WO2008022495A1 - Procédé de préparation d'une poudre métallique d'ordre de grandeur nanométrique - Google Patents

Procédé de préparation d'une poudre métallique d'ordre de grandeur nanométrique Download PDF

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Publication number
WO2008022495A1
WO2008022495A1 PCT/CN2006/002913 CN2006002913W WO2008022495A1 WO 2008022495 A1 WO2008022495 A1 WO 2008022495A1 CN 2006002913 W CN2006002913 W CN 2006002913W WO 2008022495 A1 WO2008022495 A1 WO 2008022495A1
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Prior art keywords
iron powder
powder
cutting
zero
nano
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PCT/CN2006/002913
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English (en)
Chinese (zh)
Inventor
Huimin Wang
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Huimin Wang
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Publication of WO2008022495A1 publication Critical patent/WO2008022495A1/fr

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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
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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 relates to a metal nano powder processing technology, in particular to a metal nano powder zero-bound particle cutting production process.
  • Nanotechnology is an emerging technology that emerged in the 1990s, studying the science of the properties and laws of matter ranging from 0.1 to 100 nanometers.
  • Nanoparticles refer to ultrafine particles having a particle size of the order of nanometers, and the nanoparticles are generally between 1 and 100 nm.
  • quantum size effects small size effects, surface effects, and macroscopic quantum tunneling effects, thus exhibiting many unique properties in catalysis, light absorption, medicine, magnetic media, and new materials. There are broad application prospects in other areas.
  • the size of the nanoparticles is continuously reduced, under certain conditions, the macroscopic physical and chemical properties of the material will be changed, giving them special mechanical, thermal, optical, magnetic and chemical properties.
  • nano-sized iron powder is widely used in many fields such as machinery, electronics, metallurgy, bioengineering, nuclear industry, chemical, pharmaceutical, textile, military and aerospace.
  • the processing technology of nano-scale iron powder materials in the world mainly includes electrolysis method, water mist method, rapid solidification method, laser method, plasma gas phase reaction method, carbonyl iron thermal decomposition method, chemical liquid phase reduction method and the like.
  • electrolysis method water mist method, rapid solidification method, laser method, plasma gas phase reaction method, carbonyl iron thermal decomposition method, chemical liquid phase reduction method and the like.
  • agglomeration, high temperature, etc. resulting in poor product shape (such as sheet, irregular), uneven particles, poor fluidity, insufficient strength and so on.
  • nano-iron powder is the most difficult to process and scale production.
  • powder agglomeration and particle shape are two of iron powder processing. Difficulties, as shown in Figure 6 and Figure 7, these two difficulties directly determine the quality and performance of nano-scale iron powder.
  • processing production of more than 1 micron is blank, and a few of them have different experimental explorations, but the products are basically irregular sheet-like particles, and their uniformity, fluidity, strength, and specific surface area are not up to The requirements of nanomaterials are required in the world market. .
  • the present invention provides a metal nano-powder zero-boundary particle cutting production process in order to solve the problems of powder agglomeration and irregular particle shape which occur in the preparation of nano-sized metal powder materials existing in the prior art.
  • the invention is realized by the following technical solution, a metal nano powder zero-boundary particle cutting production process, taking iron powder as an example, the steps include: placing the iron powder at -10 ° C ⁇ +10 ° C (preferably - 6 °C) at the zero boundary processing temperature state, then the high-speed cutting of the iron powder particles, controlled at 4000 ⁇ 6000 times per minute, preferably 6000 times/min), and then the iron powder particles after cutting are 4000 ⁇ 6000 rpm ( Preferred 4000 High-frequency grinding of rpm, physical reduction, surface treatment, and product can be obtained, and finally sorted.
  • the iron powder raw material is a reduced iron powder produced directly from iron ore as a raw material for producing zero-boundary particle-cut nano-iron powder.
  • Oxidation rate (%) 92 31 91 95 96. 32 Particle strength (Mohs) 6. 24 8. 11 6. 18 6. 02 7. 01
  • the analysis of the specific data shows that the liquidity is 14 grams higher than that of the foreign products, which fully demonstrates that the iron powder sphere shape of this product is superior to other products; the bulk density is 0. 012 grams less than the foreign products. It indicates that the particle size is much smaller than that of the comparative product, and the tap density and specific surface area indicate that the average particle diameter of the product is smaller than that of the comparative product; the oxidation time is on average 69 hours higher than the comparison product, and the oxidation rate is lower.
  • the particle strength indicates that the quality of the product produced by the present invention is higher than that of the comparative product; the particle distribution indicates that the product obtained by the present invention is relatively concentrated in a certain product segment (D50).
  • the nano-sized iron powder produced by the process of the present invention is 1/8 of the price compared with the HGNS nano-iron powder of NOG Corporation of the United States.
  • the invention adopts the physical method for cutting iron powder in the state of zero boundary to produce nano-scale iron powder, and breaks through the two major problems of processing micro- and nano-scale fine iron powder in the world, and solves the iron powder in the same way.
  • Key issues such as high temperature, agglomeration, uniformity and shape during processing and production have enabled new breakthroughs in strength and fluidity.
  • Under the premise of solving the problem of agglomeration in processing make full use of iron powder in the zero boundary state without temperature, no agglomeration, and use high frequency cutting to high frequency, uniform cutting of iron powder particles, so that it reaches the nanometer level, and then The ball is shaped by high frequency grinding itself and the grinding medium.
  • the high-speed rotating airflow is used to scatter the powder in the container, and the difference in weight is used to achieve the purpose of powder classification.
  • the invention fills a blank of metal nano materials in China and breaks the long-term technological monopoly of Europe and the United States.
  • Application examples: Diamond tools and cemented carbide products are multiphase composites produced by powder metallurgy using iron as the binder phase.
  • the iron powder prepared by the process of the invention has the advantages of spherical shape, high purity, good fluidity, high density, easy sintering and high hardness, and large holding power.
  • the iron powder produced by the process of the invention is far less expensive than the cobalt powder, and the performance of the cobalt-based binder can be achieved by the relevant physical quantity control.
  • this product Compared with Co, Ni and Cu, this product has good wettability, formability, sinterability and large adhesion to diamond. It has suitable mechanical properties such as flexural strength and hardness.
  • the materials W, Wc, TiC;, Cr 3 C 2 have good wettability; the expansion coefficient of iron is lower than that of Co, Ni and Cu, and the volume effect is small during heating and cooling, which reduces the tendency of crack occurrence; It has good compatibility with B and Si, and can eliminate compounds such as Fe 3 C, Fe 3 Si 3 , Fe 3 Si, Fe 2 Si, FeSi, Fe 2 B, Fe 3 (CB), which effectively reduces diamond and viscosity.
  • the internal interfacial tension between the joints improves the adhesion to diamond; iron can reduce the internal interfacial tension of diamond and 6-6-3 bronze, produce chemical bonding, improve the wetting of diamond by 6-6-3 bronze, reduce The amount of copper powder used.
  • the nano-scale fine iron powder produced by the technology of the invention has particularly obvious monomer particles, and the surface is smooth to form a spherical body, and the particles are hooked, the fluidity is excellent, and the strength is extremely high. It has great advantages in specific applications, such as high-speed drill bits made of fine iron powder from Germany and Russia.
  • the clock is 1400 rpm
  • the bit temperature is 1150 ° C
  • the drill made by the fine iron powder produced by this process has a bit temperature of 850 rpm at a speed of 4000 rpm.
  • Figure 2 is a photo of a 1 million-fold electron microscopic irregular sheet polygon of the US "HGNS" 80 nanometer iron powder.
  • Figure 3 is a Japanese 150 nanometer iron powder.
  • Figure 4 is a 100-nanometer 100-million electron microscope dendrimer photo of Germany
  • Figure 5 is a photo of a 1 million-fold electron microscope irregular sphere of South Korea 150 nanometer iron powder
  • Figure 6 shows the agglomeration of nano-iron powder during production and processing.
  • Figure 7 shows the serious agglomeration of nano-iron powder during production and processing.
  • Figure 8 is a photo of a 1 micron iron powder megascope produced by the technique of the present invention
  • Figure 9 is an electron micrograph of (50000 mesh) 50 nm iron powder produced by the present invention.
  • Figure 10 is a 6 micron electron microscope photograph produced by the present invention.
  • Embodiment 1 a metal nano-powder zero-boundary particle cutting production process, taking iron powder as an example, the steps include: placing the iron powder at a zero-temperature processing temperature of 5 ° C, and then performing high-speed on the iron powder particles Cutting, controlled 4,000 times per minute, and then high-frequency grinding of the iron powder particles after cutting is 4000 rpm, and then high-speed reduction, surface treatment. You can get the product. Final classification and sorting. If the iron powder index is not up to standard, secondary cutting and grinding can be performed.
  • the specific steps are as follows: 1. Iron ore mining; 2. Mechanical crushing; 3. Water washing; 4. Magnetic separation; 5. Drying; 6. Grinding 100 mesh; 7. High temperature purification; 8. Primary reduction; 9. Cyclone classification; 10 zero boundary particle cutting; 11 secondary classification; 12 high frequency grinding; 13 purification; 14 coating; 15 high speed reduction; 16 surface treatment; 17 parabolic classification; 18 negative pressure classification; 19 fluid volume; 20 vacuum oxygen; 21 packaging; 22 storage.
  • 1-8 is a raw material obtaining process
  • 9-22 is a whole process for realizing the present invention.
  • the main equipment used in the process is a high frequency cutting machine, a purification furnace, a coating furnace, a nitrogen generator, a cyclone classifier, a polishing machine, a powder surface treatment machine, and the like.
  • the raw material uses the primary reduced iron powder as the raw material for cutting the nano iron powder by the zero boundary particle.
  • the grading is performed once by the cyclone classifier, and the required iron powder is input into the ⁇ frequency cutting machine, and the cutting is performed at a frequency of 6000 times per minute.
  • the zero-edge grinding machine using the iron powder in the zero boundary state and the same point cutting tool to grind the mixture to perform nano-scale cutting, and simultaneously grinding to make the sphere shape, and then perform secondary reduction (reduction)
  • the process is well known to those skilled in the art), so that various physical and chemical indicators meet the requirements of nano iron powder, and at the same time, the iron-containing substance is proposed to increase the purity of the iron powder, and then the iron powder particles.
  • Oxidation-proof coating is carried out to achieve an oxidation prevention time of more than 60 hours, and the oxidation rate is less than 5%, thereby achieving an international level of oxidation prevention index, forming a loose block after the oxidation prevention coating, and then performing the same.
  • High-speed pulverization in a sealed state the particle diameter is up to the micron level, and then input into the B-level zero-boundary cutting and grinding process, so that the iron powder completely reaches the international level particle size, and then loaded into the secondary cyclone classifier unit, By grading different types and different particle diameters, it is possible to obtain more than 30 products of different particle sizes at the same time.
  • the key to the process lies in the zero-frequency high-frequency cutting and grinding, which can reach the nano-scale iron powder and has an excellent shape, followed by hydrogen-oxygen coating. After the coating process, the anti-oxidation time of the iron powder can be increased.
  • the temperature-controlled cooling device in the process uses the forced circulation of water to cool all the steps in the process, so that the energy consumption can be reduced, especially the cooling of the oxygen-proof coating is extremely important. If the cooling temperature control is not accurate, The anti-oxidation time of the nano-iron powder will be seriously affected in the subsequent process.
  • Example 2 The procedure and apparatus were the same as in Example 1.
  • the zero boundary processing temperature was controlled at -6 °C
  • the cutting frequency was controlled at 6000 times/min
  • the high frequency grinding was performed at 4000 rpm.
  • Example 3 The procedure and apparatus were the same as in Example 1.
  • the zero boundary processing temperature was controlled at -10 ° C
  • the cutting frequency was controlled at 5000 times / minute
  • the high frequency was milled at 5000 rpm.
  • Example 4 The procedure and apparatus were the same as in Example 1.
  • the zero boundary processing temperature was controlled at 10 ° C
  • the cutting frequency was controlled at 4000 times per minute
  • the high frequency was milled at 6000 rpm.

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  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)

Abstract

L'invention concerne un procédé de préparation d'une poudre de Fe d'ordre de grandeur nanométrique. Le procédé permet de résoudre les problèmes d'irrégularités d'agrégation et de forme qui se présentent dans la technique connue de préparation d'une poudre métallique d'ordre de grandeur nanométrique. A cet effet, le procédé est caractérisé en ce qu'il comprend les étapes suivantes : soumettre la poudre de Fe à une température de traitement de -10 ∼ +10, couper les particules de Fe à une fréquence élevée de 4000-6000 fois/minute, broyer les particules traitées à vitesse élevée, à savoir de 4000-6000 rotations/minute, puis réduire la poudre de fer et traiter la surface de la poudre de Fe, enfin, exécuter la classification et la sélection. On obtient ainsi une poudre de Fe d'ordre de grandeur nanométrique, sphérique et dispersée et d'une surface lisse.
PCT/CN2006/002913 2006-08-17 2006-10-30 Procédé de préparation d'une poudre métallique d'ordre de grandeur nanométrique WO2008022495A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN200610048168.5 2006-08-17
CNB2006100481685A CN100446900C (zh) 2006-08-17 2006-08-17 金属纳米粉体零界颗粒切割生产工艺

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WO2008022495A1 true WO2008022495A1 (fr) 2008-02-28

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CN113560586A (zh) * 2021-07-27 2021-10-29 上海爱仑倍思环境科技有限公司 一种不规则片状零价铁基纳米材料的制备装置

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CN101157137A (zh) * 2007-10-29 2008-04-09 王惠民 电磁能量转换专用铁粉
CN101157132B (zh) * 2007-10-29 2011-05-11 王惠民 磁变流技术专用金属纳米铁粉
CN101758227B (zh) * 2008-09-30 2011-10-26 王惠民 飞机玻璃座舱内电磁、雷达波屏蔽专用纳米铁粉
CN101758229B (zh) * 2008-09-30 2012-01-11 王惠民 卫星喷射损毁专用纳米铁粉
CN101758223B (zh) * 2008-12-15 2012-05-23 王惠民 金属纳米粉体表面张力和颗粒团聚处理技术
CN101758228B (zh) * 2008-12-15 2012-04-18 王惠民 金属纳米粉体颗粒材料合金制备方法

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JP2004091859A (ja) * 2002-08-30 2004-03-25 Mitsubishi Chemicals Corp 金属微粒子の製造方法
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Publication number Priority date Publication date Assignee Title
CN113560586A (zh) * 2021-07-27 2021-10-29 上海爱仑倍思环境科技有限公司 一种不规则片状零价铁基纳米材料的制备装置

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CN1911567A (zh) 2007-02-14

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