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CN109175384A - A kind of preparation method of flake micron grade iron aluminum silicon powder - Google Patents

A kind of preparation method of flake micron grade iron aluminum silicon powder Download PDF

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Publication number
CN109175384A
CN109175384A CN201810860157.XA CN201810860157A CN109175384A CN 109175384 A CN109175384 A CN 109175384A CN 201810860157 A CN201810860157 A CN 201810860157A CN 109175384 A CN109175384 A CN 109175384A
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China
Prior art keywords
milling
preparation
sendust powder
ball
micron grade
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CN201810860157.XA
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Chinese (zh)
Inventor
盛勇
李晓鹏
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Sichuan University
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Sichuan University
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Priority to CN201810860157.XA priority Critical patent/CN109175384A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/02Ferrous alloys, e.g. steel alloys containing silicon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/06Ferrous alloys, e.g. steel alloys containing aluminium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a kind of preparation methods of flake micron grade sendust powder, there are higher contact surface area and soft magnet performance with sendust powder prepared by this method, can be achieved by following technical proposals: taking ingredient is Al:5wt%-6wt%, Si:8wt%-10wt%, remaining is iron, after coarse crushing, takes partial size in 100 parts of raw material of 20-40 microns, 2-8 parts of calcium stearate, 15-30 parts of ethyl alcohol.Ethyl alcohol is added after above-mentioned raw materials are mixed with calcium stearate, it is put into ball mill, ratio of grinding media to material 100:8-15,10-35 DEG C of ball milling temperature, Ball-milling Time 0.5-2.0 hours, it is dried after taking out crushed material, is added calcium stearate 2-6 parts, is put into rod mill after being sufficiently mixed, bar ratio is 100:1-5,30-45 DEG C of rod milling temperature the rod milling time 1-5 hours, is dried in vacuo after taking out material washing up to flake micron grade sendust powder.

Description

A kind of preparation method of flake micron grade iron aluminum silicon powder
Technical field
The present invention relates to a kind of preparation processes of submicron particle, more specifically, it relates to a kind of flake micron grade The preparation method of iron aluminum silicon powder.
Background technique
Conventional iron sial (FeSiAl) alloy has high magnetic permeability μ and high saturated magnetic induction BSAnd coercivity HC It is low, the features such as Curie temperature is high, it is often used as audio, video head core material.In recent years, as people are to sendust Research gradually deeply, sendust core is used for high frequency power filter, military radar wave invisible coating, uninterruptible power supply (UPS) the high-precision pointed collar domain such as power corrector (PFC).However, traditional sendust is mostly spherical or coarse granule shape, particle it Between contact surface it is actively small, be unable to satisfy that wave absorbtion is strong, inhales that wavestrip is roomy, thickness is small, light-weight contour performance requirement, therefore, lead to Crossing improves its pattern to increase the selection that the stacked condition of three-dimensional plate layer heap is most researchers.In addition, usual flaky material phase To other topology materials have higher high frequency magnetic conductivity and absorbing property, and thickness be less than skin depth when can effectively subtract Small eddy-current loss bring influences, so, obtain laminar sendust powder, especially radius-thickness ratio (average diameter/average thickness Degree) in 5:1 or more, sheet average diameter has important application value in 5 microns of superfine sheet sendust powder below.
It is an object of the invention to provide a kind of preparation methods of flake micron grade iron aluminum silicon powder.Have compared to others The pure metallic nickel or cobalt of preferable ductility, solving sendust with preparation method of the invention has certain brittle technology Obstacle prepares flake micron grade sendust powder by special process, which has biggish radius-thickness ratio, compared with High contact surface area, high resistivity and high-wearing feature and higher comprehensive soft magnet performance, are able to satisfy absorbing material, magnetic is deposited The particular/special requirement of storage etc..
Summary of the invention
The purpose of the present invention is overcome the deficiencies in the prior art, and current material is overcome to have certain brittle technological difficulties, There is provided a kind of has high specific surface area, larger radius-thickness ratio (diameter/thickness), not easy to reunite and industrialized production easy to accomplish Sheet sendust powder preparation process.
The technical scheme is that: taking ingredient is Al:5.0wt%-6.0wt%, Si:8.0wt%- 10.0wt%, remaining is iron, after coarse crushing, takes particle diameter distribution in 100 parts of sendust powder raw material of 20-40 microns, 2-8 parts of calcium stearate, 15-30 parts of ethyl alcohol.The content of the iron sial is preferably Al:5.5wt%-5.8wt%, Si: 8.5wt%-9.5wt%, remaining is iron, and calcium stearate is preferably 4-6 parts, and ethyl alcohol is preferably 20-25 parts.Sendust powder is former Material adds ethyl alcohol after being sufficiently mixed with calcium stearate, is then placed in ball milling in ball mill, and steel ball mass of medium and iron sial close Bronze mass ratio is 100:8-15, and ball milling temperature is controlled at 10-35 DEG C, and Ball-milling Time is described most to can be compared at 0.5-2.0 hours Example are as follows: steel ball mass of medium and sendust powder mass ratio are 100:10-12, and the control of ball milling temperature is at 15-25 DEG C, ball milling Time was at 1.0-1.5 hours.It is dried after taking out ball milling powder particle, adds 2-6 parts of calcium stearate, be put into after being sufficiently mixed by column Column rod mill of the shape high duty metal stick as abrasive medium, billet quality ratio are 100:1-5, and temperature is controlled during rod milling At 30-45 DEG C, the rod milling time, the rod milling medium was preferably 2-4 parts at 1-5 hours, and billet quality ratio is preferably 100:4-5, Temperature is preferably controlled in 35-40 DEG C of range during rod milling, and the rod milling time is preferably controlled in 2-3 hours.Material is taken out, with routine After the remaining calcium stearate of method elution, using after vacuum drying up to flake micron grade sendust powder.
Specific embodiment
The present invention will be further described with reference to the examples below.
Taking ingredient is Al:5.0wt%-6.0wt%, Si:8.0wt%-10.0wt%, remaining is iron, and particle diameter distribution exists 100 parts of 20-40 microns of alloy powder raw material, 2-8 parts of ball-milling medium calcium stearate, 15-30 parts of ethyl alcohol.The content of the iron sial Preferably Al:5.5wt%-5.8wt%, Si:8.5wt%-9.5wt%, remaining is iron, and calcium stearate is preferably 4-6 parts, second Alcohol is preferably 20-25 parts.Ethyl alcohol is added after above-mentioned sendust powder raw material and calcium stearate are sufficiently mixed, is then placed in Ball milling in ball mill, steel ball mass of medium and sendust powder mass ratio are 100:8-15, and ball milling temperature is controlled in 10-35 DEG C, Ball-milling Time was at 0.5-2.0 hours, the best ratio are as follows: steel ball mass of medium is with sendust powder mass ratio 100:10-12, ball milling temperature are controlled at 15-25 DEG C, and Ball-milling Time was at 1.0-1.5 hours.It is dried after taking out ball milling powder particle, then It is added calcium stearate 2-6 parts, the column rod mill by column-shaped high-strength metal bar as abrasive medium, stick are put into after being sufficiently mixed Material mass ratio is 100:1-5, temperature is controlled during rod milling at 30-45 DEG C, the rod milling time at 1-5 hours, the rod milling medium Preferably 2-4 parts, billet quality is than being preferably 100:4-5, and temperature is preferably controlled in 35-40 DEG C of range during rod milling, rod milling Time is preferably controlled in 2-3 hours.Material is taken out, after the remaining calcium stearate of conventional method elution, after vacuum drying Up to flake micron grade sendust powder.
The flake micron grade sendust powder of above method preparation has biggish radius-thickness ratio, higher contact surface Product, high resistivity and high-wearing feature and higher comprehensive soft magnet performance, are able to satisfy the spy of absorbing material, magnetic storage etc. It is different to require.
Specific embodiment:
Embodiment 1:
Taking ingredient is Al:5.4wt%-5.6wt%, Si:9.4wt%-9.6wt%, remaining is iron, and particle diameter distribution is in 20-40 The alloy powder raw material 400g, ball-milling medium calcium stearate 16g, ethyl alcohol 84g of micron, by above-mentioned sendust powder raw material and tristearin Sour calcium adds ethyl alcohol after being sufficiently mixed, and is then placed in ball milling in ball mill, steel ball mass of medium and sendust silty amount The ratio between be 100:10, ball milling temperature control at 15-20 DEG C, Ball-milling Time was at 1.0 hours.It is dried after taking out ball milling powder particle, then 2 parts of calcium stearate are added, the column rod mill by column-shaped high-strength metal bar as abrasive medium, bar are put into after being sufficiently mixed Mass ratio is 100:4, and temperature control is controlled in 35-40 DEG C of range, rod milling time at 2 hours during rod milling.Material is taken out, is used After the remaining calcium stearate of conventional method elution, using, up to flake micron grade sendust powder, being obtained after vacuum drying Sheet sendust powder centralized particle diameter is reunited without obvious, and average piece thickness is less than 1.5 microns.
Embodiment 2:
Taking ingredient is Al:5.4wt%-5.6wt%, Si:9.4wt%-9.6wt%, remaining is iron, and particle diameter distribution is in 20-40 The alloy powder raw material 400g, ball-milling medium calcium stearate 24g, ethyl alcohol 96g of micron, by above-mentioned sendust powder raw material and tristearin Sour calcium adds ethyl alcohol after being sufficiently mixed, and is then placed in ball milling in ball mill, steel ball mass of medium and sendust silty amount The ratio between be 100:12, ball milling temperature control at 15-20 DEG C, Ball-milling Time was at 1.5 hours.It is dried after taking out ball milling powder particle, then 3 parts of calcium stearate are added, the column rod mill by column-shaped high-strength metal bar as abrasive medium, bar are put into after being sufficiently mixed Mass ratio is 100:5, and temperature control is controlled in 35-40 DEG C of range, rod milling time at 3 hours during rod milling.Material is taken out, is used After the remaining calcium stearate of conventional method elution, using, up to flake micron grade sendust powder, being obtained after vacuum drying Sheet sendust powder radius-thickness ratio is big, and sheet average diameter is less than 5 microns, and average piece thickness is less than 1.2 microns.
Embodiment 3:
Taking ingredient is Al:5.4wt%-5.6wt%, Si:9.0wt%-9.2wt%, remaining is iron, and particle diameter distribution is in 20-40 The alloy powder raw material 400g, ball-milling medium calcium stearate 20g, ethyl alcohol 100g of micron, by above-mentioned sendust powder raw material and firmly Resin acid calcium adds ethyl alcohol after being sufficiently mixed, and is then placed in ball milling in ball mill, steel ball mass of medium and sendust silty The ratio between amount is 100:12, and ball milling temperature is controlled at 15-20 DEG C, and Ball-milling Time was at 2.0 hours.It is dried after taking out ball milling powder particle, 4 parts of calcium stearate are added, the column rod mill by column-shaped high-strength metal bar as abrasive medium, stick are put into after being sufficiently mixed Material mass ratio is 100:5, and temperature control is controlled in 35-40 DEG C of range, rod milling time at 3 hours during rod milling.Material is taken out, After the remaining calcium stearate of conventional method elution, using, up to flake micron grade sendust powder, being obtained after vacuum drying Sheet sendust powder radius-thickness ratio it is big, average piece thickness is less than 1 micron.

Claims (11)

1. a kind of preparation method of flake micron grade sendust powder, it is characterised in that preparation method are as follows: with common iron silicon Al alloy powder is raw material, and technique is divided into ball milling and rod milling two parts, uses calcium stearate as abrasive medium, first uses high-energy ball milling Machine carries out ball milling, dries after taking out ball milling powder particle, then carries out rod milling using column type rod mill, and the hard of remnants is eluted after rod milling Resin acid calcium and drying to obtain flake micron grade sendust powder, it is desirable that the ingredient of sendust powder raw material is Al: 5.0wt%-6.0wt%, Si:8.0wt%-10.0wt%, remaining is iron, and particle diameter distribution is in 20-40 micron range, ball milling 2-8 parts of medium calcium stearate, 15-30 parts of ethyl alcohol, the ratio between steel ball mass of medium and sendust powder are 100:8-15, ball milling temperature Degree control is at 10-35 DEG C, and for Ball-milling Time at 0.5-2.0 hours, 2-6 parts of rod milling medium calcium stearate, billet quality ratio was 100: 1-5 controls temperature at 30-45 DEG C during rod milling, the rod milling time at 1-5 hours, elutes remaining stearic acid after taking out material Calcium and drying to obtain flake micron grade sendust powder.
2. the preparation method of flake micron grade sendust powder according to claim 1, it is characterised in that iron sial Content is Al:5.5wt%-5.8wt%, Si:8.5wt%-9.5wt%.
3. the preparation method of flake micron grade sendust powder according to claim 1, it is characterised in that ball-milling medium Calcium stearate is 4-6 parts.
4. the preparation method of flake micron grade sendust powder according to claim 1, it is characterised in that ethyl alcohol 20- 25 parts.
5. the preparation method of flake micron grade sendust powder according to claim 1, it is characterised in that steel ball medium The ratio between quality and sendust powder are 100:10-12.
6. the preparation method of flake micron grade sendust powder according to claim 1, it is characterised in that ball milling temperature Control is at 15-25 DEG C.
7. the preparation method of flake micron grade sendust powder according to claim 1, it is characterised in that Ball-milling Time At 1.0-1.5 hours.
8. the preparation method of flake micron grade sendust powder according to claim 1, it is characterised in that rod milling medium 2-4 parts of calcium stearate.
9. the preparation method of flake micron grade sendust powder according to claim 8, it is characterised in that billet quality Than being preferably 100:4-5.
10. the preparation method of flake micron grade sendust powder according to claim 8, it is characterised in that rod milling process Middle temperature control is in 35-40 DEG C of range.
11. the preparation method of flake micron grade sendust powder according to claim 8, it is characterised in that the rod milling time Control was at 2-3 hours.
CN201810860157.XA 2018-08-01 2018-08-01 A kind of preparation method of flake micron grade iron aluminum silicon powder Pending CN109175384A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110718347A (en) * 2019-10-28 2020-01-21 横店集团东磁股份有限公司 Preparation method of high-permeability scaly iron-silicon-aluminum magnetic powder
CN112207283A (en) * 2020-10-22 2021-01-12 合肥工业大学 Preparation method of flaky ferrosilicon aluminum powder with uniform particle size, micron-sized particles with large diameter-thickness ratio and particle morphology
CN112466647A (en) * 2020-11-26 2021-03-09 成都慧磁电子材料有限公司 Production process of high-permeability Fe-Si-Al soft magnetic alloy flake powder

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WO2013127515A1 (en) * 2012-02-27 2013-09-06 Tata Steel Nederland Technology B.V. Method for manufacturing a steel product
CN103350225A (en) * 2013-06-19 2013-10-16 镇江宝纳电磁新材料有限公司 Method for magnetic metal powder flattening rolling
CN103480852A (en) * 2013-06-19 2014-01-01 镇江宝纳电磁新材料有限公司 Manufacturing method of scaly metal soft magnetic micro powder
CN104008844A (en) * 2014-01-20 2014-08-27 横店集团东磁股份有限公司 Fabrication method of soft magnetic alloy materials
CN107414089A (en) * 2017-07-20 2017-12-01 上海交通大学 A kind of Fe-Si-Al magnetic and preparation method thereof
US20180044765A1 (en) * 2016-08-09 2018-02-15 GM Global Technology Operations LLC Forming high-strength, lightweight alloys

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013127515A1 (en) * 2012-02-27 2013-09-06 Tata Steel Nederland Technology B.V. Method for manufacturing a steel product
CN103350225A (en) * 2013-06-19 2013-10-16 镇江宝纳电磁新材料有限公司 Method for magnetic metal powder flattening rolling
CN103480852A (en) * 2013-06-19 2014-01-01 镇江宝纳电磁新材料有限公司 Manufacturing method of scaly metal soft magnetic micro powder
CN104008844A (en) * 2014-01-20 2014-08-27 横店集团东磁股份有限公司 Fabrication method of soft magnetic alloy materials
US20180044765A1 (en) * 2016-08-09 2018-02-15 GM Global Technology Operations LLC Forming high-strength, lightweight alloys
CN107414089A (en) * 2017-07-20 2017-12-01 上海交通大学 A kind of Fe-Si-Al magnetic and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110718347A (en) * 2019-10-28 2020-01-21 横店集团东磁股份有限公司 Preparation method of high-permeability scaly iron-silicon-aluminum magnetic powder
CN112207283A (en) * 2020-10-22 2021-01-12 合肥工业大学 Preparation method of flaky ferrosilicon aluminum powder with uniform particle size, micron-sized particles with large diameter-thickness ratio and particle morphology
CN112466647A (en) * 2020-11-26 2021-03-09 成都慧磁电子材料有限公司 Production process of high-permeability Fe-Si-Al soft magnetic alloy flake powder

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Application publication date: 20190111