CN1023583C - low-loss oxide magnetic material and manufacturing method thereof - Google Patents
low-loss oxide magnetic material and manufacturing method thereof Download PDFInfo
- Publication number
- CN1023583C CN1023583C CN 90104527 CN90104527A CN1023583C CN 1023583 C CN1023583 C CN 1023583C CN 90104527 CN90104527 CN 90104527 CN 90104527 A CN90104527 A CN 90104527A CN 1023583 C CN1023583 C CN 1023583C
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- China
- Prior art keywords
- oxygen content
- low
- sintering
- ball milling
- magnetic material
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- Expired - Fee Related
Links
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 7
- 239000000696 magnetic material Substances 0.000 title abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000001301 oxygen Substances 0.000 claims abstract description 12
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 11
- 238000000498 ball milling Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000000654 additive Substances 0.000 claims abstract description 4
- 230000000996 additive effect Effects 0.000 claims abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 abstract description 2
- 230000005291 magnetic effect Effects 0.000 description 6
- 230000035699 permeability Effects 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 150000001455 metallic ions Chemical class 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
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- Magnetic Ceramics (AREA)
- Soft Magnetic Materials (AREA)
Abstract
The invention relates to a formula of a low-loss oxide magnetic material and a manufacturing method thereof, wherein a combined additive is added, and finally sintering and cooling are carried out under the atmosphere of controlling the oxygen content according to the oxide process (ball milling, presintering and molding) to prepare a low-power-consumption Mn-Zn ferrite material which can be used for a switching power supply transformer and a U-shaped line output transformer used under the frequency of 30 KC/s.
Description
The present invention relates to a kind of prescription and manufacture method of low loss ferrite material.
The Mn-Zn based ferrite is used widely on electronic equipments such as communication, electronic computer, television set.The high frequencyization of electronic equipment, miniaturization, high reliability all require the magnetic material high frequency characteristics good, low in energy consumption, especially require low in energy consumptionly when 60～100 ℃ of working temperatures, promptly have negative temperature coefficient.
U.Konig(IEEE Trans On Magnetics, MAG-11 No5,1975) to have reported molecular formula be Zn
0.3Fe
2+ 0.07Mn
0.52Ni
0.11Fe
2O
4The low power consumption Mn-Zn ferrite material, its magnetic permeability μ
i=2800, saturation induction density Bs=370mT, power consumption 100mw/cm
3, least in power-consuming 75 ℃ of left and right sides, but power consumption still is higher.
Zhao Luoyi (magnetisable material and device, 17 volumes, 3 phases, 1986) discloses the article of making the negative temperature coefficient Ferrite Material, has added NiO, CaCO
3, adopt during last sintering vacuumize, the partial pressure of oxygen in the method control vacuum furnace such as logical nitrogen, made the low power consumption Mn-Zn ferrite material, magnetic permeability μ
i2400,25 ℃ of power consumption Pv are 6.8mw/g, and Pv is 9.8mw/g in the time of 100 ℃, its weak point, and interval least in power-consuming is at 50～70 ℃, and technical process control is complicated, is not suitable for industrial production.
In recent years, disclose JP61-42104A, a kind of high-frequency magnetic material is provided, Main Ingredients and Appearance is Fe
2O
3, MnO, ZnO, also added a certain amount of CaCO
3, SiO
2, Nb
2O
5, K
2CO
3, can be used as several watts to tens watts transformers that under 10KHz～100KHz, use, but its weak point being, sintering temperature is higher, and interval least in power-consuming is still at 50～70 ℃.
Task of the present invention is intended to overcome above-mentioned prior art deficiency, and providing a kind of is negative temperature coefficient low power consumption Mn-Zn ferrite material in 25～100 ℃ of intervals, and is suitable for a large amount of productions.
Task of the present invention can reach by following measure:
The present invention adopts conventional ceramic technique technology to make magnetic material, and raw material are Fe
2O
3(purity is 99.8%, includes Mg 9ppm, Ca 15ppm, and Ni 16ppm, Si0); MnCO
3(purity 94.51% contains Mg 22ppm, Ca 32ppm, Ni 3ppm, Cu 2ppm); ZnO(purity 97.64%, Mg 2ppm, Ca 3ppm, Cu 1ppm)
Additive: NiO, CaO, SiO
2, K
2CO
3
Process for making is as follows:
The raw material ball milling, give burning, pulverize, add additive, ball milling, filtration, oven dry again;
With 2344 gram raw material through above-mentioned operation altogether loss 217 grams, the proportion of goods damageds are 9.3%, wherein since the natural wastage and the process loss of chemical reaction respectively account for about 50%.
The characteristics of technical process are:
(1) according to a certain ratio, add the deionized water mixing and ball milling with raw material, 6 hours mix grinding time, rotating speed 88RPM, material: ball: the ratio of water is 1: 2.5: 1.1.
(2) give rotating speed 3RPM when burning, 950～1050 ℃ of temperature, 20～40 minutes time.
(3) last sintering temperature is 1260～1320 ℃, adopts only to feed nitrogen and control oxygen content in the sintering atmosphere, intensification oxygen content 15～20%, high temperature 5～8%, cooling oxygen content＜0.01%.
Below the reason of Mn-Zn Ferrite Material composition is controlled in explanation:
The selection of fundamental component: Fe
2O
350～60mol%, MnO 20～40mol%, ZnO 5～20mol%, the magnetic permeability of this scope is moderate.Fe
2O
3Very little, loss is big, can not use; Fe
2O
3Higher, and ZnO is lower, magnetic permeability is too little, and then Curie point is too low again greater than 28mol% as ZnO.
An amount of NiO that adds can reduce Fe
2+, make μ
i(t) secondary peak of curve moves to the high temperature direction, and little to the magnetic flux density influence, the NiO that adds 0.5～2.0wt% is all effective, and adding 1.2～1.8wt% has effect preferably.
Adding CaO can reduce the wastage, and the Ca ion deposition improves the grain boundary resistance rate in the grain boundary, the CaO that adds 0.05wt% makes permeability reach the highest, the CaO that adds 0.5wt% makes quality factor Q reach the highest, greater than 0.01wt% just effectively, is advisable with 0.01～0.1wt%.
The combination of NiO and CaO is added, and makes μ
iCan improve about 10%, power consumption descends about 35%.
SiO
2Interpolation, resistance is increased, reduce eddy current loss, but, can make μ greater than 0.007wt%
iDescend.Make μ
iUnder the prerequisite that does not descend, power consumption can reduce about 6mw/g.
K
2CO
3, the monovalent ion radius is bigger, and (K is 1.33
), add monovalent metallic ion, can reduce Fe
2+Generate, improve resistivity, μ
iWith Q the K of preferable effect is arranged all
2CO
3Addition is 10
-3The order of magnitude is advisable with 0.1wt%.
The present invention compares with prior art has following outstanding effect:
1. prior art adopts the partial pressure of oxygen in the method control vacuum furnaces such as vacuumizing, lead to nitrogen when sintering, and the technology controlling and process complexity is not suitable for big production.The present invention need not vacuumize, sintering and cooling under the nitrogen of control partial pressure of oxygen, and technology is simple, is applicable to the big production of industry, has remarkable economic efficiency.
2. prior art has less power consumption 50～70 ℃ of temperature ranges, and power consumption increases again when being higher than 70 ℃, and the present invention has negative temperature coefficient (seeing embodiment) 25～100 ℃ of temperature ranges.The working temperature interval is improved 10～30 ℃ than prior art.
The present invention will be described further in conjunction with the following example:
Embodiment
Stock: Fe
2O
355.75mol%, MnO 27.28mol%, ZnO 15.45mol%; Add Ni
2O
31.52wt%, CaO 0.05wt%, SiO
20.007wt%, K
2CO
30.1wt% after the mixing and ball milling, gives and burns 1050 ℃ of temperature, through pulverizing, ball milling, moulding; Make the garden ring of Φ 25 * 20 * 7, sintering and cooling under the nitrogen of control oxygen content (heating up 15～20%, high temperature 5～8%, cooling＜0.01%) at 16KC/S, record the following table performance under the condition of 1500GS.
K
2CO
3P
v（mw/g） B
s（GS）
（wt%） μi 25℃ 80℃ 100℃ 25℃ 100℃
Comparative example 0 2,056 13.5 13.0 15.3 4,500 3200
0 2450 10.1 9.72 11.6 4620 3230
The present invention 0.1 2,340 13.1 7.9 8.2 4,990 3660
Claims (2)
1, a kind of low loss ferrite material is by Fe
2O
3, MnO, compositions such as ZnO is characterized in that: stock
(1)Fe
2O
350～60mol%
(2)MnO20～40mol%
(3)ZnO5～20mol%
The combination additive is:
(1)NiO0.5～2.0wt%
(2)CaO0.01～0.1wt%
(3)SiO
2＜0.007wt%
(4)K
2CO
30.1wt%
2,, through ball milling, give burnings, pulverizing, ball milling, oven dry, processes such as sintering at last again, it is characterized in that according to the manufacture method of the described low loss ferrite material of claim 1:
(1) gives 950～1050 ℃ of burning temperature, 20～40 minutes time;
(2) last sintering temperature is 1260～1320 ℃, adopts only to feed nitrogen and control oxygen content in the sintering atmosphere, intensification oxygen content 15～20%, high temperature oxygen content 5～8%, cooling oxygen content＜0.01%
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90104527 CN1023583C (en) | 1990-07-14 | 1990-07-14 | low-loss oxide magnetic material and manufacturing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90104527 CN1023583C (en) | 1990-07-14 | 1990-07-14 | low-loss oxide magnetic material and manufacturing method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1058287A CN1058287A (en) | 1992-01-29 |
| CN1023583C true CN1023583C (en) | 1994-01-19 |
Family
ID=4878596
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 90104527 Expired - Fee Related CN1023583C (en) | 1990-07-14 | 1990-07-14 | low-loss oxide magnetic material and manufacturing method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1023583C (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11214213A (en) * | 1998-01-23 | 1999-08-06 | Tdk Corp | Ferrite, transformer and its driving method |
| JP3758464B2 (en) * | 2000-05-12 | 2006-03-22 | 株式会社村田製作所 | Laminated electronic components |
| CN100344571C (en) * | 2005-03-21 | 2007-10-24 | 乳源东阳光磁性材料有限公司 | Lowloss ferritc in manganese zinc series and preparation method thereof |
| CN100340524C (en) * | 2005-03-21 | 2007-10-03 | 乳源东阳光磁性材料有限公司 | Ferrite in manganese zinc series in both five thousands of high curie temperature and lowloss and preparing process thereof |
| CN100340523C (en) * | 2005-03-21 | 2007-10-03 | 乳源东阳光磁性材料有限公司 | Higher magnetic permcability lowloss ferritc in manganese zinc series and preparation method thereof |
| CN100344572C (en) * | 2005-03-21 | 2007-10-24 | 乳源东阳光磁性材料有限公司 | High additivity ferrite in manganese zinc series and preparation method thereof |
| CN101859622B (en) * | 2009-04-08 | 2012-02-15 | 广东江粉磁材股份有限公司 | Method for manufacturing intermediate-frequency low-loss MnZn ferrite magnetic core |
| WO2012151714A1 (en) * | 2011-05-09 | 2012-11-15 | 临沂中瑞电子有限公司 | Nicuzn ferrite material with high magnetic conductivity |
| CN102416476A (en) * | 2011-12-09 | 2012-04-18 | 东阳市金砖磁业有限公司 | Method for preparing low-resistivity ferrite magnet material |
-
1990
- 1990-07-14 CN CN 90104527 patent/CN1023583C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1058287A (en) | 1992-01-29 |
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