WO2011082596A1 - Short-flow preparation method for fine spherical titanium powder - Google Patents

Short-flow preparation method for fine spherical titanium powder Download PDF

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Publication number
WO2011082596A1
WO2011082596A1 PCT/CN2010/077381 CN2010077381W WO2011082596A1 WO 2011082596 A1 WO2011082596 A1 WO 2011082596A1 CN 2010077381 W CN2010077381 W CN 2010077381W WO 2011082596 A1 WO2011082596 A1 WO 2011082596A1
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powder
titanium
titanium powder
short
fine
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PCT/CN2010/077381
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French (fr)
Chinese (zh)
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郭志猛
盛艳伟
曲选辉
郝俊杰
邵慧萍
罗骥
林涛
王述超
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北京科技大学
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Publication of WO2011082596A1 publication Critical patent/WO2011082596A1/en

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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
    • B22F9/023—Hydrogen absorption
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Definitions

  • the invention belongs to the technical field of powder preparation, and in particular provides a short-flow preparation method of fine spherical titanium powder.
  • Titanium and titanium alloys have excellent properties such as low density, high specific strength, good corrosion resistance, high heat resistance, non-magnetic, and good splicing performance. They can be widely used in aerospace, automotive, bioengineering, watches, sporting goods, Environmental protection and other fields. However, in the preparation of titanium and titanium alloy near-net forming products with complex shapes, uniform structure and high performance, the most applied powder injection molding and gel injection molding have higher requirements on the powder in the process, and it requires titanium powder. The particle size is fine, uniform, regular in shape, good in fluidity, and low in oxygen content, while ordinary titanium powder is difficult to meet its requirements.
  • the shape of the titanium powder prepared by the gas atomization method is spherical, the fluidity is good, the oxygen content is low, the particle size distribution is uneven, and the production cost is high, it is important to provide a method for preparing the fine spherical titanium powder.
  • a method for preparing fine spherical metal titanium powder has low productivity and high cost.
  • the radio frequency plasma method can prepare titanium powder or titanium alloy powder with uniform composition, less defects, good fluidity and good sphericity, and has low production cost and high productivity. It is a good technique. way.
  • the plasma has the characteristics of high temperature, high enthalpy, high activity and large temperature gradient.
  • the use of plasma as a heat source has great technical advantages in the micron submicron and the spheroidization treatment of some nano powder materials.
  • RF plasma technology and equipment are more widely used in the field of powder materials than microwave and DC arc plasma heat sources because they do not introduce any impurities, stable operation, fast material processing speed, high productivity and moderate equipment cost.
  • the principle of radio frequency (RF) plasma spheroidizing metal powder is as follows: The metal powder is fed into the high temperature plasma with a carrier gas under a protective atmosphere, and the powder particles rapidly absorb heat to melt the surface (or the whole), and the surface tension Under the action, it is condensed into a spherical shape, and the powder passes through the plasma high temperature zone and enters the cooling chamber, and the spherical shape is fixed by the quenching action, thereby obtaining a spherical powder.
  • Plasma melting spheroidization is considered to be the most effective means of obtaining dense, regular spherical particles.
  • the powder prepared by radio frequency (RF) plasma melting spheroidization technology has high sphericity, good fluidity, uniform particle size and low impurity content.
  • the invention aims to solve the problems of oxidation and the like in the process of spheroidization and spheroidization of fine titanium powder, and provides a preparation method of fine spherical titanium powder used for injection molding, gel injection molding technology and the like in powder metallurgy This method saves energy, reduces pollution, improves production efficiency, and reduces production costs.
  • the object of the present invention is achieved by a short-flow preparation method of fine spherical titanium powder, which uses titanium hydride (TiH 2 ) powder as a raw material to directly dehydrogenate, crush and melt the ball by radio frequency (RF) plasma spheroidization.
  • TiH 2 titanium hydride
  • RF radio frequency
  • a short-flow preparation method of fine spherical titanium powder comprises the following steps: filling the entire reaction device with argon gas as a shielding gas, establishing a stable operating RF plasma, and feeding the raw material into the plasma high temperature region with argon as a carrier gas
  • the raw material is rapidly and endothermicly cracked to form fine titanium powder, and the titanium powder absorbs heat and spheroidizes and rapidly solidifies into a spherical powder;
  • the preparation method selects titanium hydride powder as a raw material, and the titanium hydride powder is sucked in a high temperature radio frequency plasma. It decomposes with heat and decomposes rapidly, and is cracked and broken during dehydrogenation to form fine titanium powder.
  • TiH 2 titanium hydride
  • the main process parameters are: power 30 ⁇ 80KW, argon working gas flow 20 ⁇ 35slpm, argon shielding gas flow 150 ⁇ 300slpm, system negative pressure 200 ⁇ 280mm Hg.
  • TiH 2 titanium hydride
  • Titanium hydride (TiH 2 ) powder absorbs heat in high-temperature RF plasma and rapidly decomposes dehydrogenation. At the same time, in the process of dehydrogenation, the particles are cracked and broken to form fine titanium powder due to rapid heat absorption and release of a large amount of hydrogen. The powder is absorbed by heat and spheroidized and quenched and solidified into a spherical powder; the fine spherical titanium powder is collected by cyclone separation.
  • the titanium hydride powder raw material has an average particle size of 50 to 250 ⁇ m, and the prepared fine spherical titanium powder has a particle size of 10 to 50 m.
  • the titanium hydride powder is injected from the upper portion of the radio frequency plasma center to sufficiently heat the titanium hydride powder to prevent electrode contamination.
  • the radio frequency plasma is used as the heat source, and the argon gas is the plasma working gas to reduce the oxidation problem of the titanium powder during the spheroidization process.
  • the powder can be injected from the upper part of the plasma center, and the volume is large, the heating is sufficient, and there is no electrode pollution.
  • the prepared fine spherical titanium powder has fine particle size, uniformity, good fluidity, high sphericity and low oxygen content.
  • FIG. 1 is a schematic view showing the preparation of fine spherical titanium powder by the short process of the present invention
  • 2 is a scanning electron micrograph of a titanium hydride (TiH 2 ) powder used in the present invention
  • FIG. 3 is a scanning electron micrograph of the fine spherical titanium powder prepared by the present invention.
  • a short-flow preparation method of fine spherical titanium powder is carried out as follows: First, titanium hydride (TiH 2 ) powder is selected as a raw material, and argon gas is used as a shielding gas to fill the entire reaction device to avoid oxidation during powder spheroidization .
  • TiH 2 titanium hydride
  • Titanium hydride belongs to a metal type hydride, which can be used as a hydrogen storage material itself, and can be used to prepare high-purity fine titanium powder by utilizing its brittleness and dehydrogenation behavior under vacuum high temperature.
  • TiH 2 undergoes the following decomposition reaction at 620 to 720 ° C in the absence of oxygen and nitrogen:
  • TiH 2 Ti + H 2 ⁇
  • the argon working gas flow required for RF plasma input is 20 ⁇ 35slpm, maintaining the power of 30 ⁇ 80KW, inputting argon shielding gas flow rate 150 ⁇ 300slpm, system negative pressure 200 ⁇ 280mmHg, establishing stable operation of RF plasma .
  • the titanium hydride (TiH 2 ) powder was fed into the plasma high temperature zone with argon as the carrier gas, and the carrier gas flow rate was 4 to 7 slpm, and the powder feeding rate was 25 to 80 g/min.
  • the titanium hydride powder can also be injected from the upper portion of the RF plasma center to sufficiently heat the titanium hydride powder to prevent electrode contamination.
  • the use of larger particle size hydrogenated titanium powder as raw material solves the problems of powder agglomeration and discontinuous transport during the transportation of fine powder.
  • Titanium hydride (TiH 2 ) powder is fed into a high temperature plasma with a carrier gas under a protective atmosphere. Hydrogenated-dehydrogenation (HDH) technology is combined with RF plasma melting spheroidization technology to form titanium hydride (TiH 2 ) powder. In the high temperature plasma, it absorbs heat and decomposes rapidly, and at the same time, in the process of dehydrogenation, the particles are cracked and broken to form fine titanium powder due to rapid heat absorption and release of a large amount of hydrogen. The titanium powder absorbs heat and spheroidizes and acts under surface tension.
  • HDH Hydrogenated-dehydrogenation
  • RF plasma melting spheroidization technology to form titanium hydride (TiH 2 ) powder.
  • the titanium powder absorbs heat and spheroidizes and acts under surface tension.
  • FIG. 1 is The schematic diagram of preparing the fine spherical titanium powder by the short process of the invention is as shown in the figure:
  • the large particle titanium hydride powder is transported into the radio frequency plasma, decomposes and dehydrogenates due to rapid heat absorption, and the powder is cracked and broken into fine titanium powder, and the titanium powder is After the radio frequency plasma, it absorbs heat and melts to form spherical titanium powder.
  • Figure 2 provides a scanning electron micrograph of the original titanium hydride powder.
  • the original shape of the titanium hydride powder is irregular, and the powder particles have polygonal corners, and most of the particles are in the range of about 100 to 250 ⁇ m.
  • Figure 3 provides a scanning electron micrograph of the fine spherical titanium powder prepared by the present invention.
  • the spherical titanium powder prepared has a high spheroidization rate, a good sphericity, and a uniform particle size, and most of the powder has a particle size of 10 to 25 m. about.
  • the preparation method of the invention directly completes the dehydrogenation and spheroidization treatment process of the titanium hydride powder by plasma treatment, and realizes a short process to prepare the fine spherical titanium powder.
  • a fine spherical titanium powder having an average particle diameter of 15 pm was prepared.
  • titanium hydride (TiH 2 ) powder with an average particle size of lOOpm as the raw material the stable operating radio frequency (RF) plasma power is 50 KW, the argon working gas flow rate is 30 slpm, the argon shielding gas flow rate is 150 slpm, and the system negative pressure is 200mm Hg.
  • the titanium hydride powder was fed into a high-temperature plasma at a flow rate of 4 slpm, and the powder was conveyed at a rate of 40 g/min. After the spheroidization treatment, fine spherical titanium powder having an average particle diameter of 15 pm was obtained by cyclone separation.
  • a fine spherical titanium powder having an average particle diameter of 20 pm was prepared.
  • titanium hydride (TiH 2 ) powder with an average particle size of 150 pm as the raw material the stable operating radio frequency (RF) plasma power is 60 KW, the argon working gas flow rate is 40 slpm, the argon shielding gas flow rate is 200 slpm, and the system negative pressure is 230 mm Hg.
  • the titanium hydride powder was fed into a high-temperature plasma at a flow rate of 4.5 slpm, and the powder was transported at a rate of 50 g/min. After spheroidization, fine spherical titanium powder having an average particle diameter of 20 ⁇ m was obtained by cyclone separation.
  • a fine spherical titanium powder having an average particle diameter of 10 pm was prepared.
  • the stable operating radio frequency (RF) plasma power is 45 KW
  • the argon working gas flow rate is 30 slpm
  • the argon shielding gas flow rate is 200 slpm
  • the system negative pressure is 200mm Hg.
  • the titanium hydride powder was fed into a high-temperature plasma at a flow rate of 4 slpm, and the powder was conveyed at a rate of 30 g/min. After the spheroidization treatment, fine spherical titanium powder having an average particle diameter of 10 pm was obtained by cyclone separation.
  • a fine spherical titanium powder having an average particle diameter of 40 pm was prepared.
  • titanium hydride (TiH 2 ) powder with an average particle size of 250 ⁇ as raw material the stable operating radio frequency (RF) plasma power is 65KW, the argon working gas flow rate is 40slpm, the argon shielding gas flow rate is 280slpm, and the system negative pressure is 260mm Hg.
  • the titanium hydride powder was fed into a high-temperature plasma at a flow rate of 6 slpm, and the powder was conveyed at a rate of 60 g/min. After spheroidization, a fine spherical titanium powder having an average particle diameter of 40 ⁇ m was obtained by cyclone separation.

Abstract

A short-flow preparation method for fine spherical titanium powder combines hydrogenation-dehydrogenation process with a radio frequency plasma fusion spheroidization process. In the method, the titanium hydride powder as raw material absorbs heat in the high-temperature plasma zone and quickly decomposes and dehydrogenates, and it cracks and smashes to produce fine titanium powder during the dehydrogenation process. By performing the method, the dehydrogenation process of the titanium hydride powder and the spheroidization process of the generated titanium powder are finished in one step by the plasma treatment, so that the short-flow preparation of the fine spherical titanium powder is realized. The invention shortens the production flow, improves the production efficiency and reduces the production cost. Furthermore, the generated spherical titanium powder has fine and even particles, a good fluidity, a high sphericity and low oxygen content.

Description

一种微细球形钛粉的短流程制备方法  Short flow preparation method of fine spherical titanium powder
技术领域 Technical field
本发明属于粉末制备技术领域， 特别是提供了一种微细球形钛粉 的短流程制备方法。 技术背景  The invention belongs to the technical field of powder preparation, and in particular provides a short-flow preparation method of fine spherical titanium powder. technical background
钛及钛合金具有密度低、 比强度高、 耐蚀性好、 耐热性高、 无磁、 悍接性能好等优良性能， 可广泛应用于航空航天、 汽车、 生物工程、 手表、 体育用品、 环保等领域。 但目前在制备形状复杂、 结构均匀、 高性能的钛及钛合金近净成形产品方面， 应用最多的粉末注射成型及 凝胶注摸成型在工艺上对粉体的要求较高， 它要求钛粉粒度细小、 均 匀， 形状规则， 流动性好， 且氧含量低， 而普通钛粉难于满足其要求。 对于气雾化法制备的钛粉形状虽为球形， 流动性好、 氧含量低， 但粒 度分布不均匀， 且生产成本高， 因此提供一种制备微细球形钛粉的方 法是很重要的。  Titanium and titanium alloys have excellent properties such as low density, high specific strength, good corrosion resistance, high heat resistance, non-magnetic, and good splicing performance. They can be widely used in aerospace, automotive, bioengineering, watches, sporting goods, Environmental protection and other fields. However, in the preparation of titanium and titanium alloy near-net forming products with complex shapes, uniform structure and high performance, the most applied powder injection molding and gel injection molding have higher requirements on the powder in the process, and it requires titanium powder. The particle size is fine, uniform, regular in shape, good in fluidity, and low in oxygen content, while ordinary titanium powder is difficult to meet its requirements. Although the shape of the titanium powder prepared by the gas atomization method is spherical, the fluidity is good, the oxygen content is low, the particle size distribution is uneven, and the production cost is high, it is important to provide a method for preparing the fine spherical titanium powder.
目前制备细小球形金属钛粉末的方法， 生产率较低， 成本较高。 射频等离子体法能制备出组分均匀、 缺陷少、 流动性好、 球形度好的 钛粉或钛合金粉， 又兼备较低的生产成本， 较高的生产率， 是一种较 好的技述途径。 等离子体具有高温、 高焓、 高活性和温度梯度大的特 性， 用等离子体做热源在微米亚微米以及某些纳米粉末材料的球化处 理方面， 具有较大的技术优势。 射频等离子体技术和设备由于其不引 入任何杂质、 运行持续稳定、 材料处理速度快、 产能高和设备造价适 中， 使之较微波和直流弧等离子体热源更广泛地应用于粉末材料技术 领域。 在高性能结构材料或功能材料制备和加工领域具有更高的应用 价值。 射频 （RF) 等离子体球化处理金属粉末的原理为： 在保护气氛 下用载气将金属粉末送入高温等离子体中， 粉末颗粒迅速吸热使其表 面 (或整体） 熔融， 并在表面张力作用下缩聚成球状， 粉末通过等离子 高温区后进入冷却室， 由于骤冷作用而将球形固定下来， 从而获得球 形粉末。 等离子熔融球化技术被认为是获得致密、 规则球形颗粒的最 有效手段。 射频 （RF) 等离子体熔融球化技术制备的粉末球形度高、 流动性好、 粒度均匀、 杂质含量低。 At present, a method for preparing fine spherical metal titanium powder has low productivity and high cost. The radio frequency plasma method can prepare titanium powder or titanium alloy powder with uniform composition, less defects, good fluidity and good sphericity, and has low production cost and high productivity. It is a good technique. way. The plasma has the characteristics of high temperature, high enthalpy, high activity and large temperature gradient. The use of plasma as a heat source has great technical advantages in the micron submicron and the spheroidization treatment of some nano powder materials. RF plasma technology and equipment are more widely used in the field of powder materials than microwave and DC arc plasma heat sources because they do not introduce any impurities, stable operation, fast material processing speed, high productivity and moderate equipment cost. Higher application in the field of high performance structural materials or functional material preparation and processing Value. The principle of radio frequency (RF) plasma spheroidizing metal powder is as follows: The metal powder is fed into the high temperature plasma with a carrier gas under a protective atmosphere, and the powder particles rapidly absorb heat to melt the surface (or the whole), and the surface tension Under the action, it is condensed into a spherical shape, and the powder passes through the plasma high temperature zone and enters the cooling chamber, and the spherical shape is fixed by the quenching action, thereby obtaining a spherical powder. Plasma melting spheroidization is considered to be the most effective means of obtaining dense, regular spherical particles. The powder prepared by radio frequency (RF) plasma melting spheroidization technology has high sphericity, good fluidity, uniform particle size and low impurity content.
以氢化钛为原料， 应用上述射频 （RF) 等离子体球化处理金属粉 末的原理制备微细球形钛粉的方法， 目前还未见报道。 发明内容  The method of preparing fine spherical titanium powder by using the above-mentioned radio frequency (RF) plasma spheroidizing metal powder by using titanium hydride as a raw material has not been reported yet. Summary of the invention
本发明的目的在于解决微细钛粉球化和球化过程中的氧化等问 题， 提供一种用于粉末冶金中的注射成型、 凝胶注模成型技术等工艺 使用的微细球形钛粉的制备方法， 本方法节约能源、 减少污染、 提高 生产效率、 降低生产成本。  The invention aims to solve the problems of oxidation and the like in the process of spheroidization and spheroidization of fine titanium powder, and provides a preparation method of fine spherical titanium powder used for injection molding, gel injection molding technology and the like in powder metallurgy This method saves energy, reduces pollution, improves production efficiency, and reduces production costs.
本发明的目的通过以下方式实现， 一种微细球形钛粉的短流程制 备方法， 以氢化钛（TiH2)粉末为原料， 直接通过射频 （RF) 等离子体 球化处理脱氢、 破碎、 熔融球化制备球形钛粉， 实现球形钛粉的短流 程制备。 The object of the present invention is achieved by a short-flow preparation method of fine spherical titanium powder, which uses titanium hydride (TiH 2 ) powder as a raw material to directly dehydrogenate, crush and melt the ball by radio frequency (RF) plasma spheroidization. The spherical titanium powder is prepared to realize the short process preparation of spherical titanium powder.
一种微细球形钛粉的短流程制备方法， 包括以下步骤： 以氩气为 保护气充满整个反应装置， 建立稳定运行的射频等离子体， 以氩气为 携带气将原料送入等离子体高温区后， 原料迅速吸热裂解生成的微细 钛粉， 钛粉吸热熔融球化并骤冷固化成球形粉末； 所述制备方法选取 氢化钛粉末为原料， 所述氢化钛粉末在高温射频等离子体中吸热并迅 速分解脱氢， 并在脱氢过程中裂解、 破碎生成微细钛粉。  A short-flow preparation method of fine spherical titanium powder comprises the following steps: filling the entire reaction device with argon gas as a shielding gas, establishing a stable operating RF plasma, and feeding the raw material into the plasma high temperature region with argon as a carrier gas The raw material is rapidly and endothermicly cracked to form fine titanium powder, and the titanium powder absorbs heat and spheroidizes and rapidly solidifies into a spherical powder; the preparation method selects titanium hydride powder as a raw material, and the titanium hydride powder is sucked in a high temperature radio frequency plasma. It decomposes with heat and decomposes rapidly, and is cracked and broken during dehydrogenation to form fine titanium powder.
具体包括以下步骤：  Specifically, the following steps are included:
( 1 ) 选取氢化钛（ TiH2)粉末为原料， 以氩气为保护气充满整个反应 装置， 避免粉末球化过程中的氧化。 (1) Select titanium hydride (TiH 2 ) powder as raw material, and fill the whole reaction with argon as shielding gas. Device to avoid oxidation during powder spheroidization.
(2)建立稳定运行的射频等离子体， 其主要工艺参数为： 功率 30〜 80KW, 氩气工作气流量 20〜35slpm， 氩气保护气流量 150〜300slpm， ***负压 200〜280mm汞柱。  (2) Establish stable operation of RF plasma. The main process parameters are: power 30~80KW, argon working gas flow 20~35slpm, argon shielding gas flow 150~300slpm, system negative pressure 200~280mm Hg.
(3 ) 以氩气为携带气将氢化钛 （TiH2) 粉末送入等离子高温区， 其 携带气流量 4〜7 slpm, 送粉速率为 25〜80g/min。 (3) The titanium hydride (TiH 2 ) powder is fed into the plasma high temperature zone with argon as the carrier gas, and the carrier gas flow rate is 4 to 7 slpm, and the powder feeding rate is 25 to 80 g/min.
(4)氢化钛 (TiH2)粉末在高温射频等离子体中吸热并迅速分解脱氢， 同时在脱氢过程中由于迅速吸热和释放出大量氢气使颗粒裂解、 破碎生 成微细钛粉， 钛粉吸热熔融球化并骤冷固化成球形粉末； 旋风分离收集 微细球形钛粉。 (4) Titanium hydride (TiH 2 ) powder absorbs heat in high-temperature RF plasma and rapidly decomposes dehydrogenation. At the same time, in the process of dehydrogenation, the particles are cracked and broken to form fine titanium powder due to rapid heat absorption and release of a large amount of hydrogen. The powder is absorbed by heat and spheroidized and quenched and solidified into a spherical powder; the fine spherical titanium powder is collected by cyclone separation.
所述的氢化钛粉末原料的平均粒度为 50〜250μηι， 制备出的微细球 形钛粉的粒度为 10〜50 m。  The titanium hydride powder raw material has an average particle size of 50 to 250 μm, and the prepared fine spherical titanium powder has a particle size of 10 to 50 m.
所述氢化钛粉末从射频等离子体中心上部注入， 使氢化钛粉末加 热充分， 防止电极污染。  The titanium hydride powder is injected from the upper portion of the radio frequency plasma center to sufficiently heat the titanium hydride powder to prevent electrode contamination.
本发明的优点在于：  The advantages of the invention are:
( 1 )采用氢化钛粉末为原料， 减少了氢化一脱氢工艺流程的脱氢工 序， 缩短工艺流程， 提高生产效率， 节约能源， 降低生产成本。  (1) Using titanium hydride powder as raw material, the dehydrogenation process of the hydrogenation-dehydrogenation process is reduced, the process flow is shortened, the production efficiency is improved, the energy is saved, and the production cost is reduced.
(2)采用较大粒度氢化钛粉末为原料， 解决微细粉末输送过程中存 在的粉末团聚和输送不连续等问题。  (2) Using a larger particle size hydrogenated titanium powder as a raw material to solve the problems of powder agglomeration and discontinuous transport during the transportation of fine powder.
(3 )采用射频等离子体为热源， 氩气为等离子工作气， 减少球化过 程中钛粉的氧化问题， 同时粉末可从等离子体中心上部注入， 体积大， 加热充分， 无电极污染。  (3) The radio frequency plasma is used as the heat source, and the argon gas is the plasma working gas to reduce the oxidation problem of the titanium powder during the spheroidization process. At the same time, the powder can be injected from the upper part of the plasma center, and the volume is large, the heating is sufficient, and there is no electrode pollution.
(4) 制备的微细球形钛粉粒度细小、 均匀， 流动性好、 球形度高、 氧含量低。 附图说明  (4) The prepared fine spherical titanium powder has fine particle size, uniformity, good fluidity, high sphericity and low oxygen content. DRAWINGS
图 1是本发明短流程制备微细球形钛粉的示意图； 图 2是本发明使用的氢化钛 （TiH2) 原粉扫描电镜图； 图 3是本发明制备的微细球形钛粉的扫描电镜图。 具体实施方式 Figure 1 is a schematic view showing the preparation of fine spherical titanium powder by the short process of the present invention; 2 is a scanning electron micrograph of a titanium hydride (TiH 2 ) powder used in the present invention; and FIG. 3 is a scanning electron micrograph of the fine spherical titanium powder prepared by the present invention. detailed description
一种微细球形钛粉的短流程制备方法， 该方法按以下步骤进行： 首先选取氢化钛（ TiH2)粉末为原料， 以氩气为保护气充满整个反应装 置， 避免粉末球化过程中的氧化。 A short-flow preparation method of fine spherical titanium powder, the method is carried out as follows: First, titanium hydride (TiH 2 ) powder is selected as a raw material, and argon gas is used as a shielding gas to fill the entire reaction device to avoid oxidation during powder spheroidization .
采用氢化钛粉末为原料， 减少了氢化一脱氢工艺流程的脱氢工序， 缩 短工艺流程， 节约能源， 降低生产成本。 氢化钛 (TiH2)属于一种金属型氢 化物， 其本身可以作为储氢材料， 利用其脆性及在真空高温下的脱氢行 为， 可以用它来制备高纯微细钛粉。 Using titanium hydride powder as raw material, the dehydrogenation process of the hydrogenation-dehydrogenation process is reduced, the process flow is shortened, energy is saved, and production cost is reduced. Titanium hydride (TiH 2 ) belongs to a metal type hydride, which can be used as a hydrogen storage material itself, and can be used to prepare high-purity fine titanium powder by utilizing its brittleness and dehydrogenation behavior under vacuum high temperature.
TiH2在无氧、 氮气存在的条件下 620〜720°C发生如下分解反应： TiH 2 undergoes the following decomposition reaction at 620 to 720 ° C in the absence of oxygen and nitrogen:
TiH2 = Ti + H2† TiH 2 = Ti + H 2 †
向射频等离子体输入所需要的氩气工作气流量 20〜35slpm， 保持 30〜80KW的功率，输入氩气保护气流量 150〜300slpm，***负压 200〜 280mm汞柱， 建立稳定运行的射频等离子体。  The argon working gas flow required for RF plasma input is 20~35slpm, maintaining the power of 30~80KW, inputting argon shielding gas flow rate 150~300slpm, system negative pressure 200~280mmHg, establishing stable operation of RF plasma .
以氩气为携带气将氢化钛 （TiH2) 粉末送入等离子高温区， 其携带 气流量 4〜7 slpm, 送粉速率为 25〜80g/min。 氢化钛粉末还可从射频等 离子体中心上部注入， 使氢化钛粉末加热充分， 防止电极污染。 采用较 大粒度氢化钛粉末为原料， 解决微细粉末输送过程中存在的粉末团聚和 输送不连续等问题。 The titanium hydride (TiH 2 ) powder was fed into the plasma high temperature zone with argon as the carrier gas, and the carrier gas flow rate was 4 to 7 slpm, and the powder feeding rate was 25 to 80 g/min. The titanium hydride powder can also be injected from the upper portion of the RF plasma center to sufficiently heat the titanium hydride powder to prevent electrode contamination. The use of larger particle size hydrogenated titanium powder as raw material solves the problems of powder agglomeration and discontinuous transport during the transportation of fine powder.
在保护气氛下， 用载气将氢化钛 ( TiH2)粉末送入高温等离子体中，利用 氢化一脱氢 （HDH) 技术与射频等离子体熔融球化技术相结合， 氢化钛 (TiH2)粉末在高温等离子体中吸热并迅速分解脱氢， 同时在脱氢过程中由 于迅速吸热和释放大量氢气使颗粒裂解、 破碎生成微细钛粉， 钛粉吸热 熔融球化并在表面张力作用下缩聚成球状， 粉末通过等离子高温区后进 入冷却室， 由于骤冷作用而将球形固定下来， 从而获得球形粉末。 图 1是 本发明短流程制备微细球形钛粉的示意图， 如图所示： 大颗粒氢化钛粉 末输送到射频等离子体中， 由于迅速吸热而分解脱氢， 粉末裂解、 破碎 为微细钛粉， 钛粉在经过射频等离子体后吸热熔融形成球形钛粉。 Titanium hydride (TiH 2 ) powder is fed into a high temperature plasma with a carrier gas under a protective atmosphere. Hydrogenated-dehydrogenation (HDH) technology is combined with RF plasma melting spheroidization technology to form titanium hydride (TiH 2 ) powder. In the high temperature plasma, it absorbs heat and decomposes rapidly, and at the same time, in the process of dehydrogenation, the particles are cracked and broken to form fine titanium powder due to rapid heat absorption and release of a large amount of hydrogen. The titanium powder absorbs heat and spheroidizes and acts under surface tension. The polycondensation is spherical, and the powder passes through the plasma high temperature zone and enters the cooling chamber, and the spherical shape is fixed by the quenching action, thereby obtaining a spherical powder. Figure 1 is The schematic diagram of preparing the fine spherical titanium powder by the short process of the invention is as shown in the figure: The large particle titanium hydride powder is transported into the radio frequency plasma, decomposes and dehydrogenates due to rapid heat absorption, and the powder is cracked and broken into fine titanium powder, and the titanium powder is After the radio frequency plasma, it absorbs heat and melts to form spherical titanium powder.
图 2提供了氢化钛原粉的扫描电镜图， 如图所示， 氢化钛原粉形状 不规则， 粉末颗粒具有多边的棱角， 大部分颗粒在 100〜250μπι左右。 图 3提供了本发明制备的微细球形钛粉的扫描电镜图，如图所示，制备的球 形钛粉球化率高，球形度好，并且粒度均匀细小，大部分粉末粒度在 10〜 25 m左右。  Figure 2 provides a scanning electron micrograph of the original titanium hydride powder. As shown in the figure, the original shape of the titanium hydride powder is irregular, and the powder particles have polygonal corners, and most of the particles are in the range of about 100 to 250 μm. Figure 3 provides a scanning electron micrograph of the fine spherical titanium powder prepared by the present invention. As shown in the figure, the spherical titanium powder prepared has a high spheroidization rate, a good sphericity, and a uniform particle size, and most of the powder has a particle size of 10 to 25 m. about.
本发明的制备方法直接通过等离子体处理使氢化钛粉的脱氢与球化 处理过程一步完成， 实现短流程制备微细球形钛粉。  The preparation method of the invention directly completes the dehydrogenation and spheroidization treatment process of the titanium hydride powder by plasma treatment, and realizes a short process to prepare the fine spherical titanium powder.
实例 1  Example 1
制备平均粒径为 15pm的微细球形钛粉。  A fine spherical titanium powder having an average particle diameter of 15 pm was prepared.
以平均粒度为 lOOpm 的氢化钛 （TiH2) 粉末为原料， 稳定运行的射 频 （RF) 等离子体功率为 50KW, 氩气工作气流量为 30slpm， 氩气保护 气的流量为 150slpm， ***负压为 200mm汞柱。 以流量为 4slpm的氩气 将氢化钛粉末送入高温等离子体中， 输送粉末速率为 40g/min， 球化处理 后经旋风分离即可收到平均粒径为 15pm的微细球形钛粉。 Using titanium hydride (TiH 2 ) powder with an average particle size of lOOpm as the raw material, the stable operating radio frequency (RF) plasma power is 50 KW, the argon working gas flow rate is 30 slpm, the argon shielding gas flow rate is 150 slpm, and the system negative pressure is 200mm Hg. The titanium hydride powder was fed into a high-temperature plasma at a flow rate of 4 slpm, and the powder was conveyed at a rate of 40 g/min. After the spheroidization treatment, fine spherical titanium powder having an average particle diameter of 15 pm was obtained by cyclone separation.
实例 2  Example 2
制备平均粒径为 20pm的微细球形钛粉。  A fine spherical titanium powder having an average particle diameter of 20 pm was prepared.
以平均粒度为 150pm 的氢化钛 （TiH2) 粉末为原料， 稳定运行的射 频 （RF) 等离子体功率为 60KW, 氩气工作气流量为 40slpm， 氩气保护 气的流量为 200slpm， ***负压为 230mm汞柱。 以流量为 4.5slpm的氩 气将氢化钛粉末送入高温等离子体中， 输送粉末速率为 50g/min， 球化处 理后经旋风分离即可收到平均粒径为 20μηι的微细球形钛粉。 Using titanium hydride (TiH 2 ) powder with an average particle size of 150 pm as the raw material, the stable operating radio frequency (RF) plasma power is 60 KW, the argon working gas flow rate is 40 slpm, the argon shielding gas flow rate is 200 slpm, and the system negative pressure is 230 mm Hg. The titanium hydride powder was fed into a high-temperature plasma at a flow rate of 4.5 slpm, and the powder was transported at a rate of 50 g/min. After spheroidization, fine spherical titanium powder having an average particle diameter of 20 μm was obtained by cyclone separation.
实施例 3  Example 3
制备平均粒径为 10pm的微细球形钛粉。 以平均粒度为 50pm的氢化钛（TiH2)粉末为原料， 稳定运行的射频 (RF) 等离子体功率为 45KW, 氩气工作气流量为 30slpm， 氩气保护气 的流量为 200slpm， ***负压为 200mm汞柱。 以流量为 4 slpm的氩气将 氢化钛粉末送入高温等离子体中， 输送粉末速率为 30g/min， 球化处理后 经旋风分离即可收到平均粒径为 10pm的微细球形钛粉。 A fine spherical titanium powder having an average particle diameter of 10 pm was prepared. Using titanium hydride (TiH 2 ) powder with an average particle size of 50 pm as the raw material, the stable operating radio frequency (RF) plasma power is 45 KW, the argon working gas flow rate is 30 slpm, the argon shielding gas flow rate is 200 slpm, and the system negative pressure is 200mm Hg. The titanium hydride powder was fed into a high-temperature plasma at a flow rate of 4 slpm, and the powder was conveyed at a rate of 30 g/min. After the spheroidization treatment, fine spherical titanium powder having an average particle diameter of 10 pm was obtained by cyclone separation.
实施例 4  Example 4
制备平均粒径为 40pm的微细球形钛粉。  A fine spherical titanium powder having an average particle diameter of 40 pm was prepared.
以平均粒度为 250μηι的氢化钛 （TiH2) 粉末为原料， 稳定运行的 射频 （RF ) 等离子体功率为 65KW, 氩气工作气流量为 40slpm， 氩气 保护气的流量为 280slpm， ***负压为 260mm汞柱。 以流量为 6slpm 的氩气将氢化钛粉末送入高温等离子体中， 输送粉末速率为 60g/min， 球化处理后经旋风分离即可收到平均粒径为 40μηι的微细球形钛粉。 Using titanium hydride (TiH 2 ) powder with an average particle size of 250μηι as raw material, the stable operating radio frequency (RF) plasma power is 65KW, the argon working gas flow rate is 40slpm, the argon shielding gas flow rate is 280slpm, and the system negative pressure is 260mm Hg. The titanium hydride powder was fed into a high-temperature plasma at a flow rate of 6 slpm, and the powder was conveyed at a rate of 60 g/min. After spheroidization, a fine spherical titanium powder having an average particle diameter of 40 μm was obtained by cyclone separation.

Claims

权 利 要 求 书 Claim
1.一种微细球形钛粉的短流程制备方法，包括以下步骤： 以氩气为保 护气充满整个反应装置， 建立稳定运行的射频等离子体， 以氩气为携带 气将原料送入等离子体高温区后， 原料迅速吸热裂解生成的微细钛粉， 钛粉吸热熔融球化并骤冷固化成球形粉末， 其特征在于， 所述制备方法 选取氢化钛粉末为原料， 所述氢化钛粉末在高温射频等离子体中吸热并 迅速分解脱氢， 并在脱氢过程中裂解、 破碎生成微细钛粉。 A short-flow preparation method of fine spherical titanium powder, comprising the steps of: filling the entire reaction device with argon as a shielding gas, establishing a stable operation of the radio frequency plasma, and feeding the raw material into the plasma with argon as a carrier gas; After the zone, the raw material is rapidly and endothermicly cracked to form fine titanium powder, and the titanium powder absorbs heat and spheroidizes and rapidly solidifies into a spherical powder, wherein the preparation method selects titanium hydride powder as a raw material, and the titanium hydride powder is The high-temperature RF plasma absorbs heat and rapidly decomposes dehydrogenation, and is cracked and broken in the dehydrogenation process to form fine titanium powder.
2.根据权利要求 1所述的微细球形钛粉的短流程制备方法，其特征在 于， 所述氢化钛粉末平均粒度为 50〜250μπι。 The short-flow preparation method of the fine spherical titanium powder according to claim 1, wherein the titanium hydride powder has an average particle size of 50 to 250 μm.
3. 根据权利要求 1所述的微细球形钛粉的短流程制备方法， 其特征 在于， 所述射频等离子体的功率为 30〜80KW， 氩气工作气流量 20〜 35slpm, 氩气保护气流量 150〜300slpm， ***负压 200〜280mm汞柱。 3. The short-flow preparation method of the fine spherical titanium powder according to claim 1, wherein the radio frequency plasma has a power of 30 to 80 KW, an argon working gas flow rate of 20 to 35 slpm, and an argon gas shielding gas flow rate of 150. ~300slpm, system negative pressure 200~280mm Hg.
4. 根据权利要求 1或 2所述的微细球形钛粉的短流程制备方法， 其 特征在于， 所述氢化钛粉末携带气流量为 4〜7 slpm, 送粉速率为 25〜 80g/min。 The short-flow preparation method of the fine spherical titanium powder according to claim 1 or 2, wherein the hydrogenated titanium powder has a gas flow rate of 4 to 7 slpm and a powder feeding rate of 25 to 80 g/min.
5. 根据权利要求 1或 3所述的微细球形钛粉的短流程制备方法， 其 特征在于， 所述氢化钛粉末从射频等离子体中心上部注入， 氢化钛粉末 加热更充分。 The short-flow preparation method of the fine spherical titanium powder according to claim 1 or 3, wherein the titanium hydride powder is injected from the upper portion of the radio frequency plasma center, and the titanium hydride powder is heated more fully.
6. 根据权利要求 1或 2所述的微细球形钛粉的短流程制备方法， 其 特征在于， 所述的微细球形钛粉的短流程制备方法制备出的微细球形钛 粉的粒度为 10〜50 m。 The short-flow preparation method of the fine spherical titanium powder according to claim 1 or 2, wherein the fine spherical titanium powder prepared by the short-flow preparation method of the fine spherical titanium powder has a particle size of 10 to 50 m.
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