CN112500149A - Preparation method of manganese zinc ferrite material with high saturation magnetic induction strength and low loss - Google Patents
Preparation method of manganese zinc ferrite material with high saturation magnetic induction strength and low loss Download PDFInfo
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- CN112500149A CN112500149A CN202011352072.4A CN202011352072A CN112500149A CN 112500149 A CN112500149 A CN 112500149A CN 202011352072 A CN202011352072 A CN 202011352072A CN 112500149 A CN112500149 A CN 112500149A
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- zinc ferrite
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- 239000000463 material Substances 0.000 title claims abstract description 74
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 title claims abstract description 29
- 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 29
- 230000006698 induction Effects 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000000498 ball milling Methods 0.000 claims abstract description 26
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 239000011230 binding agent Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 238000005303 weighing Methods 0.000 claims abstract description 12
- 238000004321 preservation Methods 0.000 claims abstract description 8
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000003825 pressing Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 31
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 9
- 229920000570 polyether Polymers 0.000 claims description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 9
- 229920002545 silicone oil Polymers 0.000 claims description 9
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 4
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 abstract description 4
- 229910000859 α-Fe Inorganic materials 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000000748 compression moulding Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000004891 communication Methods 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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Abstract
The invention discloses a preparation method of a manganese zinc ferrite material with high saturation magnetic induction intensity and low loss, which comprises the following steps: s1, weighing the main materials according to a formula with a certain mol percentage: fe2O3MnO, ZnO; s2, adding water into the main materials, ball-milling, drying, and carrying out heat preservation and pre-sintering to obtain a pre-sintered material; s3, weighing appropriate amount of CaCO based on the weight of the pre-sintered material3、TiO2、Nb2O5、Bi2O3Mixing the mixture with the pre-sintering material uniformly, adding water and ball milling to obtain a mixture; s4, uniformly mixing the mixture with the binder, and then granulating and pressing to form a blank; and S5, performing heat preservation sintering on the blank to obtain the manganese zinc ferrite material with high saturation magnetic induction strength and low loss. The manganese-zinc ferrite material prepared by the invention has high saturationAnd magnetic induction intensity, low loss and excellent magnetic performance.
Description
Technical Field
The invention relates to the technical field of ferrite materials, in particular to a preparation method of a manganese zinc ferrite material with high saturation magnetic induction strength and low loss.
Background
Ferrite is a composite oxide of iron and one or more other metal elements, is a novel non-metallic magnetic material, and is generally used as a magnetic medium to be widely applied to the fields of microwave communication, aerospace, instruments and meters, automobile industry and the like. With the continuous development of the technology, ferrite magnetic materials with different purposes and varieties are developed, wherein a soft magnetic ferrite material refers to a ferrite material which is easy to magnetize and demagnetize under a weaker magnetic field, and typical examples of the ferrite material are manganese zinc ferrite and nickel zinc ferrite.
The Mn-Zn ferrite is mainly used as various inductance elements and is used in key equipment such as various choke coil suppressors, inductors, transformers and the like in the communication field. In recent years, the information industry has been rapidly developed, and demands for miniaturization and thinning of devices have been gradually increased. The high saturation magnetic induction and low power loss of the manganese-zinc ferrite material are beneficial to reducing the volume of components and parts and achieving further miniaturization. Therefore, in order to meet the trend of industry, manganese-zinc ferrite materials are required to have lower loss and higher saturation magnetic induction.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a preparation method of a high-saturation-magnetic-induction-strength low-loss manganese-zinc ferrite material.
The invention provides a preparation method of a manganese zinc ferrite material with high saturation magnetic induction intensity and low loss, which comprises the following steps:
s1, weighing the main materials according to the following molar percentage: 50.5-53 mol% Fe2O3、37-39mol％MnO、9-10.5mol％ZnO；
S2, adding water into the main materials, ball-milling, drying, heating to 900-;
s3, weighing 0.05-0.08 wt% of CaCO based on the weight of the pre-sintered material3、0.03-0.05wt％TiO2、0.005-0.01wt％Nb2O5、0.003-0.005wt％Bi2O3Mixing the pre-sintering material uniformly, adding water, and ball milling to obtain a mixture;
s4, uniformly mixing the mixture with a binder, and then granulating and pressing to obtain a blank, wherein the binder comprises the following raw materials: polyvinyl alcohol, water-soluble polyether silicone oil, a silane coupling agent and water;
s5, heating the blank to 1250-1300 ℃ for heat preservation and sintering to obtain the manganese zinc ferrite material with high saturation magnetic induction strength and low loss.
Preferably, the binder comprises the following raw materials in percentage by weight: 6.5-8% of polyvinyl alcohol, 0.5-1% of water-soluble polyether silicone oil, 0.1-0.3% of silane coupling agent and the balance of water.
Preferably, the weight ratio of the mixture to the binder is (8-10): 1.
preferably, in the step S5, the blank is first heated to 400-.
Preferably, in step S2, the burn-in time is maintained for 2-4 h.
Preferably, in step S2, the mass ratio of the main material to the water during ball milling is (0.5-1): 1, the ball milling time is 1.5-2.5 h.
Preferably, in step S3, the mass ratio of the pre-sintered material to water during ball milling is (0.5-1): 1, the ball milling time is 6-8 h.
A manganese zinc ferrite material with high saturation magnetic induction strength and low loss is prepared by the preparation method.
The invention has the following beneficial effects:
in the preparation method of the invention, proper main material proportion and CaCO are selected3、TiO2、Nb2O5、Bi2O3The additive enables the prepared manganese-zinc ferrite material to have higher saturation magnetic induction intensity and lower power loss; on the basis, polyvinyl alcohol, water-soluble polyether silicone oil and a silane coupling agent are compounded to serve as a binder, the good thermal conductivity of the polyether silicone oil is utilized, the temperature distribution in the blank body is more uniform in the sintering starting stage, volatile substances in the blank body are more easily discharged when the temperature is raised, and residual air holes are not discharged in time and can be relieved by combining the optimization of a sintering process in the sintering processThe remaining problem is beneficial to forming fine, uniform and compact crystal grains, so that the prepared manganese-zinc ferrite material can simultaneously meet the use requirements of high saturation magnetic induction intensity and low loss and has excellent magnetic performance.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A preparation method of a manganese zinc ferrite material with high saturation magnetic induction strength and low loss comprises the following steps:
s1, weighing the main materials according to the following molar percentage: 52.5 mol% Fe2O3、37.5mol％MnO、10mol％ZnO；
S2, adding water into the main material, and performing ball milling, wherein the mass ratio of the main material to the water is 0.75: 1, ball milling for 2 hours, drying, heating to 950 ℃, preserving heat and presintering for 3 hours to obtain a presintering material;
s3, weighing 0.06 wt% CaCO based on the weight of the pre-sintered material3、0.045wt％TiO2、0.008wt％Nb2O5、0.004wt％Bi2O3And uniformly mixing the powder with a pre-sintering material, adding water, and ball-milling, wherein the mass ratio of the pre-sintering material to the water is 0.75: 1, ball milling for 6-8h to obtain a mixture;
s4, mixing the mixture with a binder according to the weight ratio of 9: 1, uniformly mixing, granulating, and performing compression molding to obtain a blank, wherein the binder comprises the following raw materials in percentage by weight: 7.5 percent of polyvinyl alcohol, 0.8 percent of Dow Corning OFX-0400 polyether silicone oil, KH-5700.2 percent of silane coupling agent and the balance of water;
s5, heating the blank to 450 ℃ at a heating rate of 70 ℃/h, heating to 780 ℃ at a heating rate of 180 ℃/h, heating to 1000 ℃ at a heating rate of 300 ℃/h, heating to 1275 ℃ at a heating rate of 150 ℃/h, and carrying out heat preservation sintering for 5h to obtain the high saturation magnetic induction density low-loss manganese-zinc ferrite material.
Example 2
A preparation method of a manganese zinc ferrite material with high saturation magnetic induction strength and low loss comprises the following steps:
s1, weighing the main materials according to the following molar percentage: 50.5 mol% Fe2O3、39mol％MnO、10.5mol％ZnO；
S2, adding water into the main material, and performing ball milling, wherein the mass ratio of the main material to the water is 0.5: 1, ball milling for 1.5h, then drying, heating to 900 ℃, preserving heat and presintering for 4h to obtain a presintering material;
s3, weighing 0.05 wt% CaCO based on the weight of the pre-sintered material3、0.03wt％TiO2、0.01wt％Nb2O5、0.005wt％Bi2O3And uniformly mixing the pre-sintered material and the pre-sintered material, and then adding water for ball milling, wherein the mass ratio of the pre-sintered material to the water is 0.5: 1, ball milling for 6 hours to obtain a mixture;
s4, mixing the mixture with a binder according to a weight ratio of 8: 1, uniformly mixing, granulating, and performing compression molding to obtain a blank, wherein the binder comprises the following raw materials in percentage by weight: 6.5 percent of polyvinyl alcohol, 0.5 percent of Dow Corning OFX-0400 polyether silicone oil, 0.78 percent of silane coupling agent KH-5700.1 percent and the balance of water;
s5, heating the blank to 400 ℃ at a heating rate of 60 ℃/h, heating to 750 ℃ at a heating rate of 150 ℃/h, heating to 950 ℃ at a heating rate of 240 ℃/h, heating to 1250 ℃ at a heating rate of 120 ℃/h, and carrying out heat preservation sintering for 6h to obtain the high-saturation-magnetic-induction-strength low-loss manganese-zinc ferrite material.
Example 3
A preparation method of a manganese zinc ferrite material with high saturation magnetic induction strength and low loss comprises the following steps:
s1, weighing the main materials according to the following molar percentage: 53 mol% Fe2O3、38mol％MnO、9mol％ZnO；
S2, adding water into the main material, and performing ball milling, wherein the mass ratio of the main material to the water is 1: 1, ball milling for 1.5h, then drying, heating to 1000 ℃, preserving heat and presintering for 2h to obtain a presintering material;
s3, weighing 0.08 wt% CaCO based on the weight of the pre-sintered material3、0.05wt％TiO2、0.01wt％Nb2O5、0.005wt％Bi2O3And uniformly mixing the pre-sintering material and water, and then adding water for ball milling, wherein the mass ratio of the pre-sintering material to the water is 1: 1, ball milling for 6-8h to obtain a mixture;
s4, mixing the mixture with a binder according to the weight ratio of 10: 1, uniformly mixing, granulating, and performing compression molding to obtain a blank, wherein the binder comprises the following raw materials in percentage by weight: 8% of polyvinyl alcohol, 1% of Dow Corning OFX-0400 polyether silicone oil, 1% of silane coupling agent KH-5700.3% and the balance of water;
s5, heating the blank to 500 ℃ at a heating rate of 75 ℃/h, heating to 850 ℃ at a heating rate of 210 ℃/h, heating to 1050 ℃ at a heating rate of 360 ℃/h, heating to 1300 ℃ at a heating rate of 180 ℃/h, and carrying out heat preservation sintering for 4h to obtain the high-saturation-magnetic-induction-strength low-loss manganese-zinc ferrite material.
Comparative example 1
Comparative example 1 differs from example 1 only in that in step S4, the binder used was an aqueous polyvinyl alcohol solution having a mass concentration of 7.5%.
The ferrite materials prepared in examples 1 to 3 and comparative example 1 were subjected to a performance test under the test conditions of a saturation magnetic induction Bs of 1194A/m and 100 ℃; the test conditions for the power loss Pcv were 200mT, 100 ℃. The test results are shown in table 1:
TABLE 1 ferrite Material Performance test results
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. A preparation method of a manganese zinc ferrite material with high saturation magnetic induction strength and low loss is characterized by comprising the following steps:
s1, weighing the main materials according to the following molar percentage: 50.5-53 mol% Fe2O3、37-39mol％MnO、9-10.5mol％ZnO；
S2, adding water into the main materials, ball-milling, drying, heating to 900-;
s3, weighing 0.05-0.08 wt% of CaCO based on the weight of the pre-sintered material3、0.03-0.05wt％TiO2、0.005-0.01wt％Nb2O5、0.003-0.005wt％Bi2O3Mixing the pre-sintering material uniformly, adding water, and ball milling to obtain a mixture;
s4, uniformly mixing the mixture with a binder, and then granulating and pressing to obtain a blank, wherein the binder comprises the following raw materials: polyvinyl alcohol, water-soluble polyether silicone oil, a silane coupling agent and water;
s5, heating the blank to 1250-1300 ℃ for heat preservation and sintering to obtain the manganese zinc ferrite material with high saturation magnetic induction strength and low loss.
2. The method for preparing a manganese zinc ferrite material with high saturation magnetic induction and low loss according to claim 1, wherein the binder comprises the following raw materials in percentage by weight: 6.5-8% of polyvinyl alcohol, 0.5-1% of water-soluble polyether silicone oil, 0.1-0.3% of silane coupling agent and the balance of water.
3. The preparation method of the high saturation magnetic induction density low loss manganese zinc ferrite material according to claim 1 or 2, characterized in that the weight ratio of the mixture to the binder is (8-10): 1.
4. the method as claimed in any one of claims 1 to 3, wherein in the step S5, the temperature of the blank is raised to 400-850 ℃ at a temperature rise rate of 60-75 ℃/h, then raised to 750-850 ℃ at a temperature rise rate of 150-210 ℃/h, then raised to 950-1050 ℃ at a temperature rise rate of 240-360 ℃/h, and finally raised to 1250-1300 ℃ at a temperature rise rate of 120-180 ℃/h, and then sintered for 4-6 h.
5. The method for preparing a manganese zinc ferrite material with high saturation magnetic induction and low loss according to any one of claims 1 to 4, wherein in the step S2, the heat preservation and pre-sintering time is 2 to 4 hours.
6. The method for preparing a manganese zinc ferrite material with high saturation magnetic induction and low loss according to any one of claims 1 to 5, wherein in the step S2, the mass ratio of the main material to water during ball milling is (0.5-1): 1, the ball milling time is 1.5-2.5 h.
7. The method for preparing a manganese zinc ferrite material with high saturation magnetic induction and low loss according to any one of claims 1 to 6, wherein in the step S3, the mass ratio of the pre-sintering material to water during ball milling is (0.5-1): 1, the ball milling time is 6-8 h.
8. A high saturation magnetic induction low loss manganese zinc ferrite material prepared by the preparation method of any one of claims 1 to 7.
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