CN104628371A - Manganese zinc soft magnetic ferrite material and preparation method thereof - Google Patents
Manganese zinc soft magnetic ferrite material and preparation method thereof Download PDFInfo
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- CN104628371A CN104628371A CN201410855445.8A CN201410855445A CN104628371A CN 104628371 A CN104628371 A CN 104628371A CN 201410855445 A CN201410855445 A CN 201410855445A CN 104628371 A CN104628371 A CN 104628371A
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Abstract
The invention discloses a manganese zinc soft magnetic ferrite material with high initial permeability and high Curie temperature and a preparation method thereof. The manganese zinc soft magnetic ferrite material comprises a main component and an auxiliary component, wherein the main component comprises 51-54 mol% of ferric oxide, 20-26 mol% of zinc oxide and the balance of manganese oxide; the auxiliary component according to the total weight of the main component comprises: 50-300 ppm of calcium oxide, 10-800 ppm of bismuth oxide, 20-1500 ppm of titanium dioxide and 10-500 ppm of molybdenum oxide. The preparation method comprises the following steps: (1) mixing; (2) pre-sintering; (3) grinding; (4) spray granulating; (5) forming; (6) sintering. The manganese zinc soft magnetic ferrite material has the advantages of simple preparation process, low energy consumption and strong raw material adaptability and meets the current requirements of the fields such as automobiles, new energy resources and electronic information on the miniaturization, thinness and high reliability of the components.
Description
Technical field
The present invention relates to that soft magnetism is high leads material correlative technology field, refer in particular to a kind of Mn-Zn soft magnetic ferrite and preparation method thereof.
Background technology
Along with developing rapidly and MEMS (Micro Electronical Mechanical System of the high frequency of electronic devices and components, high speed and integrated circuit technique, MEMS (micro electro mechanical system)) progress of technology, the overall power density of electronic devices and components increases substantially and its physical size is more and more less, heat flow density also increases thereupon, under therefore a lot of electronic devices and components all can be operated in higher temperature environment.This just requires more and more higher to the hot properties of material in these electronic devices and components, and especially those are applied in the components and parts of automobile and new energy field, and its Curie temperature to material requires higher.
Mn-Zn ferrite soft magnetic materials have the advantages such as high initial permeability, good frequency response characteristic, low loss and in widespread attention and application.MnZn ferrite material manufactures magnetic core of transformer, noise filter, local area network isolating transformer and digital network magnetic core of transformer in a large number.Magnetic core is mainly applied to broadband and pulse transformer, reactance coil and DSL transformer.Along with the high speed development in the fields such as automotive electronics, new forms of energy, network service, aerospace and satellite communications, new higher requirement is proposed to manganese zinc ferrite material.
The Mn-Zn soft magnetic ferrite of conventional high initial magnetoconductivity, between initial permeability μ i and Curie temperature Tc, also exists contradiction.Such as: the material of μ i=15000, Curie temperature Tc is generally 100-110 DEG C.This kind of material can not to have met the application of automotive electronics, network service and space flight and aviation etc. due to Curie temperature lower than working temperature.And on the other hand, from the requirement in components and parts miniaturization direction, high-conductive manganese-zinc soft magnetic ferrite will have higher initial permeability μ i.
At present, the material (being called for short " R15K MnZn Ferrite Material " below) of what the MnZn Ferrite Material magnetic permeability of widespread use on market was the highest is exactly initial permeability about 15000, this type of material Curie temperature is general all between 100 ~ 110 DEG C.And the working temperature of current each Application Areas is more and more higher, the temperature magnetic of existing R15K Ferrite Material more than 120 DEG C can just lose efficacy.The material of what domestic and international prior art related to have high-curie temperature mainly pays close attention to high-curie temperature and reduce power consumption, so initial permeability is usually lower, and only about 5000, and the present invention conceive the R15K soft magnetic ferrite difference in application related to.The technique means of the high magnetic conductance low-loss material that prior art provides normally adopts the ratio of adjustment ferric oxide, zinc oxide and manganese oxide, with the oxide compound changing secondary interpolation, such as, two 5,000 ferrite in manganese zinc series of the high-curie temperature low-loss that Chinese invention patent CN200510033614.0 provides, although its Curie temperature can reach more than 210 DEG C, its magnetic permeability only can arrive about 5000; The high-curie temperature material that Chinese invention patent ZL200910308782.4 provides, although Curie temperature can reach more than 150 DEG C, initial permeability only has about 10000.
Summary of the invention
There is above-mentioned deficiency to overcome in prior art in the present invention, provides a kind of high initial magnetoconductivity and Mn-Zn soft magnetic ferrite of high-curie temperature and preparation method thereof.
To achieve these goals, the present invention is by the following technical solutions:
A kind of Mn-Zn soft magnetic ferrite, comprise main composition and auxiliary ingredients, described main composition consists of: ferric oxide is 51 ~ 54mol%, zinc oxide is 20 ~ 26mol%, all the other are manganese oxide; The described auxiliary ingredients by main composition total weight comprises: calcium oxide is 50 ~ 300ppm, bismuth oxide is 10 ~ 800ppm, titanium dioxide is 20 ~ 1500ppm and molybdenum oxide is 10 ~ 500ppm.
In addition, present invention also offers the preparation method of above-mentioned Mn-Zn soft magnetic ferrite, comprise the steps: (1) combination treatment; (2) preheating; (3) sanded; (4) mist projection granulating; (5) forming processes; (6) sintering processes.This preparation method has that process is simple, energy consumption is low and the adaptable advantage of starting material.
As preferably, in step (1), the concrete operations technique of combination treatment is as follows: by the main composition of the raw material combination treatment 20-60 minute in ball mill taken by formula rate.
As preferably, in step (2), the concrete operations technique of preheating is as follows: by the material after combination treatment in 700 ~ 1000 DEG C of preheating 60 ~ 180 minutes.
As preferably, in step (3), the concrete operations technique of sanded is as follows: the powder that preheating obtains adds the auxiliary ingredients and other additives that take in proportion, milled processed 60-140 minute.
As preferably, in step (3), after sanded, control material particle size D50 between 1.0 ~ 1.6 μm.
As preferably, in step (6), the concrete operations technique of sintering processes is as follows: the blank that forming processes obtains is the N of 0.005% ~ 21% in oxygen level
2carry out sintering processes in protective atmosphere, wherein said sintering temperature is 1350 ~ 1500 DEG C, and sintering total time is 15 ~ 35 hours, and after sintering processes, nitrogen protection borehole cooling can obtain desired Mn-Zn soft magnetic ferrite.
As preferably, the MnZn ferrite material of preparation is when room temperature, 10kHz, and initial permeability μ i is between 13000-18000, and the Curie temperature Tc of this MnZn ferrite material is more than 130 DEG C.High performance like this Mn-Zn soft magnetic ferrite can meet the requirement of the fields such as current automobile, new forms of energy and electronic information to components and parts miniaturization, slimming and height reliability.
The invention has the beneficial effects as follows: preparation method has that process is simple, energy consumption is low and the adaptable advantage of starting material; Mn-Zn soft magnetic ferrite meets the requirement of the fields such as current automobile, new forms of energy and electronic information to components and parts miniaturization, slimming and height reliability.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
In the present invention, if not refer in particular to, all parts, per-cent are weight unit, and all equipment and raw material etc. all can be buied from market or the industry is conventional.
Embodiment 1:
Be Fe proportioning
2o
3: three kinds of main composition material of 51mol%, ZnO:20mol%, MnO:29mol% weigh, in ball mill, mix 60 minutes, and then pre-burning 2 hours at 700 DEG C, adds ancillary component CaO (50ppm), the Bi by main composition total weight
2o
3(350ppm), TiO
2(600ppm) and MoO
3(200ppm), obtain by the sanded of 140 minutes the material that D50 is 1.10 μm, then carry out mist projection granulating, obtain Mn-Zn soft magnetic ferrite powder.
Then with full-automatic dry press, powder pressing is become 10, the blank sample of H25 × 15 × 8, at most high sintering temperature is 1450 DEG C, oxygen level is the N of 12%
2sinter 28 hours in protective atmosphere, finally cooling obtains finished product.Sample number into spectrum is 1.Test data gets 10 sample calculating mean values, and result is as shown in table 1.
Embodiment 2:
Be Fe proportioning
2o
3: three kinds of main composition material of 53.5mol%, ZnO:25.5mol%, MnO:21mol% weigh, put into ball mill mixing 40 minutes, then 900 DEG C of pre-burnings 2 hours, ancillary component CaO (200ppm), the Bi by main composition total weight is added
2o
3(200ppm), TiO
2(1500ppm) and MoO
3(400ppm), obtain by the sanded of 100 minutes the material that D50 is 1.55 μm, then mist projection granulating, obtain Mn-Zn soft magnetic ferrite powder.
Then with full-automatic dry press, powder pressing is become 10, the blank sample of H25 × 15 × 8, at most high sintering temperature is 1480 DEG C, oxygen level is the N of 5%
2sinter 18 hours in protective atmosphere, finally cooling obtains finished product.Sample number into spectrum is 2.Test data gets 10 sample calculating mean values, and result is as shown in table 1.
Embodiment 3:
Be Fe proportioning
2o
3: three kinds of main composition material of 52mol%, ZnO:22.5mol%, MnO:25.5mol% weigh, put into ball mill mixing 30 minutes, then 700 DEG C of pre-burnings 3 hours, ancillary component CaO (300ppm), the Bi by main composition total weight is added
2o
3(700ppm), TiO
2(1000ppm) and MoO
3(100ppm), obtain by the sanded of 80 minutes the material that D50 is 1.3 μm, then mist projection granulating, obtain MnZn soft magnet ferrite powder.
Then with full-automatic dry press, powder pressing is become 10, the blank sample of H25 × 15 × 8, at most high sintering temperature is 1370 DEG C, oxygen level is the N of 18%
2sinter 30 hours in protective atmosphere, finally cooling obtains finished product.Sample number into spectrum is 3.Test data gets 10 sample calculating mean values, and result is as shown in table 1.
Comparative example 1
Be Fe proportioning
2o
3: three kinds of main composition material of 56.0mol%, ZnO:15.5mol%, MnO:28.5mol% weigh, put into ball mill mixing 35 minutes, then 850 DEG C of pre-burnings 2 hours, ancillary component CaO (50ppm), the Bi by three kinds of main composition total weight is added
2o
3(350ppm), MoO
3(150ppm) and TiO
2(100ppm), obtain by the sanded of 2 hours the material that D50 is 1.1 μm, then mist projection granulating, obtain Mn-Zn soft magnetic ferrite powder.
Then with full-automatic dry press, powder pressing is become the blank sample of H25 × 15 × 8, at sintering temperature is 1370 DEG C, oxygen level is the N of 4.5%
2sinter 20 hours in protective atmosphere, finally cooling obtains finished product.Sample number into spectrum is 4.The test data often organized gets 10 sample calculating mean values, and result is as shown in table 1.
Table 1 different preparation method MnZn Ferrite Material magnetic property contrast table
| Sample number into spectrum | Initial permeability μ i | Curie temperature Tc |
| 1 | 13500 | 142℃ |
| 2 | 15900 | 131℃ |
| 3 | 15200 | 135℃ |
| 4 | 11000 | 195℃ |
Claims (8)
1. a Mn-Zn soft magnetic ferrite, is characterized in that, comprises main composition and auxiliary ingredients, and described main composition consists of: ferric oxide is 51 ~ 54mol%, zinc oxide is 20 ~ 26mol%, all the other are manganese oxide; The described auxiliary ingredients by main composition total weight comprises: calcium oxide is 50 ~ 300ppm, bismuth oxide is 10 ~ 800ppm, titanium dioxide is 20 ~ 1500ppm and molybdenum oxide is 10 ~ 500ppm.
2. a preparation method for Mn-Zn soft magnetic ferrite as claimed in claim 1, is characterized in that, comprises the steps:
(1) combination treatment;
(2) preheating;
(3) sanded;
(4) mist projection granulating;
(5) forming processes;
(6) sintering processes.
3. the preparation method of Mn-Zn soft magnetic ferrite according to claim 2, it is characterized in that, in step (1), the concrete operations technique of combination treatment is as follows: by the main composition of the raw material combination treatment 20-60 minute in ball mill taken by formula rate.
4. the preparation method of Mn-Zn soft magnetic ferrite according to claim 2, it is characterized in that, in step (2), the concrete operations technique of preheating is as follows: by the material after combination treatment in 700 ~ 1000 DEG C of preheating 60 ~ 180 minutes.
5. the preparation method of Mn-Zn soft magnetic ferrite according to claim 2, it is characterized in that, in step (3), the concrete operations technique of sanded is as follows: the powder that preheating obtains adds the auxiliary ingredients and other additives that take in proportion, milled processed 60-140 minute.
6. the preparation method of Mn-Zn soft magnetic ferrite according to claim 5, is characterized in that, in step (3), after sanded, controls material particle size D50 between 1.0 ~ 1.6 μm.
7. the preparation method of Mn-Zn soft magnetic ferrite according to claim 2, is characterized in that, in step (6), the concrete operations technique of sintering processes is as follows: the blank that forming processes obtains is the N of 0.005% ~ 21% in oxygen level
2carry out sintering processes in protective atmosphere, wherein said sintering temperature is 1350 ~ 1500 DEG C, and sintering total time is 15 ~ 35 hours, and after sintering processes, nitrogen protection borehole cooling can obtain desired Mn-Zn soft magnetic ferrite.
8. the preparation method of Mn-Zn soft magnetic ferrite according to claim 2, it is characterized in that, the MnZn ferrite material of preparation is when room temperature, 10kHz, and initial permeability μ i is between 13000-18000, and the Curie temperature Tc of this MnZn ferrite material is more than 130 DEG C.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105110785A (en) * | 2015-09-21 | 2015-12-02 | 无锡清杨机械制造有限公司 | High-frequency low-loss MnZn ferrite, and preparation method thereof |
| CN105541316A (en) * | 2015-12-16 | 2016-05-04 | 横店集团东磁股份有限公司 | Manganese zinc ferrite material for resisting EMI and preparation method thereof |
| CN105819847A (en) * | 2016-03-16 | 2016-08-03 | 横店集团东磁股份有限公司 | MnZn ferrite material with high Bs and high ui and preparation method thereof |
| CN107098693A (en) * | 2017-04-28 | 2017-08-29 | 苏州冠达磁业有限公司 | A kind of anti-interference manganese-zinc ferrite of high frequency and preparation method thereof |
| CN107216137A (en) * | 2017-04-28 | 2017-09-29 | 苏州冠达磁业有限公司 | The high-curie temperature GH10H of resistance to electric current manganese-zinc ferrites and preparation method thereof |
| CN107954706A (en) * | 2017-12-08 | 2018-04-24 | 广东风华高新科技股份有限公司 | A kind of high magnetic conductivity soft-magnetic ferrite material and preparation method thereof |
| CN115448714A (en) * | 2022-10-12 | 2022-12-09 | 上海宝钢磁业有限公司 | Manganese-zinc ferrite material, preparation method and application |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105110785A (en) * | 2015-09-21 | 2015-12-02 | 无锡清杨机械制造有限公司 | High-frequency low-loss MnZn ferrite, and preparation method thereof |
| CN105541316A (en) * | 2015-12-16 | 2016-05-04 | 横店集团东磁股份有限公司 | Manganese zinc ferrite material for resisting EMI and preparation method thereof |
| CN105541316B (en) * | 2015-12-16 | 2017-12-22 | 横店集团东磁股份有限公司 | A kind of anti-EMI filter MnZn ferrite material and preparation method thereof |
| CN105819847A (en) * | 2016-03-16 | 2016-08-03 | 横店集团东磁股份有限公司 | MnZn ferrite material with high Bs and high ui and preparation method thereof |
| CN107098693A (en) * | 2017-04-28 | 2017-08-29 | 苏州冠达磁业有限公司 | A kind of anti-interference manganese-zinc ferrite of high frequency and preparation method thereof |
| CN107216137A (en) * | 2017-04-28 | 2017-09-29 | 苏州冠达磁业有限公司 | The high-curie temperature GH10H of resistance to electric current manganese-zinc ferrites and preparation method thereof |
| CN107098693B (en) * | 2017-04-28 | 2021-01-19 | 苏州冠达磁业有限公司 | High-frequency anti-interference manganese-zinc ferrite and preparation method thereof |
| CN107954706A (en) * | 2017-12-08 | 2018-04-24 | 广东风华高新科技股份有限公司 | A kind of high magnetic conductivity soft-magnetic ferrite material and preparation method thereof |
| CN107954706B (en) * | 2017-12-08 | 2020-05-19 | 广东风华高新科技股份有限公司 | High-permeability soft magnetic ferrite material and preparation method thereof |
| CN115448714A (en) * | 2022-10-12 | 2022-12-09 | 上海宝钢磁业有限公司 | Manganese-zinc ferrite material, preparation method and application |
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