CN1619719A - Manganese zinc ferrite soft magnet and its manufacturing method - Google Patents
Manganese zinc ferrite soft magnet and its manufacturing method Download PDFInfo
- Publication number
- CN1619719A CN1619719A CN 200310108830 CN200310108830A CN1619719A CN 1619719 A CN1619719 A CN 1619719A CN 200310108830 CN200310108830 CN 200310108830 CN 200310108830 A CN200310108830 A CN 200310108830A CN 1619719 A CN1619719 A CN 1619719A
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- China
- Prior art keywords
- temperature
- constant temperature
- zinc ferrite
- manganese
- ferrite soft
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- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 title claims abstract description 11
- JIYIUPFAJUGHNL-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] JIYIUPFAJUGHNL-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 19
- 239000001301 oxygen Substances 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000011534 incubation Methods 0.000 claims description 13
- 230000005389 magnetism Effects 0.000 claims description 7
- 239000004615 ingredient Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 claims 1
- 238000009413 insulation Methods 0.000 abstract description 6
- 229910000859 α-Fe Inorganic materials 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 7
- 238000010586 diagram Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 208000036366 Sensation of pressure Diseases 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- WJZHMLNIAZSFDO-UHFFFAOYSA-N manganese zinc Chemical class [Mn].[Zn] WJZHMLNIAZSFDO-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
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- Magnetic Ceramics (AREA)
- Soft Magnetic Materials (AREA)
Abstract
This invention discloses a method for making manganese-zinc ferrite soft-magnet, which comprises at least one constant temperature insulation in temperature reducing period of sintering process wherein the temperature of constant temperature insulation is lower at least 50 deg.C centigrade than that in temperature reducing period, the optimal is lower at least 10 deg.C, the oxygen content keeps no change in this period. Said invention also discloses a manganese-zinc ferrite made by said method. Said invention has advantages of low power consumption and simple lowest temperature adjustment.
Description
Technical field
The present invention relates to a kind of ferrite in manganese zinc series soft magnetism and manufacture method, especially be fit to make the power ferrite and the manufacture method thereof of power transformer magnetic core.
Background technology
Manganese-zinc ferrite is used widely on electronic equipments such as communication, electronic computer, television set.The miniaturization of electronic equipment, flattening and high reliability all require ferrite soft magnetic to have low-power consumption, and especially working temperature requires power consumption lower in 60-140 ℃ of interval.The least in power-consuming some temperature position (being designated hereinafter simply as " minimum temperature ") of P-T curve is most important to the power ferrite performance, and suitable minimum temperature can make power ferrite have lower power consumption in operating temperature range.
The typical scenario of the sintering circuit of mentioning in the soft magnetic ferrite users' guidebook that magnetic material AEM (MMPA) provides is seen shown in Figure 1.
Temperature-fall period among Fig. 1, temperature are to descend continuously, and oxygen content descends continuously according to oxygen balance is theoretical, its shortcoming is not consider the influence of rate of temperature fall to the oxidation-reduction reaction time, when causing adjusting temperature least in power-consuming, it is improper that Control for Oxygen Content has slightly, and power consumption will worsen.
Summary of the invention
The objective of the invention is to solve the above-mentioned deficiency of existing public technology, a kind of improved sintering method is provided, make the adjustment of manganese-zinc ferrite temperature least in power-consuming comparatively easy, and power consumption is lower.
The present invention is achieved through the following technical solutions: the principal component of Ferrite Material is the Fe that is scaled 51.5～54mol%
2O
3, the MnO of 35～39mol%, remaining is ZnO; Accessory ingredient comprises the CaO that is scaled 0.02～0.08wt%, the V of 0.03～0.06wt%
2O
5Nb with 0.01～0.04wt%
2O
5
If necessary, secondary composition also can comprise SiO
2, Ta
2O
5, ZrO
2In one or more, every kind of content is 0.005～0.04wt%.
Principal component is mixed the back pre-burning, add accessory ingredient, pulverize then, small amount of binder PVA is added in the mixture, make the particle of 80～240 μ m by spray dryer, subsequently, particle is pressed into the finished product blank of required form by mould, hair is bad at a special sintering process, can get the finished product of lower power consumption.
Described sintering process is characterised in that: at least constant temperature incubation step of experience again during the temperature-fall period, and the oxygen content during the incubation step is remained unchanged by control.
Preferably, low 50 ℃ at least of the temperature of the main constant temperature holding stage of the temperature of the constant temperature incubation step of above-mentioned temperature-fall period before, preferably at least low 100 ℃ than temperature-fall period.
The following sintering process of the present invention's process:
A) with 50 ℃ to 300 ℃ the rate of heat addition per hour, be heated to 900 ℃;
B) with 50 ℃ to 200 ℃ the rate of heat addition per hour, be heated to certain temperature between 1250 ℃ and 1360 ℃, the constant temperature insulation is 3 to 5 hours then;
C) be cooled to certain temperature between 1300 ℃ to 1000 ℃ with 50 ℃ to 150 ℃ cooldown rate per hour, be preferably certain temperature between 1250 ℃ to 1100 ℃, and at least than above-mentioned b) the temperature of main holding stage low 50 ℃, preferably hang down 100 ℃ at least, constant temperature kept 20 to 60 minutes then, during this constant temperature, the control oxygen content remains unchanged; (the present invention is called for short this c step and is " cooling insulation " step)
D) after above-mentioned cooling incubation step finishes, continue to be cooled to 1100 ℃ with 50 ℃ to 250 ℃ cooldown rate per hour;
E) cooldown rate below 1100 ℃ is per hour 50 ℃ to 300 ℃.
The oxygen content of above process is regulated according to equilibrium oxygen partial pres-sure is theoretical.
As required, after above-mentioned cooling incubation step, also can experience the incubation step of at least once lowering the temperature again.
The kiln that uses in the sintering circuit of the present invention can be continuous or in batches, but but preferably has batch formula stove of accurately controlling oxygen content and rapid temperature rise and drop.
The beneficial effect that the present invention compared with prior art has: the present invention is provided with an incubation step again at temperature-fall period, help ferrite and fully finish, make the inside and outside oxidizability of ferrite finished product corresponding with the desired oxidizability of temperature least in power-consuming in the redox reaction of this temperature spot.Unlike the prior art, this incubation step has been arranged,, power consumption and minimum temperature thereof have not been had considerable influence yet, thereby reduced power consumption, realized easy adjusting temperature least in power-consuming even temperature-fall period Control for Oxygen Content subsequently has deviation slightly.
Description of drawings
Fig. 1 is the schematic diagram of typical ferrite sintered curve.
Fig. 2 is the sintering curre schematic diagram of the embodiment of the invention 1.
Fig. 3 is the sintering curre schematic diagram of the embodiment of the invention 2.
Fig. 4 is the sintering curre schematic diagram of the embodiment of the invention 3.
Fig. 5 is the sintering curre schematic diagram of comparative example (typical sintering scheme).
The invention will be further described below in conjunction with drawings and Examples.
Embodiment
Adopt the Fe of 53.2mol%
2O
3, the MnO of 36.5mol% and 10.3mol% ZnO as main component, the CaO of 0.04wt%, the V of 0.03wt%
2O
5Nb with 0.02wt%
2O
5As accessory ingredient.Principal component is mixed the back pre-burning, add accessory ingredient, pulverize then, small amount of binder PVA is added in the mixture, make the particle of 80～240 μ m by spray dryer, subsequently, particle is pressed into 60 annular stampings by mould, and 20 the one group curve sintering of pressing respectively shown in Fig. 2,3,4 obtains the about 31mm of external diameter, the about 19mm of internal diameter, the ring specimen of thick about 6mm.
1. up to 900 ℃ the rate of heat addition: 300 ℃/hour;
2. up to 1300 ℃ the rate of heat addition: 150 ℃/hour;
3. 1300 ℃ of insulations 5 hours;
4. 1300 ℃ to 1200 ℃ cooldown rate: 100 ℃/hour;
5. 1200 ℃ of insulations 30 minutes;
6. 1200 ℃ to 1100 ℃ cooldown rate: 100 ℃/hour;
7. 1100 ℃ to 600 ℃ cooldown rate: 200 ℃/hour;
8. the cooldown rate below 600 ℃: 150 ℃/hour;
Oxygen content is regulated according to equilibrium oxygen partial pres-sure is theoretical in this example, and difference from prior art has been incubation step 5 many, and this step oxygen content also remains unchanged.
Embodiment 2: Temperature Distribution is identical with embodiment 1, moves to low temperature in order to make temperature least in power-consuming, and oxygen content integral body is lower than embodiment 1, as shown in Figure 3 curve.
Implement 3: Temperature Distribution is also identical with embodiment 1, moves to high temperature in order to make temperature least in power-consuming, and oxygen content integral body is than embodiment 1 height, curve as shown in Figure 4.
Comparative example: be according to typical sintering scheme sintering.
1. up to 900 ℃ the rate of heat addition: 300 ℃/hour;
2. up to 1300 ℃ the rate of heat addition: 150 ℃/hour;
3. kept 5 hours at 1300 ℃;
4. 1300 ℃ to 1100 ℃ cooldown rate: 100 ℃/hour;
5. 1100 ℃ to 600 ℃ cooldown rate: 200 ℃/hour;
6. the cooldown rate below 600 ℃: 150 ℃/hour;
The oxygen content of each step of comparative example is identical with the oxygen content of embodiment 1 corresponding temperature.
The main distinction of comparative example and embodiment 1,2,3 is to have lacked a constant temperature incubation step in 1300 ℃ to 1100 ℃ the temperature-fall period.
The ring specimen performance of embodiment 1 to 3 and comparative example is recorded by HP4284A and SY8232, and data mean value sees the following form:
| Power consumption P cv(mW/cm 3) | ||||||
| ????25℃ | ????80℃ | ????90℃ | ???100℃ | ???110℃ | ???120℃ | |
| Comparative example | ????649 | ????372 | ????330 | ???315 | ???364 | ???420 |
| Example 1 | ????620 | ????350 | ????310 | ???301 | ???329 | ???406 |
| Example 2 | ????590 | ????330 | ????290 | ???330 | ???350 | ???430 |
| Example 3 | ????644 | ????385 | ????360 | ???330 | ???321 | ???385 |
Data can find out that the power consumption of the embodiment of the invention is low than comparative example from table, and the adjustment of minimum temperature is easier, and can be to the power consumption generation adverse effect of minimum temperature position in the adjustment process.
Claims (5)
1, a kind of method of making the manganese-zinc ferrite soft magnetism by sintering, the temperature experience of its sintering process heats up, main constant temperature is incubated, the cooling three phases, it is characterized in that: experience at least constant temperature incubation step during the described temperature-fall period again, and the oxygen content during this incubation step remains unchanged.
2, the method for manufacturing manganese-zinc ferrite soft magnetism as claimed in claim 1 is characterized in that, low 50 ℃ at least of the temperature of the main constant temperature holding stage of the temperature of the constant temperature incubation step of described temperature-fall period before than temperature-fall period, preferably at least low 100 ℃.
3, the method for manufacturing manganese-zinc ferrite soft magnetism as claimed in claim 2 is characterized in that, the temperature of described main constant temperature holding stage is between 1250 ℃ and 1360 ℃, and the constant temperature temperature retention time is 3 to 5 hours; Be cooled to certain temperature between 1300 ℃ to 1000 ℃ with 50 ℃ to 150 ℃ cooldown rate per hour then, be preferably certain temperature between 1250 ℃ to 1100 ℃, and hang down 50 ℃ than the temperature of main constant temperature holding stage at least, preferably hang down 100 ℃ at least, constant temperature kept 20 to 60 minutes then, between this constant temperature soak, oxygen content is remained unchanged.
4, a kind of manganese-zinc ferrite soft magnetism can be made by claim 1-3 either party method, it is characterized in that: comprise the Fe that is scaled 51.5～54mol% as principal component
2O
3, the MnO of 35～39mol%, remaining is ZnO; With the CaO that is scaled 0.02～0.08wt% that comprises as accessory ingredient, the V of 0.03～0.06wt%
2O
5Nb with 0.01～0.04wt%
2O
5
5, as claim 4 described manganese-zinc ferrite soft magnetisms, it is characterized in that, also can comprise SiO
2, Ta
2O
5, ZrO
2In one or more, every kind of content is 0.005～0.04wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310108830 CN1277278C (en) | 2003-11-21 | 2003-11-21 | Manganese zinc ferrite soft magnet and its manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310108830 CN1277278C (en) | 2003-11-21 | 2003-11-21 | Manganese zinc ferrite soft magnet and its manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1619719A true CN1619719A (en) | 2005-05-25 |
| CN1277278C CN1277278C (en) | 2006-09-27 |
Family
ID=34758747
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200310108830 Expired - Lifetime CN1277278C (en) | 2003-11-21 | 2003-11-21 | Manganese zinc ferrite soft magnet and its manufacturing method |
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| Country | Link |
|---|---|
| CN (1) | CN1277278C (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1300048C (en) * | 2005-08-04 | 2007-02-14 | 浙江大学 | High saturated magnetic flux density and low loss manganese-zinc ferrite material and its preparing method |
| CN100345226C (en) * | 2005-05-30 | 2007-10-24 | 苏州冠达磁业有限公司 | Ferrite magnet material of manganese-zinc, and Method for preparing high conductive ferrite of manganese-zinc from material |
| CN100441542C (en) * | 2005-08-05 | 2008-12-10 | 横店集团东磁有限公司 | MnZn powder ferrite material |
| CN102010192A (en) * | 2010-10-29 | 2011-04-13 | 宜宾金川电子有限责任公司 | Mangan zinc ferrite resintering process |
| CN103247405A (en) * | 2012-02-10 | 2013-08-14 | Tdk株式会社 | Ferrite core and transformer |
| CN107176830A (en) * | 2017-04-01 | 2017-09-19 | 浙江工业大学 | A kind of preparation method of high permeability MnZn ferrite |
| CN107200572A (en) * | 2017-05-08 | 2017-09-26 | 中国计量大学 | A kind of ferrite sintered methods of low magnetic permeability temperature coefficient MnZn |
-
2003
- 2003-11-21 CN CN 200310108830 patent/CN1277278C/en not_active Expired - Lifetime
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100345226C (en) * | 2005-05-30 | 2007-10-24 | 苏州冠达磁业有限公司 | Ferrite magnet material of manganese-zinc, and Method for preparing high conductive ferrite of manganese-zinc from material |
| CN1300048C (en) * | 2005-08-04 | 2007-02-14 | 浙江大学 | High saturated magnetic flux density and low loss manganese-zinc ferrite material and its preparing method |
| CN100441542C (en) * | 2005-08-05 | 2008-12-10 | 横店集团东磁有限公司 | MnZn powder ferrite material |
| CN102010192A (en) * | 2010-10-29 | 2011-04-13 | 宜宾金川电子有限责任公司 | Mangan zinc ferrite resintering process |
| CN102010192B (en) * | 2010-10-29 | 2013-01-23 | 宜宾金川电子有限责任公司 | Mangan zinc ferrite resintering process |
| CN103247405A (en) * | 2012-02-10 | 2013-08-14 | Tdk株式会社 | Ferrite core and transformer |
| CN103247405B (en) * | 2012-02-10 | 2016-04-27 | Tdk株式会社 | ferrite iron core and transformer |
| CN107176830A (en) * | 2017-04-01 | 2017-09-19 | 浙江工业大学 | A kind of preparation method of high permeability MnZn ferrite |
| CN107200572A (en) * | 2017-05-08 | 2017-09-26 | 中国计量大学 | A kind of ferrite sintered methods of low magnetic permeability temperature coefficient MnZn |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1277278C (en) | 2006-09-27 |
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Owner name: TDG HOLDING CO., LTD. Free format text: FORMER NAME: TIANTONG ELECTRONICS CO., LTD., ZHEJIANG |
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| CP01 | Change in the name or title of a patent holder |
Address after: 314412 No. 11, Guo Zhen, Haining, Zhejiang, Jianshe Road Patentee after: TDG HOLDING Co.,Ltd. Address before: 314412 No. 11, Guo Zhen, Haining, Zhejiang, Jianshe Road Patentee before: Zhejiang Tiantong Electronic Co.,Ltd. |
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Granted publication date: 20060927 |
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