CN102343438A - Method for preparing hard alloy mixture by attritor milling process - Google Patents

Method for preparing hard alloy mixture by attritor milling process Download PDF

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Publication number
CN102343438A
CN102343438A CN2010102469754A CN201010246975A CN102343438A CN 102343438 A CN102343438 A CN 102343438A CN 2010102469754 A CN2010102469754 A CN 2010102469754A CN 201010246975 A CN201010246975 A CN 201010246975A CN 102343438 A CN102343438 A CN 102343438A
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China
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ball
milling
alloy mixture
mill
mixture
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CN2010102469754A
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Chinese (zh)
Inventor
张敬利
张平
陈冬华
吴立志
熊成渝
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Zhejiang Dongwu Industrial Co Ltd
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Zhejiang Dongwu Industrial Co Ltd
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Priority to CN2010102469754A priority Critical patent/CN102343438A/en
Publication of CN102343438A publication Critical patent/CN102343438A/en
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Abstract

The invention relates to a method for preparing a hard alloy mixture, in particular to a method for preparing a hard alloy mixture by an attritor milling process. |By adopting attritor milling and adding a certain amount of dispersing agent, adhesive and the like, a superfine hard alloy mixture is obtained. The method for preparing the hard alloy mixture by the attritor milling process has the characteristics of high milling efficiency, low energy consumption, suitability for mass production and the like, and can be widely applied to preparation of the superfine hard alloy mixture.

Description

A kind of method of utilizing stirring ball-milling technology to produce carbide alloy mixture
Technical field
The present invention relates to a kind of preparation method of carbide alloy mixture, specifically provide a kind of method of utilizing stirring ball-milling technology to produce carbide alloy mixture.
Background technology
Carbide alloy changes industries such as spy, mining, machining, space flight and aviation owing to it characteristic that possesses high strength, high rigidity is widely used in oil.One of key technology of making carbide alloy is the preparation of carbide alloy mixture.The traditional mixing preparation method for material is to select the satisfactory tungsten carbide powder of granularity and cobalt powder (normally adopt tungsten carbide original grain degree and sintering after the identical principle of alloy grain degree) to dispose compound; Adopt rolling ball milling; Ball milling is for up to just making the satisfactory compound of granularity and decentralization more than 96 hours; This preparation method length consuming time, cost are high, grinding efficiency is low, and require very high to raw material granularity.
Summary of the invention
The present invention be directed to above deficiency, a kind of method of utilizing stirring ball-milling technology to produce carbide alloy mixture is provided, it is through adopting stirring ball-milling, and the dispersant, binding agent etc. that add some obtain the ultra-fine cemented carbide compound.
The technical scheme that the present invention adopted is following:
A kind of method of utilizing stirring ball-milling technology to produce carbide alloy mixture; The tungsten carbide powder of choice of powder grain graininess >=2.0um and the mixture of cobalt powder are raw material; Use alcohol as ball-milling medium; Polyethylene glycol is as binding agent; And in ball-milling medium, dose stearic acid as dispersant; Carry out ball milling through agitating ball mill; The ball milling parameter of said agitating ball mill is: rotational speed of ball-mill 100-120rpm; Activity coefficient is 0.5; Solid-liquid volume ratio 1: 1, mill ball diameter are 6.0mm ± 0.2mm, ratio of grinding media to material (4-5): 1.
The polyethylene glycol proportion is 2wt%.
The stearic acid addition is 50mg/200Kg.
A kind of method of utilizing stirring ball-milling technology to produce carbide alloy mixture of the present invention; It adopts stirring ball-milling technology to produce the ultra-fine cemented carbide compound; The technical scheme of this method is that the mixture with the tungsten carbide powder of particle >=2.0um and cobalt powder is a raw material; Use agitating ball mill to carry out ball milling; Alcohol is ball-milling medium; Polyethylene glycol is a binding agent; And in abrasive media, dose an amount of stearic acid as dispersant, obtain the carbide alloy mixture of ultra-fine grain within a short period of time (8-12 hour).
Milling parameters is: rotational speed of ball-mill 100-120rpm, activity coefficient are 0.5, solid-to-liquid ratio (volume ratio) 1: 1, mill ball diameter are 6.0mm ± 0.2mm, ratio of grinding media to material (4-5): 1; The 2wt% polyethylene glycol; Stearic acid dosage 50mg/200Kg.
A kind of method of utilizing stirring ball-milling technology to produce carbide alloy mixture of the present invention, its carbide alloy mixture particle size of producing is less, be evenly distributed, be difficult for reuniting, and granularity can reach 0.6um--0.8um.Compare with the traditional preparation process method, reaching under the same particle sizes level, this method weak point consuming time, cost is low, efficient is high, is evenly distributed, and requires low to the raw material original particle size.The ball milling time is the stirring ball-milling technology of 8~12h, and the performance of prepared ultra-fine cemented carbide compound has reached that long-time (mixture performance of 80~96h) ball millings, grinding efficiency have improved 8~10 times with traditional tilting-type ball mill.A kind of method of utilizing stirring ball-milling technology to produce carbide alloy mixture of the present invention has characteristics such as grinding efficiency height, energy consumption is low, production in enormous quantities is easy, can be widely used in the preparation of ultra-fine cemented carbide compound.
A kind of method of utilizing stirring ball-milling technology to produce carbide alloy mixture of the present invention; The agitating ball mill of its use is owing to be active, the lasting application of force; Bigger than rotary mill to the active force of material; Grinding effect is at least more than high ten times; Therefore; Not only can play good immixture, mill ball can directly arrive very thin granularity with the material crushing grinding.Mechanical milling process is a dynamical system, and the surface of the ultra-fine grain that is broken can be very high, and secondary agglomeration very easily takes place, and reduces grinding efficiency, influences mixture quality.In order to guarantee to obtain ultra-fine compound, adopt in slip, to add an amount of stearic acid as dispersant, the little Molecular Adsorption of stearic acid makes particle surface have identical electric charge at powder particle surface, repels each other, and reaches the effect of dispersion.Polyethylene glycol directly adds in mechanical milling process as the binding agent of carbide alloy mixture, helps improving compound viscosity, and very even, prevents that binding agent from producing component segregation, finally obtain institutional framework evenly, the carbide alloy of function admirable.
Compared with prior art, a kind of method of utilizing stirring ball-milling technology to produce carbide alloy mixture of the present invention has following outstanding advantage:
1, adopt agitating ball mill, improve the grinding effect to powder greatly, the ball milling time significantly shortens;
2, raw material granularity is required to reduce; (traditional rolling ball milling technological requirement raw material must be very thin ,≤0.6um);
3, mixture particle is even behind the ball milling, and viscosity is good, is easy to compression moulding.
The specific embodiment
Below in conjunction with specific embodiment a kind of method of utilizing stirring ball-milling technology to produce carbide alloy mixture of the present invention is done further to describe.
Embodiment 1:
(the Fei Shi particle mean size of tungsten carbide is 2.0 μ m, and the Fei Shi particle mean size of cobalt powder is 1.0 μ m according to 93.6wt%WC+6wt%Co+0.3wt%Cr3C2+0.1wt%VC configuration raw material.); The alcohol that adds 650ml/Kg is as abrasive media; And the stearic acid that in the compound slip, adds 50ml/200Kg is as dispersant, and 2wt% polyethylene glycol (molecular weight is 300 and 4000, and wherein the same 4000 molecular weight ratios of 300 molecular weight are 1: 7) is as binding agent.Above-mentioned material carries out ball milling in SC-50 type agitating ball mill, the speed setting of the mixing arm of ball mill is 100 rev/mins, and activity coefficient is 0.5, solid-to-liquid ratio (volume ratio) 1: 1, and the mill ball diameter is 6.0mm ± 0.2mm, ratio of grinding media to material (4-5): 1; Behind the ball milling 8 hours, detection mixture particle granularity is: 0.8 μ m.
Embodiment 2:
(the Fei Shi particle mean size of tungsten carbide is 2.0 μ m, and the Fei Shi particle mean size of cobalt powder is 1.0 μ m according to 93.6wt%WC+6wt%Co+0.3wt%Cr3C2+0.1wt%VC configuration raw material.); The alcohol that adds 650ml/Kg is as abrasive media; And the stearic acid that in the compound slip, adds 50ml/200Kg is as dispersant, and 2wt% polyethylene glycol (molecular weight is 300 and 4000, and wherein the same 4000 molecular weight ratios of 300 molecular weight are 1: 7) is as binding agent.Above-mentioned material carries out ball milling in SC-50 type agitating ball mill, the speed setting of the mixing arm of ball mill is 120 rev/mins, and activity coefficient is 0.5, solid-to-liquid ratio (volume ratio) 1: 1, and the mill ball diameter is 6.0mm ± 0.2mm, ratio of grinding media to material (4-5): 1; Behind the ball milling 8 hours, detection mixture particle granularity is: 0.6 μ m.
A kind of method of utilizing stirring ball-milling technology to produce carbide alloy mixture of the present invention; In its raw material layoutprocedure; It is definite value that the gross weight of tungsten carbide powder and cobalt powder accounts for the mixture total weight ratio; Cobalt powder is usually between the 6%-10% of mixture total weight; Therefore; Tungsten carbide powder also changes thereupon, and the weight of Cr3C2 and VC does not change.Such as, the total part by weight of mixture is 100%, this constant rate of 0.3wt%Cr3C2+0.1wt%VC wherein, and when CO was 6%, WC was: 93.6wt%; When CO was 8%, WC was: 91.6wt%; When CO was 10%, WC was: 89.6wt%.
Activity coefficient is 0.5 to be meant: like the ball mill volume is V, can only load 50% compound, and promptly 50%V is referred to as activity coefficient.
The solid-liquid volume ratio refers to the mixture of tungsten carbide powder and cobalt powder and the ratio between the alcohol.
Will adorn alloying pellet earlier in the ball mill, it plays the effect of levigate material.Ratio of grinding media to material just is meant the ratio of the weight of alloying pellet weight of being packed into and the compound of being packed in the ball mill.
Above-described embodiment, the present invention specific embodiment a kind of more preferably just, common variation that those skilled in the art carries out in technical scheme scope of the present invention and replacement all should be included in protection scope of the present invention.

Claims (3)

1. method of utilizing stirring ball-milling technology to produce carbide alloy mixture; It is characterized in that; The tungsten carbide powder of choice of powder grain graininess >=2.0um and the mixture of cobalt powder are raw material; Use alcohol as ball-milling medium; Polyethylene glycol is as binding agent; And in ball-milling medium, dose stearic acid as dispersant; Carry out ball milling through agitating ball mill; The ball milling parameter of said agitating ball mill is: rotational speed of ball-mill 100-120rpm; Activity coefficient is 0.5; Solid-liquid volume ratio 1: 1, mill ball diameter are 6.0mm ± 0.2mm, ratio of grinding media to material 4-5: 1.
2. a kind of method of utilizing stirring ball-milling technology to produce carbide alloy mixture according to claim 1 is characterized in that said polyethylene glycol proportion is 2wt%.
3. a kind of method of utilizing stirring ball-milling technology to produce carbide alloy mixture according to claim 1 is characterized in that said stearic acid addition is 50mg/200Kg.
CN2010102469754A 2010-08-06 2010-08-06 Method for preparing hard alloy mixture by attritor milling process Pending CN102343438A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103540781A (en) * 2013-05-14 2014-01-29 自贡金盾硬质合金有限公司 Method for producing ultra-coarse grain cemented carbide through utilizing high energy stirring and ball-milling technology
EP3078437A1 (en) * 2015-04-09 2016-10-12 Eckart GmbH Method for the preparation of plastically reformed metal particles
CN109019603A (en) * 2018-07-25 2018-12-18 株洲硬质合金集团有限公司 A kind of preparation method of tungsten-carbide powder
CN109055796A (en) * 2018-08-30 2018-12-21 浙江德威硬质合金制造有限公司 Low temperature synthesis WC is the method that raw material produce hard alloy

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20030085746A (en) * 2002-05-01 2003-11-07 한국과학기술연구원 FABRICATION METHOD OF NANOCRYSTALLINE TiN/Ti-M COMPOSITE POWDER VIA REACTION MILLING
CN1804067A (en) * 2006-01-17 2006-07-19 武汉理工大学 Preparation process of tungsten carbide/inhibitor composite powder and superfine hard alloy thereof
CN101444846A (en) * 2008-11-21 2009-06-03 长沙有色冶金设计研究院 Preparation method of hard alloy mixture
CN101462163A (en) * 2009-01-16 2009-06-24 江西稀有稀土金属钨业集团有限公司 Ball mill technique for preparing carbide alloy mixture
CN101514405A (en) * 2009-03-09 2009-08-26 江西稀有稀土金属钨业集团有限公司 Preparation method for cemented carbide mixture
CN101624673A (en) * 2009-08-14 2010-01-13 北京工业大学 Industrialized preparation method of WC-Co hard alloy with low cost and high performance
CN101695754A (en) * 2009-10-27 2010-04-21 长沙有色冶金设计研究院 Method for preparing mixture for use in production of submicrometer hard alloy

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20030085746A (en) * 2002-05-01 2003-11-07 한국과학기술연구원 FABRICATION METHOD OF NANOCRYSTALLINE TiN/Ti-M COMPOSITE POWDER VIA REACTION MILLING
CN1804067A (en) * 2006-01-17 2006-07-19 武汉理工大学 Preparation process of tungsten carbide/inhibitor composite powder and superfine hard alloy thereof
CN101444846A (en) * 2008-11-21 2009-06-03 长沙有色冶金设计研究院 Preparation method of hard alloy mixture
CN101462163A (en) * 2009-01-16 2009-06-24 江西稀有稀土金属钨业集团有限公司 Ball mill technique for preparing carbide alloy mixture
CN101514405A (en) * 2009-03-09 2009-08-26 江西稀有稀土金属钨业集团有限公司 Preparation method for cemented carbide mixture
CN101624673A (en) * 2009-08-14 2010-01-13 北京工业大学 Industrialized preparation method of WC-Co hard alloy with low cost and high performance
CN101695754A (en) * 2009-10-27 2010-04-21 长沙有色冶金设计研究院 Method for preparing mixture for use in production of submicrometer hard alloy

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103540781A (en) * 2013-05-14 2014-01-29 自贡金盾硬质合金有限公司 Method for producing ultra-coarse grain cemented carbide through utilizing high energy stirring and ball-milling technology
EP3078437A1 (en) * 2015-04-09 2016-10-12 Eckart GmbH Method for the preparation of plastically reformed metal particles
CN109019603A (en) * 2018-07-25 2018-12-18 株洲硬质合金集团有限公司 A kind of preparation method of tungsten-carbide powder
CN109019603B (en) * 2018-07-25 2022-08-30 株洲硬质合金集团有限公司 Preparation method of tungsten carbide powder
CN109055796A (en) * 2018-08-30 2018-12-21 浙江德威硬质合金制造有限公司 Low temperature synthesis WC is the method that raw material produce hard alloy

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Application publication date: 20120208