CN113059183A - Preparation method of carbonyl iron powder special for iron powder core - Google Patents
Preparation method of carbonyl iron powder special for iron powder core Download PDFInfo
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- CN113059183A CN113059183A CN202010001653.7A CN202010001653A CN113059183A CN 113059183 A CN113059183 A CN 113059183A CN 202010001653 A CN202010001653 A CN 202010001653A CN 113059183 A CN113059183 A CN 113059183A
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- iron powder
- carbonyl iron
- carbonyl
- decomposing furnace
- steam
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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
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
- B22F9/305—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis of metal carbonyls
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
Abstract
The invention relates to a preparation method of carbonyl iron powder special for an iron powder core, which controls the internal structure of the obtained carbonyl iron powder to be more compact by controlling the decomposition parameters of carbonyl iron, and removes large particles in the powder by a physical means, thereby effectively improving direct current bias when the carbonyl iron powder is applied to the iron powder core. Meanwhile, the obtained carbonyl iron powder is subjected to micro-oxidation treatment, and when the carbonyl iron powder is applied to an iron powder core, the magnetic core loss of the carbonyl iron powder is reduced.
Description
Technical Field
The invention relates to the field of magnetic material preparation, in particular to a preparation method of carbonyl iron powder special for an iron powder core.
Background
In the field of soft magnetic materials, carbonyl iron powder occupies a certain share, is mainly applied to iron powder cores and chip inductors, is widely applied to the iron powder cores as one of key materials, has initial magnetic conductivity of about 10 mu H and direct current bias rate of 98-99 percent, and cannot meet higher and higher use requirements in some precise electrical appliances due to direct current bias.
Disclosure of Invention
The invention aims to provide a preparation method of high-density carbonyl iron powder, which aims to overcome the defects of the prior art.
In order to achieve the above purpose, the following technical scheme is provided:
a preparation method of carbonyl iron powder special for an iron powder core comprises the following steps:
s1, injecting carbonyl iron liquid into an evaporator, and heating to vaporize the carbonyl iron liquid into carbonyl iron steam;
s2, quantitatively conveying carbonyl iron steam into the decomposer through pressure, and simultaneously introducing carbon monoxide and ammonia gas in a timed and quantitative manner to mix with the carbonyl iron steam;
s3, heating by four sections outside the decomposing furnace, and controlling the decomposition temperature in the decomposing furnace into four sections;
s4, heating carbonyl iron steam and mixed gas of ammonia gas and carbon monoxide in a decomposing furnace in sequence at four stages, and decomposing and condensing carbonyl iron into carbonyl iron powder particles;
s5, screening carbonyl iron powder in a certain particle size range, and collecting the carbonyl iron powder;
and S6, carrying out micro-aerobic treatment on the carbonyl iron powder collected in the S5 by using nitrogen with certain oxygen content to obtain a finished product.
Preferably, the four-stage decomposition temperatures in the decomposition furnace are respectively as follows: the first section (320-.
Preferably, the decomposing furnace has a diameter of 2m and a heating power of (20-40) Kw.
Preferably, the carbonyl iron steam is introduced into the decomposition furnace from the evaporation furnace at a speed of (50-55) L/h.
Preferably, the ammonia gas is in the range of (1-3) m3The reaction mixture was charged into the decomposing furnace at a rate of/h.
Preferably, the carbon monoxide is present at (20-30) m3The reaction mixture was charged into the decomposing furnace at a rate of/h.
Preferably, the oxygen content in the nitrogen gas in step S6 is (1-3)%.
Preferably, the carbonyl iron powder described in step S5 has a particle size ranging from (1.5 to 2.5) μm.
The invention has the beneficial effects that:
1. according to the invention, the internal structure of the obtained carbonyl iron powder is controlled to be more compact by controlling the decomposition parameters of the carbonyl iron, and large particles in the powder are removed by a physical means, so that the direct current bias can be effectively improved when the carbonyl iron powder is applied to the iron powder core.
2. The obtained carbonyl iron powder is subjected to micro-oxidation treatment, so that the magnetic core loss of the carbonyl iron powder is reduced when the carbonyl iron powder is applied to an iron powder core.
Detailed Description
The present design will be described in detail below.
A preparation method of carbonyl iron powder special for an iron powder core comprises the following steps:
s1, injecting carbonyl iron liquid into an evaporator, and heating to vaporize the carbonyl iron liquid into carbonyl iron steam;
s2, quantitatively conveying carbonyl iron steam into the decomposing furnace through pressure, and simultaneously introducing carbon monoxide and ammonia gas in a timed and quantitative manner to mix with the carbonyl iron steam;
s3, heating by four sections outside the decomposing furnace, and controlling the decomposition temperature in the decomposing furnace into four sections;
s4, in the decomposer, the carbonyl iron steam and the mixed gas of ammonia gas and carbon monoxide are sequentially subjected to four-stage temperature heating treatment, and carbonyl iron is decomposed and condensed into carbonyl iron powder particles;
s5, screening carbonyl iron powder in a certain particle size range, and collecting the carbonyl iron powder;
and S6, carrying out micro-aerobic treatment on the carbonyl iron powder collected in the S5 by using nitrogen with certain oxygen content to obtain a finished product.
Wherein, the four-stage decomposition temperature in the decomposition furnace is respectively as follows: the first section (320-.
Wherein the diameter of the decomposing furnace is 2m, and the heating power is (20-40) Kw.
Wherein the carbonyl iron steam is introduced into the decomposition furnace from the evaporation furnace at the speed of (50-55) L/h.
Wherein the ammonia gas is (1-3) m3The reaction mixture was charged into the decomposing furnace at a rate of/h.
Wherein the carbon monoxide is present in an amount of (20-30) m3The reaction mixture was charged into the decomposing furnace at a rate of/h.
Wherein the oxygen content in the nitrogen gas in step S6 is (1-3)%.
Wherein the particle size range of the carbonyl iron powder in the step S5 is (1.5-2.5) μm.
Examples
Example one
A preparation method of carbonyl iron powder special for an iron powder core comprises the following steps:
s1, injecting carbonyl iron liquid into an evaporator, and heating to vaporize the carbonyl iron liquid into carbonyl iron steam;
s2, introducing carbonyl iron steam into a decomposing furnace with the diameter of 2m at the speed of 50L/h through pressure, and simultaneously introducing the carbonyl iron steam into the decomposing furnace at the speed of 1m3Nitrogen was injected at a rate of 20 m/h3Filling carbon monoxide at a speed of/h, wherein the carbon monoxide is mixed with the carbonyl iron steam, and the heating power is 20 Kw;
s3, heating by four sections outside the decomposing furnace, and controlling the decomposing temperature in the decomposing furnace to be divided into four sections, wherein the first section is 320 ℃, the second section is 300 ℃, the third section is 290 ℃ and the fourth section is 270 ℃;
s4, in the decomposer, the carbonyl iron steam and the mixed gas of ammonia gas and carbon monoxide are sequentially subjected to four-stage temperature heating treatment, and carbonyl iron is decomposed and condensed into carbonyl iron powder particles;
s5, screening carbonyl iron powder with the particle size range of 1.5 mu m, and collecting;
s6, carrying out micro-aerobic treatment on the carbonyl iron powder collected in the S5 by using nitrogen containing 1% of oxygen to obtain a finished product.
Example two
A preparation method of carbonyl iron powder special for an iron powder core comprises the following steps:
s1, injecting carbonyl iron liquid into an evaporator, and heating to vaporize the carbonyl iron liquid into carbonyl iron steam;
s2, passingIntroducing carbonyl iron steam into a decomposing furnace with the diameter of 2m at the speed of 53L/h under pressure, and simultaneously introducing the carbonyl iron steam into the decomposing furnace at the speed of 2m3Nitrogen was injected at a rate of 25 m/h3Filling carbon monoxide at a speed of/h to mix the nitrogen, the carbon monoxide and the carbonyl iron steam, wherein the heating power is 30 Kw;
s3, heating by four sections outside the decomposing furnace, and controlling the decomposing temperature in the decomposing furnace to be divided into four sections, namely a first section 335 ℃, a second section 310 ℃, a third section 300 ℃ and a fourth section 285 ℃;
s4, in the decomposer, the carbonyl iron steam and the mixed gas of ammonia gas and carbon monoxide are sequentially subjected to four-stage temperature heating treatment, and carbonyl iron is decomposed and condensed into carbonyl iron powder particles;
s5, screening carbonyl iron powder with the particle size range of 2 mu m, and collecting;
s6, carrying out micro-aerobic treatment on the carbonyl iron powder collected in the S5 by using nitrogen containing 2% of oxygen to obtain a finished product.
EXAMPLE III
A preparation method of carbonyl iron powder special for an iron powder core comprises the following steps:
s1, injecting carbonyl iron liquid into an evaporator, and heating to vaporize the carbonyl iron liquid into carbonyl iron steam;
s2, introducing carbonyl iron steam into a decomposing furnace with the diameter of 2m at the speed of 55L/h through pressure, and simultaneously introducing the carbonyl iron steam into the decomposing furnace at the speed of 3m3Nitrogen was injected at a rate of 30 m/h3Filling carbon monoxide at a speed of/h, wherein the carbon monoxide is mixed with the carbonyl iron steam, and the heating power is 40 Kw;
s3, heating four sections outside the decomposing furnace, and controlling the decomposing temperature in the decomposing furnace to be divided into four sections, wherein the first section is 350 ℃, the second section is 320 ℃, the third section is 310 ℃ and the fourth section is 300 ℃;
s4, in the decomposer, the carbonyl iron steam and the mixed gas of ammonia gas and carbon monoxide are sequentially subjected to four-stage temperature heating treatment, and carbonyl iron is decomposed and condensed into carbonyl iron powder particles;
s5, screening carbonyl iron powder with the particle size range of 2.5 mu m, and collecting the carbonyl iron powder so as to remove large particles in the powder;
and S6, carrying out micro-aerobic treatment on the carbonyl iron powder collected in the S5 by using nitrogen containing 3% of oxygen to obtain a finished product.
The embodiment can effectively improve the direct current bias when the carbonyl iron powder is used as the iron powder core, ensure that the direct current bias reaches 99.5 to 99.8 percent, and reduce the magnetic core loss when the carbonyl iron powder is used as the iron powder core.
Claims (8)
1. A preparation method of carbonyl iron powder special for an iron powder core is characterized by comprising the following steps:
s1, injecting carbonyl iron liquid into an evaporator, and heating to vaporize the carbonyl iron liquid into carbonyl iron steam;
s2, quantitatively conveying carbonyl iron steam into the decomposing furnace through pressure, and simultaneously introducing carbon monoxide and ammonia gas in a timed and quantitative manner to mix with the carbonyl iron steam;
s3, heating by four sections outside the decomposing furnace, and controlling the decomposition temperature in the decomposing furnace into four sections;
s4, heating carbonyl iron steam and mixed gas of ammonia gas and carbon monoxide in a decomposing furnace in sequence at four stages, and decomposing and condensing carbonyl iron into carbonyl iron powder particles;
s5, screening carbonyl iron powder in a certain particle size range, and collecting the carbonyl iron powder;
and S6, carrying out micro-aerobic treatment on the carbonyl iron powder collected in the S5 by using nitrogen with certain oxygen content to obtain a finished product.
2. The method for preparing carbonyl iron powder specially used for iron powder cores according to claim 1, wherein the four decomposition temperatures in the decomposition furnace are respectively: the first section (320-.
3. The method for preparing carbonyl iron powder specially for iron powder cores as claimed in claim 1, wherein the decomposing furnace has a diameter of 2m and a heating power of (20-40) Kw.
4. The method for preparing carbonyl iron powder specially for iron powder core as claimed in claim 1, wherein the carbonyl iron steam is introduced into the decomposing furnace from the evaporating furnace at a rate of (50-55) L/h.
5. The method for preparing carbonyl iron powder specially used for iron powder cores according to claim 1, wherein the ammonia gas is (1-3) m3The reaction mixture was charged into the decomposing furnace at a rate of/h.
6. The method for preparing carbonyl iron powder specially for iron powder core as claimed in claim 1, wherein the carbon monoxide is (20-30) m3The reaction mixture was charged into the decomposing furnace at a rate of/h.
7. The method for preparing carbonyl iron powder specially for iron powder cores as claimed in claim 1, wherein the oxygen content in the nitrogen gas in step S6 is (1-3)%.
8. The method as claimed in claim 1, wherein the carbonyl iron powder of step S5 has a particle size of (1.5-2.5) μm.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1027293A (en) * | 1949-11-11 | 1953-05-11 | Basf Ag | Process for the production of an iron powder for sintered metal metallurgy |
| 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 |
| CN101209863A (en) * | 2007-12-25 | 2008-07-02 | 金川集团有限公司 | Passivation method of carbonyl iron powder |
| CN103046033A (en) * | 2012-12-21 | 2013-04-17 | 中国钢研科技集团有限公司 | Preparation method of coated carbonyl iron powder |
| CN104475760A (en) * | 2014-12-07 | 2015-04-01 | 金川集团股份有限公司 | Production method of carbonyl iron powder |
| CN104551013A (en) * | 2014-12-07 | 2015-04-29 | 金川集团股份有限公司 | Method for controlling particle size of carbonyl iron powder during decomposition process |
| CN104588680A (en) * | 2014-12-07 | 2015-05-06 | 金川集团股份有限公司 | Carbonyl iron decomposition method capable of controlling oxygen content in iron powder |
| CN109451715A (en) * | 2018-10-31 | 2019-03-08 | 中北大学 | A kind of graphene-carbonyl iron dust@ferroso-ferric oxide electro-magnetic wave absorption composite material |
-
2020
- 2020-01-02 CN CN202010001653.7A patent/CN113059183B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1027293A (en) * | 1949-11-11 | 1953-05-11 | Basf Ag | Process for the production of an iron powder for sintered metal metallurgy |
| 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 |
| CN101209863A (en) * | 2007-12-25 | 2008-07-02 | 金川集团有限公司 | Passivation method of carbonyl iron powder |
| CN103046033A (en) * | 2012-12-21 | 2013-04-17 | 中国钢研科技集团有限公司 | Preparation method of coated carbonyl iron powder |
| CN104475760A (en) * | 2014-12-07 | 2015-04-01 | 金川集团股份有限公司 | Production method of carbonyl iron powder |
| CN104551013A (en) * | 2014-12-07 | 2015-04-29 | 金川集团股份有限公司 | Method for controlling particle size of carbonyl iron powder during decomposition process |
| CN104588680A (en) * | 2014-12-07 | 2015-05-06 | 金川集团股份有限公司 | Carbonyl iron decomposition method capable of controlling oxygen content in iron powder |
| CN109451715A (en) * | 2018-10-31 | 2019-03-08 | 中北大学 | A kind of graphene-carbonyl iron dust@ferroso-ferric oxide electro-magnetic wave absorption composite material |
Non-Patent Citations (2)
| Title |
|---|
| 何旭初、陈兆盈: "《钢结硬质合金的制备原理与技术》", 31 January 2017, 湖南科学技术出版社 * |
| 韩凤麟等: "《粉末冶金手册（上册）》", 31 May 2012, 冶金工业出版社 * |
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