device, use argon as the working gas, apply pressure to form a plasma torch, and spheroidize the powder;
6)将经过等离子球化后的粉末冷却后进行收集，得到处理后的粉末。6) Collecting the powder after plasma spheroidization after cooling to obtain the processed powder.
进一步地，步骤2)所述氢气气流的流速为1.5～5L/min，加热温度为150～280℃，在恒流恒温下流化处理100～360min。Further, the flow rate of the hydrogen gas stream in step 2) is 1.5-5 L/min, the heating temperature is 150-280° C., and the fluidization treatment is performed at a constant flow and temperature for 100-360 min.
进一步地，步骤4)中的煅烧处理工艺为：升温速率为1～2℃/min，保温时间为60～300min，降温速率为2～5℃/min。Further, the calcination process in step 4) is as follows: the heating rate is 1-2° C./min, the holding time is 60-300 minutes, and the cooling rate is 2-5° C./min.
进一步地，步骤5)中所述球化处理，其中送粉速率为10～18g/min，处理功率为10～35kw，送粉气流量为8～15L/min，中气流量为35～50L/min，边气流量为30～75L/min。Further, the spheroidization treatment described in step 5), wherein the powder feeding rate is 10-18g/min, the processing power is 10-35kw, the powder feeding air flow is 8-15L/min, and the medium air flow is 35-50L/min min, the edge air flow rate is 30-75L/min.
本发明的优点是：The advantages of the present invention are:
(1)在高纯惰性和氢气气氛下进行流化处理，由于气流的作用，粉末之间以及粉末与流化床腔体内壁发生碰撞和摩擦，使颗粒之间的团聚打开并改变其表面形貌，无污染；(1) Fluidization treatment is carried out under a high-purity inert and hydrogen atmosphere. Due to the action of the air flow, the powders collide and rub against the inner wall of the fluidized bed cavity, so that the agglomeration between the particles is opened and the surface shape is changed. Appearance, no pollution;
(2)经流化分散处理后，钨粉团聚打开，流动性变好，松装振实密度提高；(2) After fluidization and dispersion treatment, the tungsten powder is agglomerated and opened, the fluidity becomes better, and the loose packing density increases;
(3)对流化处理后的粉末进行煅烧后，可以消除流化过程中产生的内应力，减小粉末活性，在后续等离子球化过程中可避免颗粒长大；(3) After calcining the fluidized powder, the internal stress generated during the fluidization process can be eliminated, the activity of the powder can be reduced, and particle growth can be avoided in the subsequent plasma spheroidization process;
(4)等离子球化过程的能量密度高，加热强度大，得到粉末纯度高，球化率高，球形度好，适合难熔金属粉末的处理；(4) The energy density of the plasma spheroidization process is high, the heating intensity is large, the obtained powder has high purity, high spheroidization rate, and good sphericity, which is suitable for the treatment of refractory metal powder;
(5)经流化分散处理后的钨粉经射频等离子球化，由于钨粉的流动性更好，可有效避免了团聚体颗粒的聚集长大，球化后钨粉球形度好，球化充分，收得率高。(5) The tungsten powder after fluidization and dispersion treatment is spheroidized by radio frequency plasma. Due to the better fluidity of tungsten powder, it can effectively avoid the aggregation and growth of aggregate particles. Full, high yield.
附图说明Description of drawings
图1为流化-等离子球化处理前后钨粉的XRD图。Figure 1 is the XRD pattern of tungsten powder before and after fluidization-plasma spheroidization treatment.
具体实施方式Detailed ways
实施例1Example 1
1)原料粉末为市售钨粉，粒度为2μm，纯度大于99.9％；1) The raw material powder is commercially available tungsten powder with a particle size of 2 μm and a purity greater than 99.9%;
2)将原料粉末加入到流化床中，分散处理前应先自下而上地向设备中充入高纯惰性气体除去空气，为粉末提供气体保护环境，并对设备进行充气清洗；待流化床腔体内的空气排完之后，将其转移到加热装置中，在流化床处理过程中连续通入稳定流量的高纯惰性气体，气流的流速为5L/min，加热温度为250℃，在恒流恒温下流化处理180min；2) Put the raw material powder into the fluidized bed, and before dispersing, fill the equipment with high-purity inert gas from bottom to top to remove the air, provide a gas protection environment for the powder, and inflate and clean the equipment; After the air in the fluidized bed cavity is exhausted, it is transferred to the heating device, and a stable flow of high-purity inert gas is continuously introduced during the fluidized bed treatment process. The flow rate of the gas flow is 5L/min, and the heating temperature is 250°C. Fluidized treatment at constant flow and temperature for 180 minutes;
3)流化床分散处理之后，将流化床腔体从加热装置移出，并持续通入高纯惰性保护气体，待冷却至室温后，停止通保护气体，得到处理后的粉末；3) After the dispersion treatment of the fluidized bed, remove the fluidized bed cavity from the heating device, and continuously feed high-purity inert protective gas, and after cooling to room temperature, stop the protective gas to obtain the processed powder;
4)在纯度大于99.9％的高纯氢气为保护气氛下，将流化处理后的粉末以1℃/min升温到400℃，保温60min进行两次煅烧处理，降温速率为3℃/min；4) Under the protective atmosphere of high-purity hydrogen with a purity greater than 99.9%, the fluidized powder was heated up to 400°C at 1°C/min, kept for 60 minutes and calcined twice, with a cooling rate of 3°C/min;
5)将处理后的粉末送入送粉装置，以氩气为工作气体，施加压力形成等离子炬，对粉末进行球化处理，其中送粉速率为15g/min，处理功率为30kw，送粉气流量为15L/min，中气流量为50L/min，边气流量为75L/min；5) Send the processed powder into the powder feeding device, use argon as the working gas, apply pressure to form a plasma torch, and perform spheroidization treatment on the powder, wherein the powder feeding rate is 15g/min, the processing power is 30kw, and the powder feeding gas The flow rate is 15L/min, the middle air flow rate is 50L/min, and the side air flow rate is 75L/min;
6)将经过等离子化后的粉末冷却后进行收集，得到粒度分布集中在2μm左右、球化率接近100％、球形度好的球形钨粉。6) Collect the plasmaized powder after cooling to obtain a spherical tungsten powder with a particle size distribution concentrated at about 2 μm, a spheroidization rate close to 100%, and good sphericity.
实施例2Example 2
1)原料粉末为市售钨粉，粒度为1μm，纯度大于99.9％；1) The raw material powder is commercially available tungsten powder with a particle size of 1 μm and a purity greater than 99.9%;
2)将原料粉末加入到流化床中，分散处理前应先自下而上地向设备中充入高纯惰性气体除去空气，为粉末提供气体保护环境，并对设备进行充气清洗；待流化床腔体内的空气排完之后，将其转移到加热装置中，在流化床处理过程中连续通入稳定流量的高纯氢气气体，气流的流速为4L/min，加热温度为200℃，在恒流恒温下流化处理120min；2) Put the raw material powder into the fluidized bed, and before dispersing, fill the equipment with high-purity inert gas from bottom to top to remove the air, provide a gas protection environment for the powder, and inflate and clean the equipment; After the air in the fluidized bed cavity is exhausted, it is transferred to the heating device, and a stable flow of high-purity hydrogen gas is continuously introduced during the fluidized bed treatment process. The flow rate of the air flow is 4L/min, and the heating temperature is 200°C. Fluidized treatment at constant flow and temperature for 120 minutes;
3)流化分散处理之后，将流化床腔体从加热装置移出，并持续通入高纯惰性保护气体，待冷却至室温后，停止通保护气体，得到处理后的粉末。3) After the fluidized dispersion treatment, the fluidized bed chamber is removed from the heating device, and the high-purity inert protective gas is continuously introduced into it, and after cooling to room temperature, the protective gas is stopped to obtain the treated powder.
4)在纯度大于99.9％的高纯氢气为保护气氛下，将流化处理后的粉末以2℃/min升温到300℃，保温90min进行一次煅烧处理，降温速率为4℃/min；4) Under the protective atmosphere of high-purity hydrogen with a purity greater than 99.9%, the fluidized powder was heated up to 300°C at 2°C/min, kept for 90 minutes for a calcination treatment, and the cooling rate was 4°C/min;
5)将处理后的粉末送入送粉装置，以氩气为工作气体，施加压力形成等离子炬，对粉末进行球化处理，其中送粉速率为12g/min，处理功率为25kw，送粉气流量为10L/min，中气流量为45L/min，边气流量为65L/min；5) Send the processed powder into the powder feeding device, use argon as the working gas, apply pressure to form a plasma torch, and carry out spheroidization treatment on the powder, wherein the powder feeding rate is 12g/min, the processing power is 25kw, and the powder feeding gas The flow rate is 10L/min, the middle air flow rate is 45L/min, and the edge air flow rate is 65L/min;
6)将经过等离子球化后的粉末冷却后进行收集，得到粒度分布集中在1μm左右、球化率接近100％、球形度好的球形钨粉。6) Collect the powder after plasma spheroidization after cooling to obtain spherical tungsten powder with a particle size distribution concentrated at about 1 μm, a spheroidization rate close to 100%, and good sphericity.
实施例3Example 3
1)原料粉末为市售钨粉，粒度为0.8μm，纯度大于99.9％；1) The raw material powder is commercially available tungsten powder with a particle size of 0.8 μm and a purity greater than 99.9%;
2)将原料粉末加入到流化床中，分散处理前应先自下而上地向设备中充入高纯惰性气体除去空气，为粉末提供气体保护环境，并对设备进行充气清洗；待流化床腔体内的空气排完之后，将其转移到加热装置中，在流化床处理过程中连续通入稳定流量的高纯氢气气体，气流的流速为3L/min，加热温度为180℃，在恒流恒温下流化处理100min。2) Put the raw material powder into the fluidized bed, and before dispersing, fill the equipment with high-purity inert gas from bottom to top to remove the air, provide a gas protection environment for the powder, and inflate and clean the equipment; After the air in the fluidized bed cavity is exhausted, it is transferred to the heating device, and a stable flow of high-purity hydrogen gas is continuously introduced during the fluidized bed treatment process. The flow rate of the air flow is 3L/min, and the heating temperature is 180°C. Fluidized treatment at constant flow and temperature for 100min.
3)流化分散处理之后，将流化床腔体从加热装置移出，并持续通入高纯惰性保护气体，待冷却至室温后，停止通保护气体，得到处理后的粉末。3) After the fluidized dispersion treatment, the fluidized bed chamber is removed from the heating device, and the high-purity inert protective gas is continuously introduced into it, and after cooling to room temperature, the protective gas is stopped to obtain the treated powder.
4)在纯度大于99.9％的高纯氢气为保护气氛下，将流化处理后的粉末以1℃/min升温到250℃，保温120min进行一次煅烧处理，降温速率为2℃/min；4) Under the protective atmosphere of high-purity hydrogen with a purity greater than 99.9%, heat the fluidized powder to 250°C at a rate of 1°C/min, and heat it for 120 minutes for a calcination treatment, with a cooling rate of 2°C/min;
5)将处理后的粉末送入送粉装置，以氩气为工作气体，施加压力形成等离子炬，对粉末进行球化处理，其中送粉速率为10g/min，处理功率为25kw，送粉气流量为8L/min，中气流量为40L/min，边气流量为60L/min；5) Send the processed powder into the powder feeding device, use argon as the working gas, apply pressure to form a plasma torch, and carry out spheroidization treatment on the powder, wherein the powder feeding rate is 10g/min, the processing power is 25kw, and the powder feeding gas The flow rate is 8L/min, the middle air flow rate is 40L/min, and the edge air flow rate is 60L/min;
6)球化处理后：将经过等离子球化后的粉末冷却后进行收集，得到粒度分布集中在0.8μm左右、球化率接近100％、球形度好的球形钨粉。6) After spheroidization treatment: collect the powder after plasma spheroidization after cooling, and obtain spherical tungsten powder with a particle size distribution concentrated at about 0.8 μm, a spheroidization rate close to 100%, and good sphericity.
以上所述，仅是本发明的较佳实施例而已，并非对本发明作任何形式上的限制，虽然本发明已以较佳实施例揭露如上，然而并非用以限定本发明，任何熟悉本专业的技术人员，在不脱离本发明技术方案范围内，当可利用上述揭示的方法及技术内容作出些许的更动或修饰为等同变化的等效实施例，但凡是未脱离本发明技术方案的内容，依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰，均仍属于本发明技术方案的范围内。The above description is only a preferred embodiment of the present invention, and does not limit the present invention in any form. Although the present invention has been disclosed as above with preferred embodiments, it is not intended to limit the present invention. Anyone familiar with this field Those skilled in the art, without departing from the scope of the technical solution of the present invention, may use the method and technical content disclosed above to make some changes or modifications to equivalent embodiments with equivalent changes, but if they do not depart from the technical solution of the present invention, Any simple modifications, equivalent changes and modifications made to the above embodiments according to the technical essence of the present invention still fall within the scope of the technical solutions of the present invention.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62282635A (en) * | 1986-05-31 | 1987-12-08 | Natl Res Inst For Metals | Production of mixture of ultra-fine aluminum nitride powder and ultra-fine oxidation-resistant aluminum powder |
| CN104070173A (en) * | 2014-06-23 | 2014-10-01 | 陕西斯瑞工业有限责任公司 | Preparation method of spherical tungsten powder |
| KR20150031750A (en) * | 2013-09-16 | 2015-03-25 | 한국생산기술연구원 | Method for manufacturing powder of ruthenium-chromium with rf plasma process |
| CN107470639A (en) * | 2017-09-18 | 2017-12-15 | 北京科技大学 | A kind of preparation method of narrow size distribution globular tungsten powder |
| CN109382511A (en) * | 2018-11-23 | 2019-02-26 | 北京科技大学 | A kind of fluidisation shaping preparation method of 3D printing Low cost technique of titanium powders |
| CN112453413A (en) * | 2020-11-20 | 2021-03-09 | 中科院过程工程研究所南京绿色制造产业创新研究院 | Preparation method of oxide dispersion strengthened steel spherical powder for 3D printing |
-
2021
- 2021-12-08 CN CN202111494192.2A patent/CN114289722B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62282635A (en) * | 1986-05-31 | 1987-12-08 | Natl Res Inst For Metals | Production of mixture of ultra-fine aluminum nitride powder and ultra-fine oxidation-resistant aluminum powder |
| KR20150031750A (en) * | 2013-09-16 | 2015-03-25 | 한국생산기술연구원 | Method for manufacturing powder of ruthenium-chromium with rf plasma process |
| CN104070173A (en) * | 2014-06-23 | 2014-10-01 | 陕西斯瑞工业有限责任公司 | Preparation method of spherical tungsten powder |
| CN107470639A (en) * | 2017-09-18 | 2017-12-15 | 北京科技大学 | A kind of preparation method of narrow size distribution globular tungsten powder |
| CN109382511A (en) * | 2018-11-23 | 2019-02-26 | 北京科技大学 | A kind of fluidisation shaping preparation method of 3D printing Low cost technique of titanium powders |
| CN112453413A (en) * | 2020-11-20 | 2021-03-09 | 中科院过程工程研究所南京绿色制造产业创新研究院 | Preparation method of oxide dispersion strengthened steel spherical powder for 3D printing |
Non-Patent Citations (1)
| Title |
|---|
| 射频感应等离子体制备球形钨粉的工艺研究;古忠涛;叶高英;刘川东;童洪辉;;强激光与粒子束(第07期);第1079-1082页 * |
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