CN103357866B - A kind of carbonyl iron dust high-temperature heat treatment method for metal magnetic powder core - Google Patents

A kind of carbonyl iron dust high-temperature heat treatment method for metal magnetic powder core Download PDF

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CN103357866B
CN103357866B CN201310304759.4A CN201310304759A CN103357866B CN 103357866 B CN103357866 B CN 103357866B CN 201310304759 A CN201310304759 A CN 201310304759A CN 103357866 B CN103357866 B CN 103357866B
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carbonyl iron
iron dust
powder
heat treatment
temperature heat
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CN103357866A (en
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邹海平
李显信
李上奎
王兵
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Jiangxi Yue'an New Materials Co., Ltd.
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JIANGXI YUEAN SUPERFINE METAL Co Ltd
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Abstract

The present invention relates to a kind of carbonyl iron dust high-temperature heat treatment method for metal magnetic powder core, its concrete steps are: select carbon content < 1.0%, oxygen content < 0.8%, particle mean size to be powder based on the carbonyl iron dust of 2-10 μm, basic powder is dried and removes moisture, again Coated with Organic Matter liquid is added in carbonyl iron dust and stir, make it evenly coated, oven dry is sieved, and after 800 DEG C of high-temperature heat treatment, powder can not sinter.The invention solves carbonyl iron dust because of particle tiny, the problem of easy-sintering during high-temperature heat treatment.Adopt the carbonyl iron dust of this method after high-temperature heat treatment not sinter, do not need fragmentation, the impurity contents such as the carbon in powder, oxygen significantly reduce, and substantially increase the magnetic property of powder.

Description

A kind of carbonyl iron dust high-temperature heat treatment method for metal magnetic powder core
Technical field
The present invention relates to the preparation method of high-performance soft magnetic materials, be specifically related to a kind of carbonyl iron dust high-temperature heat treatment method for metal magnetic powder core.
Background technology
Carbonyl iron dust is by Fe (CO) 5the average grain diameter that thermal decomposition is produced is not more than the spherical super fine iron powder with onion layer structure of 10 μm, have that purity is high, particle is tiny and even, good dispersion, the active feature such as large, there is much special physicochemical property, be particularly useful for high quality factor high magnetic permeability low-power consumption soft magnetic materials under high frequency, the Frequency Surface attachment aspect such as (SMD) and electromagnetism interference (EMI) element, has the plurality of advantages such as low cost, stable performance.
The common carbonyl iron dust produced by iron pentacarbonyl pyrolysis is due to more difficult controls of technological parameter such as decomposer temperature fields, the powder produced contains the impurity such as carbon, oxygen and some adsorbed gas, carbon and oxygen content are generally all at 0.5%-1.0%, be difficult to reach the requirement making high-performance metal powder core, so must heat-treat common carbonyl iron dust, reduce the impurity contents such as carbon, oxygen and some adsorbed gas.The content of the impurity such as the carbon in carbonyl iron dust, oxygen directly affects the magnetic property of metal magnetic powder core, and impurity content more high magnetic characteristics is poorer, and the lower magnetic property of impurity content is better.High-temperature heat treatment is carried out to carbonyl iron dust and contributes to reducing the impurity contents such as carbon in powder, oxygen and some adsorbed gas, heat treatment temperature is more high is more conducive to the impurity content reducing powder, but because carbonyl iron dust particle is tiny, generally sintering phenomenon will be produced being greater than heat treatment at the temperature of 480 DEG C, agglomerate adds intractability, and the powder magnetic after pulverization process can far below the powder do not sintered.Therefore, research new technology, solves carbonyl iron dust high-temperature heat treatment Sintering Problem, improves carbonyl iron dust quality, and the research of raising powder magnetic energy has become the emphasis problem in magnetic material development field.
Summary of the invention
For above-mentioned Problems existing, the object of the invention is to overcome an above-mentioned difficult problem, a kind of carbonyl iron dust high-temperature heat treatment method for metal magnetic powder core is provided, its technology path is advanced reliable, and process equipment is simple, and continuity is strong, production cost is low, good product performance, is suitable for suitability for industrialized production.
The technical solution adopted for the present invention to solve the technical problems is: the step for the carbonyl iron dust high-temperature heat treatment method of metal magnetic powder core is: select carbon content < 1.0%, oxygen content < 0.8%, particle mean size to be powder based on the carbonyl iron dust of 2-10 μm, basic powder is dried and removes moisture, again Coated with Organic Matter liquid is added in carbonyl iron dust and stir, make it evenly coated, oven dry is sieved, after 800 DEG C of high-temperature heat treatment, powder can not sinter.
Described Coated with Organic Matter liquid by volume proportioning is organosilicon: ethanol=1:5-35, or described Coated with Organic Matter liquid by volume proportioning be organosilicon: acetone=1:5-35.
Basis powder and Coated with Organic Matter liquid proportioning are: basic powder 100kg, Coated with Organic Matter liquid 5-20L.
The inventive method and the difference of conventional carbonyl iron dust high-temperature heat treatment process are that basic carbonyl iron powder that the present invention selects after drying, organic matter is adopted to carry out coated pretreatment, oven dry is sieved, can not sinter through 800 DEG C of high-temperature heat treatment, and carbon content is down to and is less than 0.03%, oxygen content is down to and is less than 0.2%.Its action principle and advantage are:
During carbonyl iron dust high-temperature heat treatment, because its particle is tiny, powder particle is under the effect of interfacial energy, particle intergranular produces diffusion phenomena, add part iron powder and be reduced a large amount of iron palpus of rear generation, formed between iron palpus and put up a bridge, cause the powder after heat treatment seriously to sinter.
The present invention adopted organic matter to carry out coated pretreatment to carbonyl iron dust before 800 DEG C of high-temperature heat treatment, made carbonyl iron dust and organic matter carry out coated, made powder surface form one deck organic film.Organic film changes into inorganic secluding film in high-temperature heat treatment process, reduce fine grain interfacial energy, intercepted the intergranular diffusion of particle, can effectively suppress part brown iron oxide to be reduced a large amount of iron of rear generation must simultaneously, avoid being formed between the iron powder that is heat-treated putting up a bridge, prevent powder sintered.Carbonyl iron dust, by 800 DEG C of high-temperature heat treatment, can remove the impurity such as the carbon in powder, oxygen and some adsorbed gas in a large number, thus the soft carbonyl iron dust do not sintered, keep the size distribution of original base powder, improve the magnetic property of powder.
Detailed description of the invention
Following instantiation is for the invention will be further described, and its scope non-limiting.
Embodiment 1:
Get the common carbonyl iron dust produced by iron pentacarbonyl pyrolysis, carbon content is 0.9%, oxygen content is 0.7%, particle mean size is 8.5 μm, this powder is placed in the moisture that 60 DEG C of drying in oven, 1 hour removal part contains, take organosilicon: ethanol is the Coated with Organic Matter liquid that is mixed with of 1:15 by volume, the Coated with Organic Matter liquid configured by 100kg carbonyl iron dust: 8L after stirring adds and stirs, carbonyl iron dust and organic matter is made to carry out coated, powder surface is made to form one deck organic film, through 50-150 DEG C of oven dry, sieve, carbonyl iron dust after sieving is carried out 800 DEG C of high-temperature heat treatment, the powder obtained does not sinter, and the carbon content of gained powder is 0.02%, oxygen content is 0.18%, magnetic property is good after testing.
Embodiment 2:
Get the common carbonyl iron dust produced by iron pentacarbonyl pyrolysis, carbon content is 0.9%, oxygen content is 0.7%, particle mean size is 8.5 μm, this powder is placed in the moisture that 60 DEG C of drying in oven, 1 hour removal part contains, take organosilicon: ethanol is the Coated with Organic Matter liquid that is mixed with of 1:15 by volume, the Coated with Organic Matter liquid configured by 100kg carbonyl iron dust: 12L after stirring adds and stirs, carbonyl iron dust and organic matter is made to carry out coated, powder surface is made to form one deck organic film, through 50-150 DEG C of oven dry, sieve, carbonyl iron dust after sieving is carried out 800 DEG C of high-temperature heat treatment, the powder obtained does not sinter, and the carbon content of gained powder is 0.025%, oxygen content is 0.16%, magnetic property is good after testing.
Embodiment 3:
Get the common carbonyl iron dust produced by iron pentacarbonyl pyrolysis, carbon content is 0.8%, oxygen content is 0.65%, particle mean size is 9.3 μm, this powder is placed in the moisture that 60 DEG C of drying in oven, 1 hour removal part contains, take organosilicon: acetone is the Coated with Organic Matter liquid that is mixed with of 1:10 by volume, the Coated with Organic Matter liquid configured by 100kg carbonyl iron dust: 10L after stirring adds and stirs, carbonyl iron dust and organic matter is made to carry out coated, powder surface is made to form one deck organic film, through 50-150 DEG C of oven dry, sieve, carbonyl iron dust after sieving is carried out 800 DEG C of high-temperature heat treatment, the powder obtained does not sinter, and the carbon content of gained powder is 0.023%, oxygen content is 0.17%, magnetic property is good after testing.
Embodiment 4:
Get the common carbonyl iron dust produced by iron pentacarbonyl pyrolysis, carbon content is 0.8%, oxygen content is 0.65%, particle mean size is 9.3 μm, this powder is placed in the moisture that 60 DEG C of drying in oven, 1 hour removal part contains, take organosilicon: acetone is the Coated with Organic Matter liquid that is mixed with of 1:10 by volume, the Coated with Organic Matter liquid configured by 100kg carbonyl iron dust: 15L after stirring adds and stirs, carbonyl iron dust and organic matter is made to carry out coated, powder surface is made to form one deck organic film, through 50-150 DEG C of oven dry, sieve, carbonyl iron dust after sieving is carried out 800 DEG C of high-temperature heat treatment, the powder obtained does not sinter, and the carbon content of gained powder is 0.026%, oxygen content is 0.13%, magnetic property is good after testing.
More than show and describe general principle of the present invention and principal character and advantage of the present invention.The technology of the industry should be understood; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and description just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.

Claims (4)

1. the carbonyl iron dust high-temperature heat treatment method for metal magnetic powder core, it is characterized in that: the step of described method is: select carbon content 0.8-0.9%, oxygen content 0.65-0.7%, particle mean size to be powder based on the carbonyl iron dust of 8.5-9.3 μm, basic powder is dried and removes moisture, again Coated with Organic Matter liquid is added in carbonyl iron dust and stir, make it evenly coated, oven dry is sieved, and after 800 DEG C of high-temperature heat treatment, powder can not sinter.
2. a kind of carbonyl iron dust high-temperature heat treatment method for metal magnetic powder core according to claim 1, is characterized in that: described Coated with Organic Matter liquid by volume proportioning is organosilicon: ethanol=1:5-35.
3. a kind of carbonyl iron dust high-temperature heat treatment method for metal magnetic powder core according to claim 1, is characterized in that: described Coated with Organic Matter liquid by volume proportioning is organosilicon: acetone=1:5-35.
4. a kind of carbonyl iron dust high-temperature heat treatment method for metal magnetic powder core according to claim 1, is characterized in that: basic powder and Coated with Organic Matter liquid proportioning are: basic powder 100kg, Coated with Organic Matter liquid 5-20L.
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CN103600069A (en) * 2013-12-02 2014-02-26 北矿磁材科技股份有限公司 Magnetic flaky metal powder surface treating method
CN104668554B (en) * 2015-02-07 2017-03-22 兰州大学 Graphene coating method for metal powder material

Citations (3)

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SU932572A1 (en) * 1980-05-20 1982-05-30 Ленинградский Ордена Октябрьской Революции И Ордена Трудового Красного Знамени Технологический Институт Им.Ленсовета Method of manufacturing magnetodielectric cores on the base of carbonyl iron
CN101091990A (en) * 2007-07-13 2007-12-26 李上奎 Method for preparing superfine carbonyl iron powder in use for high performance magnetic powder core
CN101127269A (en) * 2007-07-13 2008-02-20 李上奎 Preparation method of high performance metal magnetic powder core for high frequency nonpolar lamp circuit

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Publication number Priority date Publication date Assignee Title
JPS5638402A (en) * 1979-09-05 1981-04-13 Tdk Corp High density sintered magnetic body and its manufacture
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Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU932572A1 (en) * 1980-05-20 1982-05-30 Ленинградский Ордена Октябрьской Революции И Ордена Трудового Красного Знамени Технологический Институт Им.Ленсовета Method of manufacturing magnetodielectric cores on the base of carbonyl iron
CN101091990A (en) * 2007-07-13 2007-12-26 李上奎 Method for preparing superfine carbonyl iron powder in use for high performance magnetic powder core
CN101127269A (en) * 2007-07-13 2008-02-20 李上奎 Preparation method of high performance metal magnetic powder core for high frequency nonpolar lamp circuit

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Address after: 341000 Dayu new century industrial city, Dayu County, Jiangxi, Ganzhou

Patentee after: Jiangxi Yue'an New Materials Co., Ltd.

Address before: 341500 Ganzhou province Dayu County, Xinhua Industrial Park, Jiangxi

Patentee before: Jiangxi Yuean Superfine Metal Co., Ltd.