CN102992753A - Low power consumption preparation method of Mn-Zn soft magnetic ferrite material - Google Patents
Low power consumption preparation method of Mn-Zn soft magnetic ferrite material Download PDFInfo
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- CN102992753A CN102992753A CN2012104831842A CN201210483184A CN102992753A CN 102992753 A CN102992753 A CN 102992753A CN 2012104831842 A CN2012104831842 A CN 2012104831842A CN 201210483184 A CN201210483184 A CN 201210483184A CN 102992753 A CN102992753 A CN 102992753A
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- sintering
- magnetic ferrite
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- 239000000463 material Substances 0.000 title claims abstract description 23
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 229910021392 nanocarbon Inorganic materials 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 238000000498 ball milling Methods 0.000 claims abstract description 10
- 238000000465 moulding Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 239000004615 ingredient Substances 0.000 claims description 15
- 235000002918 Fraxinus excelsior Nutrition 0.000 claims description 12
- 239000002956 ash Substances 0.000 claims description 12
- WJZHMLNIAZSFDO-UHFFFAOYSA-N manganese zinc Chemical compound [Mn].[Zn] WJZHMLNIAZSFDO-UHFFFAOYSA-N 0.000 claims description 12
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 9
- 238000010792 warming Methods 0.000 claims description 9
- 230000004048 modification Effects 0.000 claims description 7
- 238000012986 modification Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 3
- 239000003082 abrasive agent Substances 0.000 claims description 3
- 229910052810 boron oxide Inorganic materials 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 3
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 3
- 239000005543 nano-size silicon particle Substances 0.000 claims description 3
- 239000002105 nanoparticle Substances 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- 239000008188 pellet Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000004907 flux Effects 0.000 abstract description 2
- 238000009472 formulation Methods 0.000 abstract 1
- 238000004891 communication Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000411 inducer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
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- Soft Magnetic Materials (AREA)
- Magnetic Ceramics (AREA)
Abstract
The invention discloses a low power consumption preparation method of Mn-Zn soft magnetic ferrite material, which comprises the following steps of: preparing main material and auxiliary material; pre-sintering, mixing the main material and the auxiliary material and carrying out secondary ball-milling; and molding and sintering to obtain the Mn-Zn soft magnetic ferrite core. According to the preparation method, modified nanocarbon component is added to play a role of bridge combination among the different raw materials; therefore, the raw materials are distributed very well, high in density and grain boundary resistivity, low in porosity and large and even in crystalline grains, the raw material formulation is reasonably improved, and the magnetic core has lower power consumption after being burnt; furthermore, the indexes such as frequency characteristic, Curie temperature, saturation flux density and the like are greatly improved.
Description
Technical field
The present invention relates to a kind of preparation method of manganese zinc (Mn-Zn) soft magnetic ferrite material of reduce power consumption.
Background technology
Lower losses ferrite magnetic, magnetic core are to realize that being used as the products such as inducer, wave filter, pulse transformer in the electronicss such as program control communication, digital technique, network communication colour TV makes its miniaturization, the requisite electronic material of lightweight, constantly reduce the power consumption in the magneticsubstance, it is the pursuit of being engaged in these professional engineering technical personnel and production firm always, and the performance index of material are all unsatisfactory such as loss, frequency response characteristic, Curie temperature etc.
Summary of the invention
In order to alleviate shortcomings and deficiencies of the prior art, the object of the present invention is to provide a kind of preparation method of manganese zinc (Mn-Zn) soft magnetic ferrite material of reduce power consumption.
The present invention adopts following technical scheme to achieve these goals:
The preparation method of the manganese zinc (Mn-Zn) soft magnetic ferrite material of reduce power consumption may further comprise the steps:
(1) joins major ingredient: by mole% being Fe
2O
348-49mol%, MnO 23-25mol%, ZnO 26.5-27.5mol%, iron powder 0.2-0.3mol%, manganese powder 0.13-0.2mol% prepare burden;
(2) join auxiliary material: be equivalent to the modified Nano carbon of major ingredient 0.015-0.025wt%, the lanthanum trioxide of 0.013-0.015wt%, the boron oxide of 0.038-0.042wt%, the ZrO of 0.027-0.033wt%
2, 0.038-0.045wt% Nb
2O
5Described modified Nano carbon prepares by the following method:
A, the trees ashes are soaked 2-3 hour with the sodium hydroxide solution of 10-15% after;
B, usefulness 10-15% hydrochloric acid soln soaked 2-3 hour;
C, with deionized water wash repeatedly is neutral to the trees ashes, oven dry;
D, be ground to 0.8-1.2 μ m powder, obtain modification trees ashes;
E, in nano-sized carbon, add and be equivalent to the modification trees ashes obtained above of its weight 2-4%, the nano silicon of 2-3%, fully be mixed to get;
(3) pre-burning: the major ingredient that step (1) is prepared adds water and dispersion agent carried out one time ball milling 2-2.5 hour, and then spraying drying is carried out pre-burning, and calcined temperature is 865-915 ℃, and the pre-burning time is 2-3 hour;
(4) major ingredient, auxiliary material mix and secondary ball milling: the pre-burning major ingredient is added the auxiliary material of removing outside the modified Nano carbon, add entry and dispersion agent and carried out secondary ball milling 1-1.5 hour, spraying drying, built in 180-230 order pellet;
(5) moulding: the secondary ball abrasive material is mixed with modified Nano carbon, 12800-14500 rev/min, high speed dispersion 2-2.5 hour, then be pressed into base;
(6) sintering: put the moulded blank after the above-mentioned moulding into sintering oven, in the nitrogen atmosphere of the long-pending content of 0.08%-0.12% oxysome, be warming up to 708-730 ℃ with 170-180 ℃ of/hour speed first, be incubated 1-2 hour; In the nitrogen atmosphere of the long-pending content of 0.8%-1% oxysome, when being warming up to 875-915 ℃ with 133-138 ℃ of/hour speed, be incubated 0.5-1 hour; In the nitrogen atmosphere of the long-pending content of 3%-5% oxysome, be warming up to 1280-1350 ℃ with 80-90 ℃ of/hour speed again, the sintered heat insulating time is 2.5-3.5 hour; In the nitrogen atmosphere of the long-pending content of 0.08%-0.12% oxysome, namely get the MnZn magnetic ferrite magnetic core of reduce power consumption behind the sintering after the cooling.
Beneficial effect of the present invention:
1, the present invention can be used as the bridge keying action between the different material by adding the modified Nano carbon component, uses feed distribution better, density is high, the grain boundary resistance rate high, void content is low, crystal grain is large and even, the rational modification composition of raw materials is so that after magnetic core fires, have lower power consumption;
2, have higher dc superposition characteristic, solve the loose problem of magnetic core surface tissue, the product physical strength improves, magnetic permeability rises, loss reduces thereby make;
3, the indexs such as frequency response characteristic, Curie temperature, saturation magnetic flux density all have greatly improved.
Embodiment
Embodiment 1: the preparation method of the manganese zinc (Mn-Zn) soft magnetic ferrite material of reduce power consumption may further comprise the steps:
(1) joins major ingredient: by mole% being Fe
2O
348.5mol%, MnO 24mol%, ZnO 27.1mol%, iron powder 0.25mol%, manganese powder 0.15mol% prepare burden;
(2) join auxiliary material: be equivalent to the modified Nano carbon of major ingredient 0.02wt%, the lanthanum trioxide of 0.014wt%, the boron oxide of 0.04wt%, the ZrO of 0.03wt%
2, 0.042wt% Nb
2O
5Described modified Nano carbon prepares by the following method:
A, the trees ashes are soaked 2-3 hour with 10% sodium hydroxide solution after;
B, soaked 2-3 hour with 10% hydrochloric acid soln;
C, with deionized water wash repeatedly is neutral to the trees ashes, oven dry;
D, be ground to 0.8-1.2 μ m powder, obtain modification trees ashes;
E, in nano-sized carbon, add and be equivalent to the modification trees ashes obtained above of its weight 3%, 2.5% nano silicon, fully be mixed to get;
(3) pre-burning: the major ingredient that step (1) is prepared adds water and dispersion agent carried out one time ball milling 2-2.5 hour, and then spraying drying is carried out pre-burning, and calcined temperature is 890 ℃, and the pre-burning time is 2-3 hour;
(4) major ingredient, auxiliary material mix and secondary ball milling: the pre-burning major ingredient is added the auxiliary material of removing outside the modified Nano carbon, add entry and dispersion agent and carried out secondary ball milling 1-1.5 hour, spraying drying, built in 200 order pellets;
(5) moulding: the secondary ball abrasive material is mixed with modified Nano carbon, 13500 rev/mins, high speed dispersion 2-2.5 hour, then be pressed into base;
(6) sintering: put the moulded blank after the above-mentioned moulding into sintering oven, in the nitrogen atmosphere of the long-pending content of 0.08%-0.12% oxysome, be warming up to 720 ℃ with 175 ℃ of/hour speed first, be incubated 1-2 hour; In the nitrogen atmosphere of the long-pending content of 0.8%-1% oxysome, when being warming up to 900 ℃ with 135 ℃ of/hour speed, be incubated 0.5-1 hour; In the nitrogen atmosphere of the long-pending content of 3%-5% oxysome, be warming up to 1320 ℃ with 85 ℃ of/hour speed again, the sintered heat insulating time is 3 hours; In the nitrogen atmosphere of the long-pending content of 0.08%-0.12% oxysome, namely get the MnZn magnetic ferrite magnetic core of reduce power consumption behind the sintering after the cooling.
The performance data of the magnetic ferrite magnetic core that makes by above-described embodiment:
Claims (1)
1. the preparation method of the manganese zinc (Mn-Zn) soft magnetic ferrite material of a reduce power consumption is characterized in that may further comprise the steps:
(1) joins major ingredient: by mole% being Fe
2O
348-49mol%, MnO 23-25mol%, ZnO 26.5-27.5mol%, iron powder 0.2-0.3mol%, manganese powder 0.13-0.2mol% prepare burden;
(2) join auxiliary material: be equivalent to the modified Nano carbon of major ingredient 0.015-0.025wt%, the lanthanum trioxide of 0.013-0.015wt%, the boron oxide of 0.038-0.042wt%, the ZrO of 0.027-0.033wt%
2, 0.038-0.045wt% Nb
2O
5Described modified Nano carbon prepares by the following method:
A, the trees ashes are soaked 2-3 hour with the sodium hydroxide solution of 10-15% after;
B, usefulness 10-15% hydrochloric acid soln soaked 2-3 hour;
C, with deionized water wash repeatedly is neutral to the trees ashes, oven dry;
D, be ground to 0.8-1.2 μ m powder, obtain modification trees ashes;
E, in nano-sized carbon, add and be equivalent to the modification trees ashes obtained above of its weight 2-4%, the nano silicon of 2-3%, fully be mixed to get;
(3) pre-burning: the major ingredient that step (1) is prepared adds water and dispersion agent carried out one time ball milling 2-2.5 hour, and then spraying drying is carried out pre-burning, and calcined temperature is 865-915 ℃, and the pre-burning time is 2-3 hour;
(4) major ingredient, auxiliary material mix and secondary ball milling: the pre-burning major ingredient is added the auxiliary material of removing outside the modified Nano carbon, add entry and dispersion agent and carried out secondary ball milling 1-1.5 hour, spraying drying, built in 180-230 order pellet;
(5) moulding: the secondary ball abrasive material is mixed with modified Nano carbon, 12800-14500 rev/min, high speed dispersion 2-2.5 hour, then be pressed into base;
(6) sintering: put the moulded blank after the above-mentioned moulding into sintering oven, in the nitrogen atmosphere of the long-pending content of 0.08%-0.12% oxysome, be warming up to 708-730 ℃ with 170-180 ℃ of/hour speed first, be incubated 1-2 hour; In the nitrogen atmosphere of the long-pending content of 0.8%-1% oxysome, when being warming up to 875-915 ℃ with 133-138 ℃ of/hour speed, be incubated 0.5-1 hour; In the nitrogen atmosphere of the long-pending content of 3%-5% oxysome, be warming up to 1280-1350 ℃ with 80-90 ℃ of/hour speed again, the sintered heat insulating time is 2.5-3.5 hour; In the nitrogen atmosphere of the long-pending content of 0.08%-0.12% oxysome, namely get the MnZn magnetic ferrite magnetic core of reduce power consumption behind the sintering after the cooling.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210483184.2A CN102992753B (en) | 2012-11-23 | 2012-11-23 | Low power consumption preparation method of Mn-Zn soft magnetic ferrite material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210483184.2A CN102992753B (en) | 2012-11-23 | 2012-11-23 | Low power consumption preparation method of Mn-Zn soft magnetic ferrite material |
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| CN102992753A true CN102992753A (en) | 2013-03-27 |
| CN102992753B CN102992753B (en) | 2014-05-21 |
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| CN201210483184.2A Expired - Fee Related CN102992753B (en) | 2012-11-23 | 2012-11-23 | Low power consumption preparation method of Mn-Zn soft magnetic ferrite material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015106568A1 (en) * | 2014-01-14 | 2015-07-23 | 四川省德阳博益磁性材料有限公司 | Preparation process for mnzn soft ferrite having ultra-low value loss and high uq |
| CN106396658A (en) * | 2016-09-05 | 2017-02-15 | 中南大学 | Method for preparing spinel type ferrite material precursor by solid phase reaction |
| CN112299836A (en) * | 2020-11-25 | 2021-02-02 | 南通冠优达磁业有限公司 | High-frequency low-loss soft magnetic ferrite material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04226003A (en) * | 1990-05-09 | 1992-08-14 | Tdk Corp | Composite soft magnetic material and coated particles for composite soft magnetic material |
| CN1486958A (en) * | 2003-04-01 | 2004-04-07 | 上海大学 | Prepn of doped magnetic ferrite material |
| CN101241791A (en) * | 2007-02-06 | 2008-08-13 | 昆山尼赛拉电子器材有限公司 | Wide-temperature and low-consumption Mn-Zn soft magnetic ferrite and its production method |
| CN101266859A (en) * | 2008-01-08 | 2008-09-17 | 上海大学 | Method for quick sintering of micro-crystal ferrite magnetic core part |
-
2012
- 2012-11-23 CN CN201210483184.2A patent/CN102992753B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04226003A (en) * | 1990-05-09 | 1992-08-14 | Tdk Corp | Composite soft magnetic material and coated particles for composite soft magnetic material |
| CN1486958A (en) * | 2003-04-01 | 2004-04-07 | 上海大学 | Prepn of doped magnetic ferrite material |
| CN101241791A (en) * | 2007-02-06 | 2008-08-13 | 昆山尼赛拉电子器材有限公司 | Wide-temperature and low-consumption Mn-Zn soft magnetic ferrite and its production method |
| CN101266859A (en) * | 2008-01-08 | 2008-09-17 | 上海大学 | Method for quick sintering of micro-crystal ferrite magnetic core part |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015106568A1 (en) * | 2014-01-14 | 2015-07-23 | 四川省德阳博益磁性材料有限公司 | Preparation process for mnzn soft ferrite having ultra-low value loss and high uq |
| CN106396658A (en) * | 2016-09-05 | 2017-02-15 | 中南大学 | Method for preparing spinel type ferrite material precursor by solid phase reaction |
| CN106396658B (en) * | 2016-09-05 | 2019-10-15 | 中南大学 | A kind of method that solid phase reaction prepares spinel type ferrite material precursor |
| CN112299836A (en) * | 2020-11-25 | 2021-02-02 | 南通冠优达磁业有限公司 | High-frequency low-loss soft magnetic ferrite material and preparation method thereof |
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| CN102992753B (en) | 2014-05-21 |
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Effective date of registration: 20191218 Address after: 233000 Xianghe Home Floor No.9, Xinhuai Road, Dongsheng Street, Longzihu District, Bengbu City, Anhui Province Patentee after: Bengbu Qibang Science and Technology Information Consulting Co.,Ltd. Address before: 239300, No. three North 100 Road, Tianchang economic and Technological Development Zone, Anhui, Chuzhou Patentee before: TIANCHANG CITY ZHAOTIAN MAGNETOELECTRICITY TECHNOLOGY Co.,Ltd. |
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Effective date of registration: 20221031 Address after: 257000 Economic Development Zone, Lijin County, Dongying City, Shandong Province (to the west of Jiner Road and the north of Lixi Road) Patentee after: Shandong Bailian Chemical Co.,Ltd. Address before: 233000 No.9, 1st floor, Xianghe Jiayuan, Xinhuai Road, Dongsheng Street, Longzihu District, Bengbu City, Anhui Province Patentee before: Bengbu Qibang Science and Technology Information Consulting Co.,Ltd. |
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Granted publication date: 20140521 |