CN1217760C - Method for preparing silicon-iron coating type composite powder - Google Patents

Method for preparing silicon-iron coating type composite powder Download PDF

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Publication number
CN1217760C
CN1217760C CN 03118558 CN03118558A CN1217760C CN 1217760 C CN1217760 C CN 1217760C CN 03118558 CN03118558 CN 03118558 CN 03118558 A CN03118558 A CN 03118558A CN 1217760 C CN1217760 C CN 1217760C
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powder
type composite
composite powder
ball milling
silicon
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CN1433860A (en
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张联盟
张东明
沈强
员文杰
李淘
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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Abstract

The present invention relates to a preparation method of cladding type composite powder, which is characterized in that the preparation method of the silicon-iron uniform cladding type composite powder is carried out according to the following steps: (1) high-energy size reduction equipment is used to pulverize micro-size Si powder nanometer size into Si powder; (2) mixed ball milling is carried out to the nanometer size Si powder of which the weight percentage is from 6 to 7 and micro-size Fe powder of which the weight percentage is from 93 to 94, the ratio of grinding media to material is 4: 1, ball milling is carried out for 1 to 2 hours, and accordingly, Si is uniformly distributed on the surfaces of Fe particles, and the silicon-iron uniform cladding type composite powder is obtained. The present invention uses the surface activity of iron powder and nanometer silicon powder, and the composite powder of nanometer silicon, which is uniformity coated on the surfaces of sphere iron particles, is obtained through the ball milling processing of certain conditions. The cladding type composite powder keeps the original plastic deformation capability of alpha-Fe, and provides an acceptable material for the subsequent preparation of a high-silicon stalloy.

Description

The preparation method of the even cladded type composite powder of silicon-iron
Technical field
The present invention relates to a kind of preparation method of cladded type composite powder.
Background technology
The extraordinary silicon steel sheet of siliceous 6.5wt% is the magnetically soft alloy of a class excellent performance, compare with traditional silicon steel disc (containing 3wt%Si), it has more excellent soft magnet performance and high frequency characteristicses such as high magnetic permeability, high saturated magnetic induction, low magnetostriction and low iron loss, therefore be more suitable for being applied to generator, transformer and various motor, electrical equipment etc., its low iron loss and approach zero magnetostriction coefficient particularly, to reduce noise of transformer and realize the subminaturization of motor, electrical equipment and large, minimizing energy consumption all very favourable.But with the increase of Si content, the quality of silicon steel sheet becomes fragile, and its processing characteristics is very poor, is difficult to use the conventional method roll forming, has seriously restricted the production and the application of 6.5wt%Si steel disc.For this reason, produced the preparation method of some new 6.5wt%Si steel discs in recent years successively, as the continuous siliconising of CVD, rapid quenching technique etc.Wherein, the maturation the most of CVD technological development, the Steel tube Co., Ltd (NKK) of Japan has successfully used this technology to realize small-scale suitability for industrialized production.But, at present in the world only one family of NKK company utilize the continuous siliconising explained hereafter of CVD 6.5wt%Si steel disc, scale and output all can't satisfy the needs in international soft magnetism market, and band is still very crisp, it cuts out the laser cutting parameter of still needing, and adds this preparation process complexity, energy consumption, cost height, operating environment abominable (having high temperature chlorine to produce), can not satisfy " input-output ratio " is the requirement and the environmental protection demand of economic benefit.It is wide that rapid quenching technique can obtain 100~200mm, the thick strip of 100~400 μ m.But because the width and the thickness of product are all very limited, form accuracy is difficult to control, so large-scale industrialization production is relatively more difficult, does not form economies of scale.
The researcher is forming silicon steel fragility on the research basis of mechanism, proposes to utilize powder metallurgy process to prepare high-silicon silicon steel sheet, solves the new approaches of the fragility problem in its process.Specifically, promptly at first prepare the Si-Fe cladded type composite powder with plastic deformation ability, be rolled, the final high temperature DIFFUSION TREATMENT is evenly distributed on Si in the matrix.Therefore one of key problem of research work is the Si-Fe composite powder that preparation has clad structure.
Data shows: the preparation method of cladded type composite powder mainly contains: chemical coprecipitation, electroless plating method, fluidized-bed method etc.Chemical coprecipitation and electroless plating method technology more complicated need suitable chemical reaction, and need to handle residual liquid, are not suitable for the preparation of Si-Fe composite powder, fluidized-bed method equipment complexity, and preparation cost is too high, is not suitable for large batch of suitability for industrialized production.
Summary of the invention
The purpose of this invention is to provide a kind of more easy method, prepare the even cladded type composite powder of the Si-Fe with plastic deformation ability in enormous quantities.
The technical solution adopted for the present invention to solve the technical problems is: the preparation method of the even cladded type composite powder of silicon-iron, it is characterized in that being undertaken by following step: (1) carries out high-energy ball milling with the Si powder of the purity 99.99% of 1 μ m, ratio of grinding media to material 10~20: 1, ball milling 30~40 hours, obtain the powder of particle diameter 80~150nm, make it have high activity; (2) be that 6~7 80~150nmSi powder and percentage by weight are that ball-type α-Fe powder of 90~110um of 93~94 carries out mixing and ball milling with percentage by weight, ratio of grinding media to material 4: 1, ball milling 1~2 hour, thus Si is uniformly distributed in the Fe particle surface, obtains the even cladded type composite powder of Si-Fe.
The ball-type α that described 80~150nmSi grain weight amount percentage is 6.5,90~110um-Fe grain weight amount percentage is 93.5.
Because Si is the fragility phase, Fe is the plasticity phase, and is indeformable in mechanical milling process in order to guarantee the Fe powder, must be controlled mechanical milling process, thereby the rolling deformation condition that provides subsequently can be provided the prepared Si-Fe cladded type composite powder that goes out.
The present invention utilizes the surface-active of iron powder and nano silica fume, by the ball-milling treatment of certain condition, obtains the composite powder that nano-silicon evenly is coated on ball-type iron particle surface.This cladded type composite powder has kept the original plastic deformation ability of α-Fe, provides acceptable material for preparing high-silicon silicon steel sheet subsequently.Characteristics of the present invention are: technology is simple, and Si is evenly distributed, and is easy to prepare in enormous quantities.
Description of drawings
Fig. 1 is a process chart of the present invention
Fig. 2 is electron probing analysis of the present invention figure as a result, shows that Si is evenly distributed on around the undeformed Fe particle, forms clad structure.
The specific embodiment
As shown in Figure 1, the preparation method of the even cladded type composite powder of silicon-iron, undertaken by following step: (1) utilizes the high energy disintegrating apparatus that micron order Si powder is ground into nanoscale Si powder; (2) be that 6~7 nanoscale Si powder and percentage by weight are that 93~94 micron order Fe powder carries out mixing and ball milling with percentage by weight, ratio of grinding media to material 4: 1, ball milling 1~2 hour, thus Si is uniformly distributed in the Fe particle surface, obtains the even cladded type composite powder of Si-Fe.Ball-type α-Fe powder that described micron order Fe powder is 90~110um.
Describedly utilize concrete steps that the high energy disintegrating apparatus is ground into micron order Si powder in nanoscale Si powder to carry out high-energy ball milling for the Si powder with the purity 99.99% of 1 μ m, ball milling 30~40 hours obtains the powder of particle diameter 80~150nm.
Embodiment 1:
Be that 99.99% Si powder mixes with an amount of absolute ethyl alcohol with the purity of average grain diameter 1 μ m, place the high energy ball mill of stainless steel, ball milling 30 hours; Ratio of grinding media to material 10: 1, drum's speed of rotation are 350 rev/mins; Feed argon shield in the closed ball milling jar, to prevent the oxidation in the mechanical milling process;
The iron powders of getting silica flour 6 grams and 94 grams of average grain diameter 100 μ m after the pulverizing carry out mixing and ball milling, ratio of grinding media to material 4: 1, and 350 rev/mins of drum'ss speed of rotation, ball milling 1 hour, the powder behind the ball milling is made sample.
Embodiment 2:
To be 99.99% Si powder mix with absolute ethyl alcohol in right amount the purity of 10 gram average grain diameters 1 μ m, places the high energy ball mill of stainless steel, ball milling 40 hours.Ratio of grinding media to material 20: 1, drum's speed of rotation are 350 rev/mins.Feed argon shield in the closed ball milling jar, to prevent the oxidation in the mechanical milling process.
The iron powders of getting silica flour 6.5 grams and 93.5 grams of average grain diameter 100 μ m after the pulverizing carry out mixing and ball milling, ratio of grinding media to material 4: 1,350 rev/mins of drum'ss speed of rotation, ball milling 2 hours.Powder behind the ball milling is made sample, utilizes electron probe analysis, and the result as shown in Figure 2.The result shows that Si evenly is coated on around the Fe, and the Fe particle does not deform.Prove that thus the powder that is obtained is the spherical composite powder of the even cladded type of Si-Fe.
Embodiment 3:
Be that 99.99% Si powder mixes with an amount of absolute ethyl alcohol with the purity of average grain diameter 1 μ m, place the high energy ball mill of stainless steel, ball milling 35 hours; Ratio of grinding media to material 15: 1, drum's speed of rotation are 350 rev/mins; Feed argon shield in the closed ball milling jar, to prevent the oxidation in the mechanical milling process;
The iron powders of getting silica flour 7 grams and 93 grams of average grain diameter 100 μ m after the pulverizing carry out mixing and ball milling, ratio of grinding media to material 4: 1, and 350 rev/mins of drum'ss speed of rotation, ball milling 1.5 hours, the powder behind the ball milling is made sample.

Claims (2)

1. the preparation method of the even cladded type composite powder of silicon-iron, it is characterized in that being undertaken by following step: (1) carries out high-energy ball milling with the Si powder of the purity 99.99% of 1 μ m, ratio of grinding media to material 10~20: 1, ball milling 30~40 hours obtains the powder of particle diameter 80~150nm; (2) be that 6~7 80~150nmSi powder and percentage by weight are that ball-type α-Fe powder of 90~110um of 93~94 carries out mixing and ball milling with percentage by weight, ratio of grinding media to material 4: 1, ball milling 1~2 hour, thus Si is uniformly distributed in the Fe particle surface, obtains the even cladded type composite powder of Si-Fe.
2. the preparation method of the even cladded type composite powder of silicon-iron according to claim 1 is characterized in that described 80~150nmSi grain weight amount percentage is that the ball-type α of 6.5,90~110um-Fe grain weight amount percentage is 93.5.
CN 03118558 2003-01-28 2003-01-28 Method for preparing silicon-iron coating type composite powder Expired - Fee Related CN1217760C (en)

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CN1217760C true CN1217760C (en) 2005-09-07

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Publication number Priority date Publication date Assignee Title
CN100424505C (en) * 2005-12-21 2008-10-08 宋京伟 Vortex detecting method of plastic product crack
CN100409979C (en) * 2006-05-19 2008-08-13 江苏天一超细金属粉末有限公司 Production of nano-SiO2 for coating carbonyl iron powder
CN102059343B (en) * 2009-11-18 2013-06-05 王志平 Manufacturing method for nano-fabric NiCr-Cr3C2 compound granulation powder used for hot spraying
CN108796587B (en) * 2017-05-02 2020-12-29 贵州理工学院 Method and device for continuously preparing high-silicon steel thin strip
CN110355372B (en) * 2019-07-18 2020-07-31 北京科技大学 Method for preparing high-silicon steel sheet by powder rolling
CN111168078A (en) * 2020-03-06 2020-05-19 无锡市东杨新材料股份有限公司 Preparation method of iron-coated silicon core-shell composite powder

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