CN105710390A - Method for preparing nano-grade molybdenum powder by directly utilizing industrial-grade molybdenum trioxide - Google Patents

Method for preparing nano-grade molybdenum powder by directly utilizing industrial-grade molybdenum trioxide Download PDF

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Publication number
CN105710390A
CN105710390A CN 201610293735 CN201610293735A CN105710390A CN 105710390 A CN105710390 A CN 105710390A CN 201610293735 CN201610293735 CN 201610293735 CN 201610293735 A CN201610293735 A CN 201610293735A CN 105710390 A CN105710390 A CN 105710390A
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molybdenum
gas
grade
temperature
trioxide
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CN 201610293735
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Chinese (zh)
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张国华
王璐
周国治
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北京科技大学
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/28Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from gaseous metal compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

Abstract

The invention relates to a method for preparing nano-grade molybdenum powder by directly utilizing industrial-grade molybdenum trioxide. The method comprises the following steps: firstly, putting the industrial-grade molybdenum trioxide into a high-temperature furnace and finally collecting nano-grade ultrafine molybdenum powder through adjusting flow speeds of different carrier gas and reaction gas under the conditions that the temperature is 950-1500 DEG C, argon gas is used as the carrier gas and hydrogen gas is used as the reaction gas; and drying an obtained product under a hydrogen gas atmosphere at 100 DEG C to obtain pure molybdenum powder. In a reaction process, molybdenum trioxide is volatilized into a gas state under a high-temperature condition, and the gas-state high-temperature is reacted with the hydrogen gas at a high temperature and a nano-grade product can be prepared in short time. According to the method provided by the invention, the industrial-grade molybdenum trioxide is reacted with the hydrogen gas under the high-temperature condition so that purification of the molybdenum trioxide is not needed and the ultrafine molybdenum powder with relatively high purity can also be prepared; and the method is relatively low in cost, and simple and process, and industrial production is easy to realize.

Description

一种直接利用工业级三氧化钼制备纳米级钼粉的方法 A direct method using a molybdenum trioxide powder preparing nanoscale industrial

技术领域 FIELD

[0001 ]本发明属于纳米材料制备领域,涉及一种气相反应制备纳米级钼粉的方法。 [0001] The present invention belongs to the field of preparation of nano materials, relates to a process for preparing nanoscale gas phase reactor molybdenum powder.

背景技术 Background technique

[0002] Mo为第六副族元素,拥有体心立方晶体结构,晶胞参数为0.3147nm,密度10.22g/cm3,熔点2610°C Jo和它的合金化合物目前已经广泛地应用于化学、冶金和电子工业,高的熔点,低的热膨胀系数和高的热电导率使得Mo成为半导体材料、熔渣电极和抗腐蚀材料的重要组成部分。 [0002] Mo is the sixth subgroup of the elements, body-centered cubic crystal structure has unit cell parameters 0.3147nm, density of 10.22g / cm3, a melting point of 2610 ° C Jo present compound and its alloys have been widely used chemical, metallurgical and electronics industries, high melting point, a low coefficient of thermal expansion and a high thermal conductivity so that the semiconductor material becomes Mo, an important part of the electrodes and slag corrosion resistant material. 目前,相比普通材料来说,纳米材料已经被证实拥有更加优异的性能,例如超细纳米钼粉可以广泛地应用于电子设备的电导薄膜,可以用来生产纳米级工具钢如M50钢种,而且还可以用来制备性能更加优异的MoSi2材料等等。 At present, as compared to conventional materials, a nano-material has proven to have a more excellent performance, for example, ultrafine nano molybdenum powder can be widely used electrically conductive thin film electronic devices, it can be used to produce nanoscale M50 tool steel grades such as, but also it is used to prepare more excellent properties of MoSi2 and the like. 因此,目前纳米Mo的合成和制备已经受到了很多专家的青睐。 Therefore, the current synthesis and preparation of nano-Mo has been favored by many experts.

[0003]现在,制备纳米Mo粉的方法有很多,如微波等离子体气相沉积法,H2还原机械活化的M0O3粉末,自蔓延高温合成法,石墨碳还原机械活化的Μ0Ο3粉末,Η2还原气态MoCh法和Η2还原纯净的MoO3蒸汽法等等。 [0003] Now, a method for preparing nano Mo powder have a lot, such as microwave plasma vapor deposition, H2 reduction M0O3 mechanically activated powder, SHS method, a mechanically activated reduction of graphitic carbon powder Μ0Ο3, [eta] 2 MoCh gaseous reduction method and Η2 reduction of MoO3 pure steam method, and so on. 这些方法虽然可以制备出超细的纳米钼粉,但是成本较高。 Although these methods can be prepared ultrafine nano molybdenum powder, but at a higher cost. 本专利采用廉价的工业级三氧化钼为原料,在高温下通入氢气还原气态三氧化钼,既可以免去净化三氧化钼的过程,又可以制备出纯净的纳米钼粉,是制备纳米钼粉的一种简便实用的方法。 This patent inexpensive industrial grade molybdenum trioxide as a raw material, at a high temperature into gaseous hydrogen reduction of molybdenum trioxide, molybdenum trioxide may be removed from the purification process, and can be prepared nano pure molybdenum powder, a molybdenum preparing nano one kind of powder is simple and practical method.

发明内容 SUMMARY

[0004]本发明的目的是提供一种采用高温气气反应制备超细纳米钼粉材料的方法。 [0004] The object of the present invention is to provide a method for the preparation of high-temperature gas-gas reaction of ultrafine material using nano-molybdenum powder. 采用工业级三氧化钼为原材料,在温度为950-1500°C的范围内,使三氧化钼挥发为气态,然后再与氢气接触发生气-气反应,制备出超细的纳米钼粉。 Industrial grade molybdenum trioxide as a raw material in the temperature range of 950-1500 ° C, so that gaseous volatile molybdenum trioxide, and then brought into contact with hydrogen gas - gas reaction to prepare ultrafine nanoparticles molybdenum powder.

[0005] —种直接利用工业级三氧化钼制备纳米级钼粉的方法;其特征在于所用原材料为工业级三氧化钼,将其挥发为气态后与还原气体接触,在高温炉中进行还原反应,得到纳米级材料,得到的产物由于含水,需要在氢气气氛下,100°C进行烘干,即可得纯净钼粉,所述工艺包括以下步骤: [0005] - industrial species directly preparing nanoscale molybdenum trioxide molybdenum powder; a method which is characterized in that technical grade molybdenum trioxide, after which volatile gaseous raw materials in contact with the reducing gas, the reduction reaction is carried out in a high temperature furnace to afford nanoscale materials, because the resulting aqueous product is required under a hydrogen atmosphere, 100 ° C for drying, to give the pure molybdenum powder, the process comprising the steps of:

[0006] I)将工业级三氧化钼在温度为950-1500°C高温挥发成气态三氧化钼; [0006] I) The technical grade molybdenum trioxide at a temperature of 950-1500 ° C into gaseous high temperature volatile molybdenum trioxide;

[0007] 2)挥发出来的气态三氧化钼与还原气体接触直接发生反应,三氧化钼被迅速还原为纳米级超细钼粉。 [0007] 2) volatilizing molybdenum trioxide in contact with the gaseous direct reduction reaction gas, is rapidly reduced to molybdenum trioxide ultrafine nano molybdenum powder.

[0008]本发明使用的原料为工业级三氧化钼,利用三氧化钼在高温下蒸汽压较大的特点,使其挥发后与还原气体反应,发生的还原反应为气-气反应,反应速度快。 [0008] The starting material used in the present invention is technical grade molybdenum trioxide, molybdenum trioxide vapor pressure greater use of the characteristics at a high temperature, it reacts with the reducing gas volatilized gas for reduction reaction - the reaction gas, the reaction rate fast.

[0009]使用的还原气体为纯氢气,或者为氢气与惰性气体的混合气。 [0009] The reducing gas used is pure hydrogen, or a mixed gas of hydrogen and inert gas.

[0010]本发明与现有技术相比,具备以下优点: [0010] Compared with the prior art, it has the following advantages:

[0011] I,本发明采用工业级三氧化钼为原料,相比于纯净的三氧化钼而言,更加低廉经济,制备的温度较低,工艺流程简单,且易于工业化生产。 [0011] I, the present invention employs technical grade molybdenum trioxide as a raw material, compared to pure molybdenum trioxide, it is more economical low, low temperature preparing process is simple, and easy industrial production.

[0012] 2,本发明采用高温气气反应制备纳米钼粉,由于是气体跟气体的直接接触,因此反应速率很快。 [0012] 2, the present invention employs a high temperature gas-gas reaction Nano molybdenum powder, because the gas is in direct contact with the gas, the reaction rate is so fast.

[0013] 3,本发明制备出的钼粉纯净高,且为纳米级材料。 [0013] 3, the present invention is prepared by high-purity molybdenum powder, and a nanoscale material.

附图说明 BRIEF DESCRIPTION

[0014]图1为实施例1得到的纳米钼粉的X射线衍射图(XRD)。 [0014] FIG. 1 is a nanometer molybdenum powder obtained in Example 1 X-ray diffraction (XRD).

[0015]图2为实施例1得到的纳米钼粉扫描电镜图片。 [0015] FIG. 2 is a molybdenum powder the nano-SEM image obtained in Example 1.

[0016]图3为实施例2得到的纳米钼粉扫描电镜图片。 [0016] FIG. 3 of Example 2 nm molybdenum powder obtained SEM image.

[0017]图4为实施例3得到的纳米钼粉的扫描电镜图。 [0017] FIG. 4 is a scanning electron micrograph of nano embodiment molybdenum powder obtained in Example 3.

具体实施方式 detailed description

[0018]下面结合具体实施例对本发明的技术方案做进一步说明。 [0018] The following specific embodiments described in conjunction with further aspect of the present invention.

[0019]实施例1:将工业三氧化钼放入高温炉中,在1100°C的温度下,采用载气Ar流速300ml/min,反应气H2流速500ml/min,反应时间为30min,最终可以得到纳米钼粉。 [0019] Example 1: the molybdenum trioxide into industrial high-temperature furnace, at a temperature of 1100 ° C, using Ar carrier gas flow rate of 300ml / min, H2 gas flow rate of the reaction 500ml / min, the reaction time was 30min, eventually nanoscaled molybdenum powder. 图1是制备出的纳米钼粉的X射线衍射图(XRD)证明产物为金属钼,且不存在其他杂相。 FIG 1 is a X-ray diffraction of the prepared nano molybdenum powder (XRD) confirmed that the product is a metal molybdenum, and there is no other impurity phases. 图2制备出的纳米钼粉的扫描电镜图,可以看出制备出的金属钼粉的颗粒大小约为50nm,且尺寸均匀。 Figure 2 a scanning electron microscope prepared nano FIG molybdenum powder, molybdenum can be seen that the particle size of the powder is about 50 nm were prepared, having a uniform size.

[0020] 实施例2:将工业三氧化钼放入高温炉中,在1050°C的温度下,采用载气Ar流速300ml/min,反应气H2流速500ml/min,反应时间为30min,最终可以得到纳米钼粉。 [0020] Example 2: molybdenum trioxide into industrial high-temperature furnace, at a temperature of 1050 ° C, using Ar carrier gas flow rate of 300ml / min, H2 gas flow rate of the reaction 500ml / min, the reaction time was 30min, eventually nanoscaled molybdenum powder. 图3制备出的纳米钼粉的扫描电镜图,可以看出制备出的金属钼粉的颗粒大小约为50nm,且尺寸均匀。 FIG SEM nano molybdenum powder prepared in FIG. 3, it can be seen molybdenum powder particle size of about 50 nm were prepared, having a uniform size.

[0021] 实施例3:将工业三氧化钼放入高温炉中,在1050°C的温度下,采用载气Ar流速300ml/min,反应气H2流速300ml/min,反应时间为30min,最终可以得到纳米钼粉。 [0021] Example 3: molybdenum trioxide into industrial high-temperature furnace, at a temperature of 1050 ° C, using Ar carrier gas flow rate of 300ml / min, H2 gas flow rate of the reaction 300ml / min, the reaction time was 30min, eventually nanoscaled molybdenum powder. 图4制备出的纳米钼粉的扫描电镜图,可以看出制备出的金属钼粉的颗粒大小约为50nm,且尺寸均匀。 FIG SEM nano molybdenum powder prepared in FIG. 4, the particle size can be seen that molybdenum metal powder is about 50 nm were prepared, having a uniform size.

Claims (3)

  1. 1.一种直接利用工业级三氧化钼制备纳米级钼粉的方法;其特征在于所用原材料为工业级三氧化钼,将其挥发为气态后与还原气体接触,在高温炉中进行还原反应,得到纳米级材料,得到的产物由于含水,需要在氢气气氛下,100°c进行烘干,即可得纯净钼粉,所述工艺包括以下步骤: 1)将工业级三氧化钼在温度为950-1500 °C高温挥发成气态三氧化钼; 2)挥发出来的气态三氧化钼与还原气体接触直接发生反应,三氧化钼被迅速还原为纳米级超细钼粉。 A method of directly preparing nanoscale industrial grade molybdenum trioxide powder; characterized in that the raw materials used for the technical grade molybdenum trioxide, volatiles in the gaseous state in contact with the reducing gas, the reduction reaction is carried out in a high temperature furnace, to give nanoscale materials, because the resulting aqueous product is required under a hydrogen atmosphere, 100 ° c for drying, to give the pure molybdenum powder, the process comprising the steps of: 1) the technical grade molybdenum trioxide at a temperature of 950 -1500 ° C temperature into gaseous volatile molybdenum trioxide; 2) gaseous volatilized molybdenum trioxide with a reducing gas reaction occurs directly, molybdenum trioxide is rapidly reduced to the nanoscale ultrafine molybdenum powder.
  2. 2.根据权利要求1所述的直接利用工业级三氧化钼制备纳米级钼粉的方法,其特征在于,使用的原料为工业级三氧化钼,利用三氧化钼在高温下蒸汽压较大的特点,使其挥发后与还原气体反应,发生的还原反应为气-气反应,反应速度快。 2. The method of technical grade molybdenum trioxide directly preparing nanoscale molybdenum powder according to claim 1, characterized in that the material used was technical grade molybdenum trioxide, molybdenum trioxide vapor pressure at the use of high temperatures larger characteristics, so that the reducing gas, reduction gas to react and the volatiles - the reaction gas, the reaction speed.
  3. 3.根据权利要求1或2所述的直接利用工业级三氧化钼制备纳米级钼粉的方法,其特征在于,使用的还原气体为纯氢气,或者为氢气与惰性气体的混合气。 3. The method of technical grade molybdenum trioxide directly preparing nanoscale or molybdenum powder according to claim 12, wherein the reducing gas used is pure hydrogen, or a mixed gas of hydrogen and inert gas.
CN 201610293735 2016-05-05 2016-05-05 Method for preparing nano-grade molybdenum powder by directly utilizing industrial-grade molybdenum trioxide CN105710390A (en)

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CN103255288A (en) * 2012-02-17 2013-08-21 苏州艾默特材料技术有限公司 Purification method of industrial molybdenum powder
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