CN104084594A - Method for preparing microfine spherical niobium powder - Google Patents
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- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 43
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000002245 particle Substances 0.000 claims abstract description 31
- 229910052786 argon Inorganic materials 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims description 22
- 239000010955 niobium Substances 0.000 claims description 15
- 229910052758 niobium Inorganic materials 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 230000006698 induction Effects 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000012798 spherical particle Substances 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims 2
- 238000006243 chemical reaction Methods 0.000 claims 1
- 239000008187 granular material Substances 0.000 claims 1
- 238000010791 quenching Methods 0.000 claims 1
- 230000000171 quenching effect Effects 0.000 claims 1
- 230000001788 irregular Effects 0.000 abstract description 5
- 230000008859 change Effects 0.000 abstract description 2
- 230000000704 physical effect Effects 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 230000008569 process Effects 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 239000012495 reaction gas Substances 0.000 description 4
- 238000010146 3D printing Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000007639 printing Methods 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 238000000149 argon plasma sintering Methods 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 229910001257 Nb alloy Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 125000001475 halogen functional group Chemical group 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002887 superconductor Substances 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
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Abstract
本发明涉及一种制备微细球形铌粉的方法，所述方法包括：首先，形成稳定氩等离子体，调节各项参数以控制等离子体在反应器内的分布；然后送入铌原粉，铌粉经过等离子区域，颗粒受热熔化；离开等离子区后迅速冷却固化，得到微细球形铌粉。和不规则颗粒形状的原粉相比，粉体颗粒大多数呈球形，流动性、颗粒密度、纯度更高，颗粒表面光洁，颗粒孔隙率低；本发明提出的方法改变了铌粉颗粒的形状，球化率高，并且增加了粉末的表观密度，增加了铌粉流动性，提高了铌粉的物理性能，同时不会改变铌粉的物相，有利于一些领域中应用，并且成本低廉。
The invention relates to a method for preparing fine spherical niobium powder. The method comprises: first, forming a stable argon plasma, adjusting various parameters to control the distribution of the plasma in the reactor; After passing through the plasma region, the particles are heated and melted; after leaving the plasma region, they are rapidly cooled and solidified to obtain fine spherical niobium powder. Compared with the original powder with irregular particle shape, most of the powder particles are spherical, the fluidity, particle density and purity are higher, the surface of the particles is smooth, and the particle porosity is low; the method proposed by the present invention changes the shape of the niobium powder particles , high spheroidization rate, and increases the apparent density of the powder, increases the fluidity of the niobium powder, improves the physical properties of the niobium powder, and does not change the phase of the niobium powder, which is beneficial to the application in some fields, and the cost is low .
Description
技术领域technical field
本发明涉及一种制备微细球形铌粉的方法，属于粉末制备领域。The invention relates to a method for preparing fine spherical niobium powder, which belongs to the field of powder preparation.
背景技术Background technique
用等离子体做热源在微米亚微米以及某些纳米材料的球化处理方面，具有较大的技术优势。射频等离子体炬弧体硕大、弧流稳定、易于调节控制，使之易应用于超细粉末材料处理技术领域。目前，国外利用等离子体来处理粉体技术已具备一定的技术水平。加拿大的泰克纳(TEKNA)公司开发的等离子体粉体处理系统在感应等离子体技术方面处于国际领先地位，已实现W、Mo、Re、Ta、Ni、Cu等金属粉末和SiO2、ZrO2、YSZ、Al2O3等氧化物陶瓷粉末的球化处理。国内的核工业西南物理研究院采用自建等离子球化系统，实现了W、Al2O3等粉末的球化，球化率高，尺寸达0.5～45μm，粉体用于热喷涂和粉末冶金，具有很好的性能。Using plasma as a heat source has great technical advantages in the spheroidization of micron, submicron and certain nanomaterials. The radio frequency plasma torch has a large arc body, stable arc flow, and easy adjustment and control, making it easy to apply to the field of ultrafine powder material processing technology. At present, foreign countries use plasma to process powder technology has a certain technical level. The plasma powder treatment system developed by Canada's Tekna (TEKNA) company is in the international leading position in the induction plasma technology, and has realized W, Mo, Re, Ta, Ni, Cu and other metal powders and SiO 2 , ZrO 2 , Spheroidization treatment of oxide ceramic powders such as YSZ and Al 2 O 3 . The Southwest Institute of Physics of the domestic nuclear industry adopts a self-built plasma spheroidization system to realize the spheroidization of W, Al 2 O 3 and other powders, with a high spheroidization rate and a size of 0.5-45 μm. The powder is used for thermal spraying and powder metallurgy , with good performance.
因为球化粉末在一些领域中的优良应用，各种粉末尤其是高难熔粉末的球化成为粉末制备的需求。金属铌是一种高难熔金属，熔点高达2740℃，能吸收气体，用作除气剂，也是一种良好的超导体，应用于许多高技术领域。如在高能物理领域，需要得到高性能、大尺寸的铌制品，若使用激光3D打印工艺来制备铌制品，相比传统工艺，有可能得到性能更优，尺寸更大的产品。然而，在采用激光3D打印致密的高性能铌制品时，采用颗粒形状不规则的粉末，在打印铺料时，流动性不好，造成打印速率慢，并且堆积密度小，容易形成孔洞，不致密；若采用球形粉末为原料铌粉，在打印铺料时，流动性好，堆积密度大，激光烧结后制品收缩均匀，可实现较为精确的尺寸控制，制品密度均匀，气孔率低，更加致密，制备过程耗时大为减少，激光烧结功率也将降低；并且通过射频等离子球化的粉末，杂质含量能进一步降低，尤其是降低微量氧杂质含量，从而进一步优化铌制品的超导电性能。Because of the excellent application of spheroidized powders in some fields, the spheroidization of various powders, especially high refractory powders, has become a demand for powder preparation. Metal niobium is a highly refractory metal with a melting point as high as 2740°C. It can absorb gas and be used as a degasser. It is also a good superconductor and is used in many high-tech fields. For example, in the field of high-energy physics, it is necessary to obtain high-performance and large-sized niobium products. If laser 3D printing technology is used to prepare niobium products, compared with traditional processes, it is possible to obtain products with better performance and larger sizes. However, when laser 3D printing is used to print dense high-performance niobium products, powders with irregular particle shapes are used. When printing and laying materials, the fluidity is not good, resulting in slow printing speed, and the packing density is small, which is easy to form holes and is not dense. ; If spherical powder is used as raw material niobium powder, it has good fluidity and high bulk density when printing and laying materials. After laser sintering, the product shrinks evenly, which can achieve more accurate size control. The product has uniform density, low porosity, and is more dense. The time consumption of the preparation process is greatly reduced, and the laser sintering power will also be reduced; and the impurity content of the powder spheroidized by radio frequency plasma can be further reduced, especially the trace oxygen impurity content, so as to further optimize the superconductivity of niobium products.
在这个背景要求之下，需要有一种确实可行、具有一定生产能力的方法，来进行微细球形铌粉的制备。Under this background requirement, it is necessary to have a method that is feasible and has a certain production capacity to prepare fine spherical niobium powder.
发明内容Contents of the invention
本发明的目的在于提供一种成本低廉、球化率高、具备一定生产能力的制备微细球形铌粉的方法。The purpose of the present invention is to provide a method for preparing fine spherical niobium powder with low cost, high spheroidization rate and certain production capacity.
本发明通过如下技术方案实现：、The present invention realizes through following technical scheme:,
一种制备微细球形铌粉的方法，该方法包括以下步骤：A method for preparing fine spherical niobium powder, the method comprises the following steps:
1)形成稳定的氩等离子体炬；1) forming a stable argon plasma torch;
2)通过携带气体，将金属铌原粉送入到等离子体炬的高温区，铌粉受热，形成颗粒液滴；2) Send the metal niobium raw powder into the high temperature zone of the plasma torch by carrying the gas, and the niobium powder is heated to form particle droplets;
3)铌粉颗粒液滴离开等离子区域后，冷却固化形成球形颗粒粉末；3) After the niobium powder particle droplet leaves the plasma region, it cools and solidifies to form a spherical particle powder;
4)收集球形铌粉末。4) Collect spherical niobium powder.
根据本发明，步骤1)中，在高频等离子反应器中，形成氩等离子体炬所需要的反应气体(优选Ar)输入流量为40～60slpm，感应线圈上加载的高电压为6～8KV。所述的氩等离子体稳定运行时的反应气体(优选Ar)输入流量为20～50slpm，保护气体(Ar)输入流量为30～120slpm，系统内部气压为0.03～0.06MPa。According to the present invention, in step 1), in the high-frequency plasma reactor, the input flow rate of the reaction gas (preferably Ar) required to form the argon plasma torch is 40-60 slpm, and the high voltage applied to the induction coil is 6-8KV. When the argon plasma is in stable operation, the input flow rate of the reaction gas (preferably Ar) is 20-50 slpm, the input flow rate of the protective gas (Ar) is 30-120 slpm, and the internal pressure of the system is 0.03-0.06 MPa.
根据本发明，步骤2)中，所述携带气体可用氩气、氢气等在高温环境中不与金属粉体发生化学反应的气体。所加入的金属铌原粉的平均粒径为0.5～45μm，携带气体控制流量为0.5～5slpm，铌粉喂料控制流量为5～50g/min。According to the present invention, in step 2), the carrier gas may be argon, hydrogen or other gas that does not chemically react with the metal powder in a high temperature environment. The average particle size of the added metal niobium raw powder is 0.5-45 μm, the control flow rate of the carrying gas is 0.5-5 slpm, and the control flow rate of the niobium powder feeding is 5-50 g/min.
根据本发明，步骤3)中，铌粉颗粒液滴离开等离子炬后，在极高的温度梯度(10-6)下迅速冷却、进入热交换室骤冷凝固，在表面张力的作用下形成球形的颗粒。According to the present invention, in step 3), after leaving the plasma torch, the droplets of niobium powder particles are rapidly cooled under a very high temperature gradient (10 -6 ), enter the heat exchange chamber to be quenched and solidified, and form a spherical shape under the action of surface tension particle.
根据本发明，步骤4)中，使用收集器来收集球形铌粉末。According to the present invention, in step 4), a collector is used to collect spherical niobium powder.
本发明的优点是，和不规则颗粒形状的原粉相比，粉体颗粒大多数呈球形，流动性、颗粒密度、纯度更高，颗粒表面光洁，颗粒孔隙率低。本发明提出的方法改变了铌粉颗粒的形状，球化率高，同时提高了铌粉的纯度，并且增加了粉末的表观密度，增加了铌粉流动性，提高了铌粉的物理性能，同时不会改变铌粉的物相，有利于粉末致密成型和烧结、3D打印高性能铌制品、致密涂层等的应用，并且成本低廉，能获得很高的技术附加值。和其它关于铌合金粉末球化的专利相比，本发明采用的纯铌粉熔点很高，铌粉球化的同时提高了纯度，并且具有一定的粉末球化生产力。The invention has the advantages that, compared with the original powder with irregular particle shape, most of the powder particles are spherical, the fluidity, particle density and purity are higher, the surface of the particles is smooth, and the particle porosity is low. The method proposed by the invention changes the shape of the niobium powder particles, has a high spheroidization rate, improves the purity of the niobium powder, increases the apparent density of the powder, increases the fluidity of the niobium powder, and improves the physical properties of the niobium powder. At the same time, it will not change the phase of niobium powder, which is conducive to the application of dense powder forming and sintering, 3D printing of high-performance niobium products, dense coatings, etc., and the cost is low, and high technical added value can be obtained. Compared with other patents on niobium alloy powder spheroidization, the pure niobium powder used in the present invention has a high melting point, and the niobium powder spheroidization improves the purity at the same time, and has a certain powder spheroidization productivity.
附图说明Description of drawings
图1是制备球形铌粉的工艺流程图。Figure 1 is a process flow chart for preparing spherical niobium powder.
图2是实施例1中采用的-200目铌原粉的扫描电镜图。2 is a scanning electron microscope image of the -200 mesh niobium raw powder used in Example 1.
图3是实施例1中采用的-200目铌原粉球化后的扫描电镜图。FIG. 3 is a scanning electron micrograph of the -200 mesh niobium raw powder used in Example 1 after spheroidization.
图4是实施例1中粉末球化前后的XRD衍射谱对比。FIG. 4 is a comparison of XRD diffraction spectra before and after powder spheroidization in Example 1.
图5是实施例2中采用的-300目铌原粉球化后的扫描电镜图。FIG. 5 is a scanning electron micrograph of the -300 mesh niobium raw powder used in Example 2 after spheroidization.
具体实施方式Detailed ways
下面结合附图与实施例对本发明作进一步详细说明。但本领域技术人员了解，本发明并不局限于此。任何在本发明基础上做出的改进和变化，都在本发明的保护范围之内。The present invention will be described in further detail below in conjunction with the accompanying drawings and embodiments. However, those skilled in the art understand that the present invention is not limited thereto. Any improvements and changes made on the basis of the present invention are within the protection scope of the present invention.
一种制备微细球形铌粉的方法，流程如图1所示，它按下述步骤依次进行：A kind of method for preparing fine spherical niobium powder, flow process as shown in Figure 1, it carries out successively by following steps:
1、建立稳定运行的氩等离子体炬：向等离子体反应器输入40～60slpm持续氩气流，感应线圈加载高电压，电压可以是6～8KV，同时点火器放电，高压线圈感应耦合及点火器电晕触发，使氩气电离产生氩等离子体炬。此时使整个等离子体反应器内保持负压状态，即可保证等离子体炬稳定运行。1. Establish a stable argon plasma torch: input 40-60 slpm continuous argon flow into the plasma reactor, load the induction coil with high voltage, the voltage can be 6-8KV, and at the same time the igniter discharges, the high-voltage coil is inductively coupled and the igniter electric The halo is triggered to ionize the argon gas to generate the argon plasma torch. At this time, maintaining a negative pressure in the entire plasma reactor can ensure the stable operation of the plasma torch.
2、利用携带气体将金属铌粉(原粉)注入氩等离子体炬的芯部高温区加热。携带气体可用氩气、氢气等在高温环境中不与金属粉体发生化学反应的气体。铌粉被送入等离子体炬的芯部高温区，吸收大量的热量，颗粒表面开始熔化，由于表面张力的作用，形成球形度很高的铌粉颗粒。2. Use the carrier gas to inject metal niobium powder (raw powder) into the high temperature zone of the core of the argon plasma torch for heating. The carrying gas can be argon, hydrogen and other gases that do not chemically react with the metal powder in a high temperature environment. The niobium powder is sent into the high temperature zone of the core of the plasma torch, where a large amount of heat is absorbed, and the surface of the particles begins to melt. Due to the effect of surface tension, niobium powder particles with a high degree of sphericity are formed.
3、将加热熔融后的铌粉颗粒液滴冷却固化形成球形铌粉末。铌粉颗粒液滴离开等离子炬后，在极高的温度梯度(10-6)下迅速冷却、进入热交换室骤冷凝固，从而形成球形的颗粒。3. Cool and solidify the heated and melted niobium powder particle droplets to form spherical niobium powder. After the niobium powder particles leave the plasma torch, they are rapidly cooled under a very high temperature gradient (10 -6 ), enter the heat exchange chamber, and are quenched and solidified to form spherical particles.
4、将气体抽离，收集球形铌粉。球化过程完成后，将气体抽离、处理排放，球化粉体进入收集储罐，自动计量收集。最后进行真空包装。4. Extract the gas and collect spherical niobium powder. After the spheroidization process is completed, the gas is extracted, treated and discharged, and the spheroidized powder enters the collection storage tank for automatic metering and collection. Finally vacuum pack.
实施例1：Example 1:
以200目的铌粉为原料，球化过程稳定运行时，感应线圈上加载的高电压为7.8KV，Ar反应气体输入流量为40slpm，保护气75slpm，系统内气压为0.04MPa；携带气体控制流量为1slpm，铌粉喂料控制流量为19g/min。球化后得到200目的球形铌粉。Using 200-mesh niobium powder as raw material, when the spheroidization process is running stably, the high voltage loaded on the induction coil is 7.8KV, the input flow rate of Ar reaction gas is 40slpm, the protective gas is 75slpm, the pressure in the system is 0.04MPa; the control flow rate of the carrying gas is 1slpm, niobium powder feeding control flow rate is 19g/min. After spheroidization, 200-mesh spherical niobium powder was obtained.
图2是原料铌粉的不规则颗粒显微形貌，颗粒具有多边的棱角。Figure 2 is the microscopic appearance of irregular particles of raw material niobium powder, the particles have polygonal edges and corners.
图3是实施例1制备的球形铌粉显微形貌图。如图3所示，制备的铌粉颗粒球化率高，球形度好，表面光洁。FIG. 3 is a microscopic view of the spherical niobium powder prepared in Example 1. As shown in Figure 3, the prepared niobium powder particles have high spheroidization rate, good sphericity and smooth surface.
图4是实施例1制备的球形铌粉物相测试(XRD)，与原粉对比。由图4可知，球化处理前粉末(图4a)与Nb粉标准衍射峰匹配，没有其他物质衍射峰存在。经等离子体球化处理后(图4b)，Nb粉的X射线衍射位置未发生变化，仍为(110)、(200)、(211))的特征衍射峰，晶体结构均为单一Nb相。这说明本发明中，等离子体的高温没有影响粉体的物相。Figure 4 is the phase test (XRD) of the spherical niobium powder prepared in Example 1, compared with the original powder. It can be seen from Figure 4 that the powder before spheroidization (Figure 4a) matches the standard diffraction peak of Nb powder, and no diffraction peaks of other substances exist. After plasma spheroidization (Figure 4b), the X-ray diffraction position of Nb powder has not changed, and it is still the characteristic diffraction peaks of (110), (200), (211)), and the crystal structure is a single Nb phase. This shows that in the present invention, the high temperature of the plasma does not affect the phase of the powder.
实施例2：Example 2:
以300目的铌粉为原料，球化过程稳定运行时，感应线圈上加载的高电压为11.5KV，Ar反应气体输入流量为25slpm，保护气120slpm，系统内气压为0.05MPa；携带气体控制流量为1slpm，铌粉喂料控制流量为30g/min。球化后得到300目的球形铌粉，扫描电镜如图5。Using 300-mesh niobium powder as raw material, when the spheroidization process is running stably, the high voltage loaded on the induction coil is 11.5KV, the input flow rate of the Ar reaction gas is 25slpm, the protective gas is 120slpm, and the pressure in the system is 0.05MPa; the control flow rate of the carrying gas is 1slpm, niobium powder feeding control flow rate is 30g/min. After spheroidization, 300-mesh spherical niobium powder was obtained, and the scanning electron microscope is shown in Figure 5.
图5是实施例2制备的球形铌粉显微形貌图。如图5所示，制备的铌粉颗粒球化率高，球形度好，表面光洁。Fig. 5 is a microscopic view of the spherical niobium powder prepared in Example 2. As shown in Figure 5, the prepared niobium powder particles have high spheroidization rate, good sphericity and smooth surface.
实施例2中使用的原料铌粉的显微形貌与实施例1中使用的原料铌粉类似，均为不规则颗粒，颗粒具有多边的棱角。The microscopic appearance of the raw material niobium powder used in Example 2 is similar to that of the raw material niobium powder used in Example 1, both of which are irregular particles with polygonal edges and corners.
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