CN1276897C - Manganese zinc ferrite soft magnetic sinitering method - Google Patents
Manganese zinc ferrite soft magnetic sinitering method Download PDFInfo
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- CN1276897C CN1276897C CN 200310109093 CN200310109093A CN1276897C CN 1276897 C CN1276897 C CN 1276897C CN 200310109093 CN200310109093 CN 200310109093 CN 200310109093 A CN200310109093 A CN 200310109093A CN 1276897 C CN1276897 C CN 1276897C
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- Prior art keywords
- temperature
- fall period
- constant temperature
- sintering method
- ferrite soft
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- 238000000034 method Methods 0.000 title claims abstract description 23
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 title abstract 2
- 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 abstract 2
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 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
- 238000009413 insulation Methods 0.000 claims abstract description 10
- 229910000859 α-Fe Inorganic materials 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 13
- 230000005389 magnetism Effects 0.000 claims description 6
- 238000011534 incubation Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 abstract 1
- 229910001308 Zinc ferrite Inorganic materials 0.000 abstract 1
- 230000000630 rising effect Effects 0.000 abstract 1
- WGEATSXPYVGFCC-UHFFFAOYSA-N zinc ferrite Chemical compound O=[Zn].O=[Fe]O[Fe]=O WGEATSXPYVGFCC-UHFFFAOYSA-N 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 7
- 238000010586 diagram Methods 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000000470 constituent Substances 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- 208000036366 Sensation of pressure Diseases 0.000 description 2
- 239000011230 binding agent Substances 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
- 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
- WJZHMLNIAZSFDO-UHFFFAOYSA-N manganese zinc Chemical class [Mn].[Zn] WJZHMLNIAZSFDO-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
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Abstract
The present invention discloses a sintering method for a manganese zinc ferrite soft magnet. At least one step for warming-up or insulation again is experienced during a temperature fall period in the sintering process. The start point temperature of the first time warming-up again is at least 100 DEG C lower than that of the anterior main constant insulation stage in a temperature fall period. The temperature of the step for insulation after the step for warming-up again is at least lower 50 DEG C than that of the main constant insulation stage, and oxygen content experiences a rising and a holding processes synchronously during the steps for warming-up again and insulation. The sintering method of the present invention make the adjustment of power consumption lowest temperature of mangan zinc ferrite simple, and power consumption is lower.
Description
Technical field
The present invention relates to a kind of ferrite in manganese zinc series soft magnetism sintering method, especially be fit to the sintering method of the power ferrite of making power transformer magnetic core.
Background technology
Mn-Zn ferrite is used widely on electronic equipments such as communication, robot calculator, televisor.The miniaturization of electronic equipment, flattening and high reliability all require ferrite soft magnetic to have reduce 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 magneticsubstance AEM (MMPA) provides is seen shown in Figure 1.
Temperature-fall period among Fig. 1, temperature are to descend continuously, and oxygen level 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 times, when causing adjusting temperature least in power-consuming, it is improper that Control for Oxygen Content has slightly, and power consumption will worsen.
For addressing the above problem, the applicant has submitted a patent application (application number 200310108830.8) on November 21st, 2003, a kind of technical scheme (abbreviation scheme 1) has been proposed in this application, it mainly passes through to experience the step of at least constant temperature insulation again during temperature-fall period, and the oxygen level during this step is also remained unchanged.
Summary of the invention
The objective of the invention is to solve the above-mentioned deficiency of existing public technology, a kind of obvious improved sintering method (abbreviation scheme 2) is provided, make the adjustment of Mn-Zn ferrite temperature least in power-consuming comparatively easy, and power consumption is lower.And scheme 2 is better than such scheme 1.
The present invention is achieved through the following technical solutions: the principal constituent of Ferrite Material is the Fe that is scaled 51.5～54mol%
2O
3, the MnO of 35～39mol% and the ZnO of 8～12mol% (each main composition sum is 100%); Minor component is 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
In ferrite of the present invention, if necessary, also can comprise SiO in the secondary composition
2, Ta
2O
5, ZrO
2In one or more, every kind content is 0.005～0.04wt%.
Principal constituent is mixed the back pre-burning, add minor component, 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 desired shape by mould, hair is bad at a special sintering process, can get the finished product of lower power consumption.
This sintering process experiences intensification, main constant temperature insulation, cooling three phases, experiences the step that at least once heats up again and be incubated during its temperature-fall period again, and the oxygen level during this step also experiences the step that rises and keep synchronously.
Based on above-mentioned characteristic optimization be, the temperature of the incubation step after low 100 ℃ at least of the temperature of the main constant temperature holding stage of the origin temp that heats up again the first time of described temperature-fall period before than temperature-fall period, the terminal temperature of this heavy heating step promptly heavily heat up is than low 50 ℃ at least of the temperature of described main constant temperature holding stage.
The following sintering process of the present invention's process:
A) with 50 ℃ to 300 ℃ heating rate per hour, be heated to 900 ℃;
B) with 50 ℃ to 200 ℃ heating rate 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 950 ℃ with 50 ℃ to 150 ℃ rate of cooling per hour, be preferably 1200 ℃ to 1000 ℃, and at least than b) in the temperature of main constant temperature holding stage low 100 ℃, at this moment, be warmed up to certain temperature of 1100 ℃ to 1250 ℃ with 100 ℃ to 300 ℃ speed per hour again, and at least than b) in the temperature of main constant temperature holding stage low 50 ℃, and constant temperature kept 20 to 60 minutes;
D) after above-mentioned heavy heating and heat preservation step finishes, continue to be cooled to 1100 ℃ with 150 ℃ to 300 ℃ speed per hour;
E) rate of cooling below 1100 ℃ is per hour 50 ℃ to 300 ℃.
The oxygen level of above process is regulated according to equilibrium oxygen partial pres-sure is theoretical.
If necessary, 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 successive or batch-wise, 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 a heavy heating and heat preservation step again at temperature-fall period, helping ferrite fully finishes in the redox reaction of this temperature spot, make the inside and outside oxidisability of ferrite finished product corresponding with the desired oxidisability of temperature least in power-consuming, afterwards, with the fast speeds cooling, the oxygen balance state that weighs the heating and heat preservation stage is remained to low temperature.Unlike the prior art, this heavy heating and heat preservation step has been arranged, other step oxygen level of temperature-fall period does not have big influence to power consumption and minimum temperature thereof, thereby reduces power consumption, realizes the easy adjusting to temperature least in power-consuming simultaneously.
Description of drawings
Fig. 1 is the synoptic diagram of typical ferrite sintered curve.
Fig. 2 is the sintering curre synoptic diagram of the embodiment of the invention 1.
Fig. 3 is the sintering curre synoptic diagram of the embodiment of the invention 2.
Fig. 4 is the sintering curre synoptic diagram of the embodiment of the invention 3.
Fig. 5 is the sintering curre synoptic 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 minor component.Principal constituent is mixed the back pre-burning, add minor component, 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 ℃ heating rate: 300 ℃/hour;
2. up to 1300 ℃ heating rate: 150 ℃/hour;
3. 1300 ℃ of insulations 5 hours;
4. 1300 ℃ to 1100 ℃ rate of cooling: 100 ℃/hour;
5. be warmed up to 1200 ℃ with 300 ℃/hour heating rate again, and constant temperature kept 30 minutes;
6. 1200 ℃ to 600 ℃ rate of cooling: 200 ℃/hour;
7. the rate of cooling below 600 ℃: 150 ℃/hour;
Oxygen level is regulated according to equilibrium oxygen partial pres-sure is theoretical in this example, and how difference from prior art has been heavy heating and heat preservation step 5, and the oxygen level during this step also experiences the process that rises and remain unchanged synchronously.
Embodiment 2: temperature rate is identical with embodiment 1 with temperature distribution, moves to low temperature in order to make temperature least in power-consuming, and oxygen level integral body is lower than embodiment 1, as shown in Figure 3 curve.
Implement 3: temperature rate is also identical with embodiment 1 with temperature distribution, moves to high temperature in order to make temperature least in power-consuming, and oxygen level integral body is than embodiment 1 height, curve as shown in Figure 4.
Comparative example: be that sintering process as shown in Figure 5 according to typical sintering scheme sintering.
1. up to 900 ℃ heating rate: 300 ℃/hour;
2. up to 1300 ℃ heating rate: 150 ℃/hour;
3. kept 5 hours at 1300 ℃;
4. 1300 ℃ to 1100 ℃ rate of cooling: 100 ℃/hour;
5. 1100 ℃ to 600 ℃ rate of cooling: 200 ℃/hour;
6. the rate of cooling below 600 ℃: 150 ℃/hour;
The oxygen level of each step of comparative example is identical with the oxygen level of embodiment 1 corresponding temperature.
After being to be cooled to 1100 ℃, the key distinction of comparative example and embodiment 1,2,3 lacked heavily intensification, an incubation step.
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 |
| | 610 | 345 | 302 | 294 | 329 | 396 |
| Embodiment 2 | 579 | 324 | 280 | 299 | 340 | 410 |
| Embodiment 3 | 638 | 380 | 351 | 322 | 312 | 373 |
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 disadvantageous effect of minimum temperature position in the adjustment process.
The embodiment of the last patent application (scheme 1) that the sample performance of the embodiment of the invention and applicant have been proposed compares, and power consumption all has further reduction.
Claims (4)
1, a kind of Mn-Zn ferrite soft magnetism sintering method, its sintering process experience heats up, main constant temperature is incubated, the cooling three phases, it is characterized in that: experience the step that at least once heats up again and be incubated during the described temperature-fall period again, and the oxygen level during this step also experiences the step that rises and keep synchronously.
2, Mn-Zn ferrite soft magnetism sintering method as claimed in claim 1, it is characterized in that, low 100 ℃ at least of the temperature of the main constant temperature holding stage of the origin temp that heats up again first of described temperature-fall period before than temperature-fall period, the temperature of the incubation step after the described heavy intensification is than low 50 ℃ at least of the temperature of described main constant temperature holding stage.
3, Mn-Zn ferrite soft magnetism sintering method as claimed in claim 2 is characterized in that, the temperature of described main constant temperature insulation is between 1250 ℃ and 1360 ℃, and the constant temperature soaking time is 3 to 5 hours; Be cooled to certain temperature between 1300 ℃ to 950 ℃ with 50 ℃ to 150 ℃ rate of cooling per hour then, be warmed up to certain temperature of 1100 ℃ to 1250 ℃ with 100 ℃ to 300 ℃ speed per hour this moment again, and constant temperature kept 20 to 60 minutes.
4, Mn-Zn ferrite soft magnetism sintering method as claimed in claim 3 is characterized in that, during temperature-fall period, the described origin temp that heats up again is between 1200 ℃ to 1000 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310109093 CN1276897C (en) | 2003-12-01 | 2003-12-01 | Manganese zinc ferrite soft magnetic sinitering method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310109093 CN1276897C (en) | 2003-12-01 | 2003-12-01 | Manganese zinc ferrite soft magnetic sinitering method |
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| CN1623953A CN1623953A (en) | 2005-06-08 |
| CN1276897C true CN1276897C (en) | 2006-09-27 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100466114C (en) * | 2006-06-14 | 2009-03-04 | 横店集团东磁有限公司 | Sintering method for high saturated flux density MnZn ferrite |
| CN101121547B (en) * | 2006-08-08 | 2011-03-30 | 上海依林磁业有限公司 | Method for sintering manganese-zinc-ferrite with high cutoff frequency and super-high magnetic conductivity |
| CN101367645B (en) * | 2008-08-06 | 2011-08-10 | 中国地质大学（北京） | Novel method for preparing ferrite ceramic soft magnetic material |
| CN101665362B (en) * | 2009-08-31 | 2013-05-01 | 广西冶金研究院 | Synthesis method of Mn-Zn ferrite crystal |
| CN101817679A (en) * | 2010-05-12 | 2010-09-01 | 宜宾金川电子有限责任公司 | Manganese-zinc power ferrite sintering process |
| CN111777419B (en) * | 2020-05-29 | 2022-05-31 | 天长市烁源磁电有限公司 | Sintering process of magnetic ferrite core |
| CN114656254A (en) * | 2022-04-27 | 2022-06-24 | 湖北华磁电子科技有限公司 | Preparation method of soft magnetic ferrite material |
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2003
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Owner name: TDG HOLDING CO., LTD. Free format text: FORMER NAME: TIANTONG ELECTRONICS CO., LTD., ZHEJIANG |
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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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