CN104177075A - Heat-shock-resistant soft magnetic ferrite material and preparation method thereof - Google Patents
Heat-shock-resistant soft magnetic ferrite material and preparation method thereof Download PDFInfo
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- CN104177075A CN104177075A CN201410399488.XA CN201410399488A CN104177075A CN 104177075 A CN104177075 A CN 104177075A CN 201410399488 A CN201410399488 A CN 201410399488A CN 104177075 A CN104177075 A CN 104177075A
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- soft magnetic
- controlled
- sintering
- magnetic ferrite
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Abstract
The invention discloses a heat-shock-resistant soft magnetic ferrite material and a preparation method thereof. The heat-shock-resistant soft magnetic ferrite material comprises the following components in percentage by weight according to each reference substance: 62.3-77% of Fe2O3, 10.5-16.55% of NiO, 8.35-12.55% of ZnO, 3.5-5.5% of CuO, 0.15-0.95% of Li2CO3, 0.1-0.95% of Bi2O3, 0.25-0.55% of nano Al2O3 and 0.15-0.65% of nano SiO2. The heat-shock-resistant soft magnetic ferrite material is prepared by adopting an oxide method and is sintered under a certain condition. A sintered product has relatively good electromagnetic performance and excellent heat shock resistance, and is suitable for the requirements of a winding power inductor on soft magnetic materials.
Description
Technical field
The present invention relates to a kind of heat shock resistance soft magnetic ferrite and preparation method thereof.
Background technology
Winding power inductance is generally divided into the power inductance and the SMD power inductance that connect PIN formula.The power inductance that connects PIN formula is plugged PIN pin often on magnetic core; SMD power inductance plates silver electrode often on the end face of magnetic core.This two classes power inductance often needs could be induction soldering on pcb board by the high temperature scolding tin of 400 DEG C of left and right, and this has just proposed higher requirement to the heat-resistant impact ability of soft magnetic ferrite.
For the requirement of the heat shock resistance of corresponding winding power inductance, on the basis of electromagnetic performance that ensures material, high heat shock resistance soft magnetic ferrite corresponding to exploitation is very necessary.
The patent of more existing relevant heat shock resistance soft magnetic ferrites and preparation method thereof at home, specific as follows:
(1) publication number is CN101684044, open day is 2010.03.31, the Chinese patent that denomination of invention is " MnZnLi based ferrite " discloses a kind of novel MnZnLi based ferrite, it has the temperature dependent performance of high saturation magnetic flux density and good reduction magnetic loss (core loss) value, can also realize the raising of bending strength, thereby further improve the output of product, and magnetic core also has good resistance to sudden heating.This MnZnLi based ferrite, contains with Fe as principal constituent
2o
3conversion count the ferric oxide of 54.0～58.0mol%, with ZnO convert count the zinc oxide of 3.0～10.0mol%, with LiO
0.5conversion is counted the Lithium Oxide 98min, surplus (converting taking MnO) of 0.3～1.5mol% as manganese oxide, contains the Co that counts 500～2000 ppm by weight with respect to described principal constituent with CoO conversion as minor component.
(2) publication number is CN102276245A, open day is 2011.12.14, the Chinese patent that denomination of invention is " a kind of high-temperature-resistant soldering tin Ni-Zn soft magnetic ferrite material " discloses a kind of Ni-Zn soft magnetic ferrite material and preparation method thereof, count by molar, a kind of high-temperature-resistant soldering tin Ni-Zn soft magnetic ferrite material, count by molar ferric oxide Fe
2o
345～50mol%, zinc oxide ZnO26～32mol%, nickel protoxide NiO17～21mol%, cupric oxide CuO4～8mol%, while are in this main formula, hundred parts of ratio meters by weight, also add the auxiliary material A of 0.2～0.5Wt%, the auxiliary material B of 0.1～0.2Wt%, described auxiliary material A is Bi
2o
3, SiO
2, Ta
2o
5in one or both, auxiliary material B is TiO
2, V
2o
5, Nb
2o
5in one or more.The Ni-Zn soft magnetic ferrite material of gained has high frequency, high magnetic permeability, high Bs, high TC characteristic.
(3) publication number is CN102432279A, open day is 2012.05.02, and the Chinese patent that denomination of invention is " a kind of high-strength thermal-shock-resistant nickel zinc ferrite and preparation method thereof " discloses applicable high-strength thermal-shock-resistant nickel zinc ferrite of a kind of power inductance and preparation method thereof.This nickel-zinc ferrite principal constituent is calculated as with oxide compound: Fe
2o
345～52mol%, NiO20～29mol%, ZnO20～30mol%, CuO3～6.5mol%, ancillary component is: CaCO
30.2～0.5wt%, Co
2o
30.01～0.09wt%, V
2o
50.05～0.19wt%, SiO
20.8～1.5wt%.The preparation of employing conventional ceramic technique, sintering under certain condition.After sintering, the crystallization grain-size of goods is 10～20 μ m, crystal boundary distinctness, and goods have high strength and the higher feature of heat shock resistance temperature, adapt to the high strength of miniaturization to material and the double requirements of heat shock resistance of power inductance.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides a kind of heat shock resistance soft magnetic ferrite and preparation method thereof, this material has the feature of good electromagnetic performance and good thermal shock resistance, adapts to the requirement of winding power inductance to soft magnetic materials.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of heat shock resistance soft magnetic ferrite, its composition is as follows in the content of standard substance separately:
Fe
2o
362.3～77wt%, NiO10.5～16.55wt%, ZnO8.35～12.55wt%, CuO3.5～5.5wt%, Li
2cO
30.15～0.95wt%, Bi
2o
30.1～0.95wt%, nanometer Al
2o
30.25～0.55wt%, nanometer SiO
20.15～0.65wt%.
Described Fe
2o
3, NiO, ZnO, CuO, Li
2cO
3and Bi
2o
3median size be 1.0～2.0 μ m, nanometer Al
2o
3with nanometer SiO
2median size be 30～50nm.
Its preferred component is taking the content of standard substance separately as Fe
2o
370.12wt%, NiO13.50wt%, ZnO10.50wt%, CuO4.00wt%, Li
2cO
30.55wt%, Bi
2o
30.63wt%, nanometer Al
2o
30.35wt%, nanometer SiO
20.35wt%.
A preparation method for heat shock resistance soft magnetic ferrite, comprises that mixing, spraying are dry, pre-burning, pulverizing, mist projection granulating, compacting and sintering step successively, wherein:
(1) mix: by carrying out wet-mixed after composition proportion batching, use deionized water as solvent, mixing time is 80～90 minutes;
(2) spraying is dry: the slurry mixing is dried in spray tower, and spray tower inlet temperature is controlled at 200 ± 10 DEG C, and spray tower air outlet temperature is controlled at 100 ± 10 DEG C;
(3) pre-burning: dried spraying material is carried out to pre-burning in rotary oven, and calcined temperature is controlled at 800 ± 20 DEG C, and the pre-burning time is 160～180 minutes, and pre-burning atmosphere is air;
(4) pulverize: the Preburning material obtaining in upper step pre-burning carries out wet pulverization, use deionized water as solvent, grinding time is 100～120 minutes, and after pulverizing, slip particle diameter is controlled at 1.0～1.5 μ m;
(5) mist projection granulating: add 13～16% the PVA that is equivalent to material weight in the slurry of upper step, be dried and obtain particulate material in spray tower, spray tower inlet temperature is controlled at 200 ± 10 DEG C, and spray tower air outlet temperature is controlled at 100 ± 10 DEG C;
(6) compacting: adopt powder former compacting to obtain blank the particulate material of upper step, the pressed density of blank is controlled at (3.1 ± 0.15) g/cm
3;
(7) sintering: carry out sintering in chamber type electric resistance furnace, sintering temperature is controlled at 1000 DEG C～1020 DEG C, is incubated 120～180 minutes, and sintering atmosphere is air, cools to room temperature with the furnace after sintering finishes.
The invention has the beneficial effects as follows: the present invention adopts rational main formula, adjust magnetic permeability and the Curie temperature of material by adjusting the content of NiO, ZnO and CuO; By adding nanometer Al
2o
3with nanometer SiO
2combination increases the thickness of crystal boundary, improves the resistivity of crystal boundary; Add a certain amount of Li
2cO
3and Bi
2o
3promote grain growing, form a certain amount of void content, thereby obtain good thermal shock resistance.This material has the feature of good electromagnetic performance and good thermal shock resistance, adapts to the requirement of winding power inductance.
The performance index of material are as follows:
(1) initial permeability μ
i: 200 (1 ± 20%);
(2) Curie temperature Tc: >=200 DEG C;
(3) scolding tin fraction defective (after 400 DEG C of thermal shockings): 0%, at 100 times of optical microphotograph Microscopic observation flawlesses.
Brief description of the drawings
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is the micro-structure diagram of specific embodiment of the present invention and comparative example.
Embodiment
According to specific embodiment, the present invention is described below, but the present invention is not limited to these embodiment.
A kind of heat shock resistance soft magnetic ferrite, its composition is as follows in the content of standard substance separately:
Fe
2o
362.3～77wt%, NiO10.5～16.55wt%, ZnO8.35～12.55wt%, CuO3.5～5.5wt%, Li
2cO
30.15～0.95wt%, Bi
2o
30.1～0.95wt%, nanometer Al
2o
30.25～0.55wt%, nanometer SiO
20.15～0.65wt%.
Wherein, described Fe
2o
3, NiO, ZnO, CuO, Li
2cO
3and Bi
2o
3median size be 1.0～2.0 μ m, nanometer Al
2o
3with nanometer SiO
2median size be 30～50nm.
For the preparation of a method for above-mentioned heat shock resistance soft magnetic ferrite, comprise successively that mixing, spraying are dry, pre-burning, pulverizing, mist projection granulating, compacting and sintering step, wherein:
(1) mix: by carrying out wet-mixed after composition proportion batching, use deionized water as solvent, mixing time is 80～90 minutes;
(2) spraying is dry: the slurry mixing is dried in spray tower, and spray tower inlet temperature is controlled at 200 ± 10 DEG C, and spray tower air outlet temperature is controlled at 100 ± 10 DEG C;
(3) pre-burning: dried spraying material is carried out to pre-burning in rotary oven, and calcined temperature is controlled at 800 ± 20 DEG C, and the pre-burning time is 160～180 minutes, and pre-burning atmosphere is air;
(4) pulverize: the Preburning material obtaining in upper step pre-burning carries out wet pulverization, use deionized water as solvent, grinding time is 100～120 minutes, and after pulverizing, slip particle diameter is controlled at 1.0～1.5 μ m;
(5) mist projection granulating: add 13～16% the PVA that is equivalent to material weight in the slurry of upper step, be dried and obtain particulate material in spray tower, spray tower inlet temperature is controlled at 200 ± 10 DEG C, and spray tower air outlet temperature is controlled at 100 ± 10 DEG C;
(6) compacting: adopt powder former compacting to obtain blank the particulate material of upper step, the pressed density of blank is controlled at (3.1 ± 0.15) g/cm
3;
(7) sintering: carry out sintering in chamber type electric resistance furnace, sintering temperature is controlled at 1000 DEG C～1020 DEG C, is incubated 120～180 minutes, and sintering atmosphere is air, cools to room temperature with the furnace after sintering finishes.
Make described magnet ring sample (T25 × 15 × 7.5) and square center pillar I shape sample (DR8 × 10) by above operation.
Magnet ring after sintering and I shape sample are tested respectively and evaluated.Under number of turn N=20Ts condition, with the initial permeability μ of HP-4285 type LCR tester test magnet ring sample
i, coordinate high low-temperature bake oven to test the Curie temperature Tc of sample; Use the pendulum face of one end of I shape sample to be immersed in completely in the tin soldering liquid of 400 DEG C, kept for 3 seconds, then take out cooling after, have flawless at 100 times of optical microphotograph Microscopic observations.
The composition proportion of table 1 embodiment and comparative example
The magnetic property of table 2 embodiment and comparative example
Table 1 is listed moiety and the part by weight of multiple embodiment of the present invention and comparative example, table 2 has been listed performance and the evaluation of embodiment and comparative example, as can be seen from Table 2, embodiments of the invention and comparative example are compared, ensureing that on the magnetic permeability of material and the basis of Curie temperature, the present invention has improved the heat-resistant impact ability of material effectively.As shown in Figure 1, the grain-size of embodiment 1 is 60～100 μ m, but pore is more very even; The grain-size of comparative example 1 is 20～30 μ m, and pore is less and inhomogeneous.In material, generating the inner pore uniformly of the grain boundary layer of high resistivity and crystal grain should be the major cause that material has good heat-resistant impact ability, therefore the preferred composition of the present invention is taking the content of standard substance separately as Fe
2o
370.12wt%, NiO13.50wt%, ZnO10.50wt%, CuO4.00wt%, Li
2cO
30.55wt%, Bi
2o
30.63wt%, nanometer Al
2o
30.35wt%, nanometer SiO
20.35wt%; Material of the present invention can meet the requirement of the heat shock resistance of winding power inductance to soft magnetic materials.
The performance index of material are as follows:
(1) initial permeability μ
i: 200 (1 ± 20%);
(2) Curie temperature Tc: >=200 DEG C;
(3) scolding tin fraction defective (after 400 DEG C of thermal shockings): 0%, at 100 times of optical microphotograph Microscopic observation flawlesses.
Specific embodiment described in the invention is only to the present invention's explanation for example, the expert of correlative technology field or technician can make amendment in various degree to described specific embodiment, supplementary or alternative by similar mode, but can't depart from spirit of the present invention or surmount the defined scope of appended claims.
Claims (4)
1. a heat shock resistance soft magnetic ferrite, is characterized in that: its composition is as follows in the content of standard substance separately:
Fe
2o
362.3～77wt%, NiO10.5～16.55wt%, ZnO8.35～12.55wt%, CuO3.5～5.5wt%, Li
2cO
30.15～0.95wt%, Bi
2o
30.1～0.95wt%, nanometer Al
2o
30.25～0.55wt%, nanometer SiO
20.15～0.65wt%.
2. a kind of heat shock resistance soft magnetic ferrite according to claim 1, is characterized in that: described Fe
2o
3, NiO, ZnO, CuO, Li
2cO
3and Bi
2o
3median size be 1.0～2.0 μ m, nanometer Al
2o
3with nanometer SiO
2median size be 30～50nm.
3. a kind of heat shock resistance soft magnetic ferrite according to claim 1, is characterized in that: its composition is taking the content of standard substance separately as Fe
2o
370.12wt%, NiO13.50wt%, ZnO10.50wt%, CuO4.00wt%, Li
2cO
30.55wt%, Bi
2o
30.63wt%, nanometer Al
2o
30.35wt%, nanometer SiO
20.35wt%.
4. a preparation method for the heat shock resistance soft magnetic ferrite as described in claim 1～3 any one, is characterized in that: comprise successively that mixing, spraying are dry, pre-burning, pulverizing, mist projection granulating, compacting and sintering step, wherein:
(1) mix: by carrying out wet-mixed after composition proportion batching, use deionized water as solvent, mixing time is 80～90 minutes;
(2) spraying is dry: the slurry mixing is dried in spray tower, and spray tower inlet temperature is controlled at 200 ± 10 DEG C, and spray tower air outlet temperature is controlled at 100 ± 10 DEG C;
(3) pre-burning: dried spraying material is carried out to pre-burning in rotary oven, and calcined temperature is controlled at 800 ± 20 DEG C, and the pre-burning time is 160～180 minutes, and pre-burning atmosphere is air;
(4) pulverize: the Preburning material obtaining in upper step pre-burning carries out wet pulverization, use deionized water as solvent, grinding time is 100～120 minutes, and after pulverizing, slip particle diameter is controlled at 1.0～1.5 μ m;
(5) mist projection granulating: add 13～16% the PVA that is equivalent to material weight in the slurry of upper step, be dried and obtain particulate material in spray tower, spray tower inlet temperature is controlled at 200 ± 10 DEG C, and spray tower air outlet temperature is controlled at 100 ± 10 DEG C;
(6) compacting: adopt powder former compacting to obtain blank the particulate material of upper step, the pressed density of blank is controlled at (3.1 ± 0.15) g/cm
3;
(7) sintering: carry out sintering in chamber type electric resistance furnace, sintering temperature is controlled at 1000 DEG C～1020 DEG C, is incubated 120～180 minutes, and sintering atmosphere is air, cools to room temperature with the furnace after sintering finishes.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105261437A (en) * | 2015-09-15 | 2016-01-20 | 苏州凯欧曼新材料科技有限公司 | Preparation method of heat-resistant composite magnetic material |
| CN106495677A (en) * | 2016-10-10 | 2017-03-15 | 电子科技大学 | A kind of high-strength thermal-shock power nickel-zinc ferrite and preparation method thereof |
| CN106830914A (en) * | 2017-02-16 | 2017-06-13 | 珠海乾牌环保科技有限公司 | A kind of Bs high intensity soft magnetic ferrite high and preparation method thereof |
| CN106830915A (en) * | 2017-02-16 | 2017-06-13 | 珠海乾牌环保科技有限公司 | A kind of Bs high intensity soft magnetic ferrite high and preparation method thereof |
| CN107828372A (en) * | 2017-11-21 | 2018-03-23 | 常州思宇环保材料科技有限公司 | A kind of preparation method of silicon coating-codoping Conjugate ferrite microwave absorption |
| CN112430081A (en) * | 2020-11-25 | 2021-03-02 | 南通冠优达磁业有限公司 | High-saturation-flux-density soft magnetic ferrite material and preparation method thereof |
| CN113788671A (en) * | 2021-09-30 | 2021-12-14 | 横店集团东磁股份有限公司 | High-temperature-resistant tin-immersion high-performance nickel-zinc soft magnetic ferrite material and preparation method thereof |
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| CN113788671A (en) * | 2021-09-30 | 2021-12-14 | 横店集团东磁股份有限公司 | High-temperature-resistant tin-immersion high-performance nickel-zinc soft magnetic ferrite material and preparation method thereof |
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Application publication date: 20141203 |
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