CN114031388A - Mn-Zn ferrite material and preparation method thereof - Google Patents
Mn-Zn ferrite material and preparation method thereof Download PDFInfo
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- CN114031388A CN114031388A CN202111393852.8A CN202111393852A CN114031388A CN 114031388 A CN114031388 A CN 114031388A CN 202111393852 A CN202111393852 A CN 202111393852A CN 114031388 A CN114031388 A CN 114031388A
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- 239000000463 material Substances 0.000 title claims abstract description 88
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title description 7
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 21
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims description 40
- 239000001301 oxygen Substances 0.000 claims description 22
- 229910052760 oxygen Inorganic materials 0.000 claims description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 21
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000004576 sand Substances 0.000 claims description 11
- 238000005469 granulation Methods 0.000 claims description 10
- 230000003179 granulation Effects 0.000 claims description 10
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 claims description 9
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 229910052681 coesite Inorganic materials 0.000 claims description 7
- 229910052906 cristobalite Inorganic materials 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 229910052682 stishovite Inorganic materials 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052905 tridymite Inorganic materials 0.000 claims description 7
- 238000000748 compression moulding Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 abstract description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 6
- 238000012797 qualification Methods 0.000 abstract description 6
- 239000013078 crystal Substances 0.000 description 9
- 239000012535 impurity Substances 0.000 description 9
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000011148 porous material Substances 0.000 description 5
- 238000005336 cracking Methods 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 229910017163 MnFe2O4 Inorganic materials 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- -1 chlorine ions Chemical class 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(III) oxide Inorganic materials O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 150000005837 radical ions Chemical class 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C04B35/2633—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead containing barium, strontium or calcium
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- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/342—Oxides
- H01F1/344—Ferrites, e.g. having a cubic spinel structure (X2+O)(Y23+O3), e.g. magnetite Fe3O4
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Abstract
The invention discloses a method for utilizing industrial MnO2Compared with the traditional method of preparing high-performance high-frequency low-power-consumption MnZn ferrite material by using Mn as a raw material3O4The process for preparing MnZn ferrite by using the raw material has the advantages of low cost, high quality, production efficiency and qualification rate, and obvious microstructure and performance advantages, and uses industrial iron oxide red (Fe)2O3) Pyrolusite or electrolytic MnO2Industrial ZnO is used as a raw material to prepare the high-frequency low-power soft magnetic Mn-Zn ferrite material.
Description
Technical Field
The invention relates to the technical field of magnetic materials, in particular to a Mn-Zn ferrite material and a preparation method thereof.
Background
MnZn ferrite is a widely used material for the electronics industry, and is widely used as various electronic and electrical devices such as filters and transformers. In recent years, the application of MnZn ferrite is moving toward miniaturization of high Bs high frequency, and high Bs high frequency low power consumption MnZn ferrite material is the focus of research by various MnZn ferrite manufacturers. The key point of the preparation of the high-Bs high-frequency low-power-consumption MnZn ferrite material is to ensure that the material has a microstructure with small crystal grains, few pores and a compact structure. With Mn3O4The high-frequency low-power MnZn ferrite prepared by the raw material has the problems of uneven grain size, more pores, low density and low saturation magnetic flux density Bs. The main reason is the raw material Mn3O4In the pre-sintering stage, the raw material Fe is mixed with2O3Ferrite reaction occurs:
3Fe2O3+Mn3O4→3MnFe2O4+1/2O2
the ferrite is made of MnFe in the secondary sintering process2O4The crystal nucleus grows up, and part of crystal grains grow up abnormally, so that the crystal grains are uneven in size, multiple in air holes and low in density. And with MnO2The raw material does not react with Fe in the pre-sintering process2O3Reaction, thus with MnO2The high-frequency low-power consumption soft magnetic ferrite material prepared from the raw materials has the advantages of fine and uniform crystal grains, few pores and high density and saturation magnetic flux density Bs.
Further, with Mn3O4The MnZn ferrite material prepared by the raw material is pre-sintered to form MnFe in the temperature range of 500-700 ℃ during the sintering process2O4Oxidation reactions can occur, causing shrinkage cracking of the blank.
2MnFe2O4+1/2O2→Mn2O3+2Fe2O3
In order to avoid such problems, it is necessary to increase the temperature at a very slow rate in the temperature increase stage to avoid MnFe2O4Cracking of blank caused by oxidation。
The conventional MnZn ferrite material is generally Fe2O3、Mn3O4And ZnO is used as a main raw material, and the ZnO is mixed according to a certain proportion and then is subjected to presintering, sanding, granulation and sintering. Wherein Fe2O3The iron oxide red is mainly a byproduct of steel-making production, and because acid pickling is needed in the preparation process of the iron oxide red, a lot of impurities such as chloride ions, sulfate ions and the like are inevitably contained in the raw material iron oxide red, and the impurities need to be removed under the conditions of high temperature, high oxygen and slow temperature rise in the pre-sintering or secondary sintering process, otherwise, great harm is brought to the production of the ferrite magnetic core.
For the reasons stated above, Mn is used3O4The problems of easy cracking of a blank, insufficient impurity removal, long sintering time, low production efficiency and the like exist in the sintering process of the MnZn ferrite material, the quality and the qualification rate of the product are seriously influenced, and the production cost of an enterprise is indirectly improved. Relative to Mn3O4，MnO2Has the following application characteristics:
(1)MnO2belongs to high valence oxide, is unstable, and is firstly changed into Mn at 500-600 ℃ in the heating process2O3Then changed into Mn at 900-1000 DEG C3O4. The MnZn ferrite needs to be pre-sintered in the production process, and the pre-sintering temperature is 800-1000 ℃. MnO2Since it does not become Mn until 900 deg.C3O4And thus do not react with Fe2O3The direct reaction is adopted, the blank pressed by the powder is not easy to crack during secondary sintering, the temperature can be rapidly raised in the temperature raising stage, and the production qualification rate and the production efficiency are greatly improved.
(2)MnO2During the high temperature addition, Mn is first changed2O3And then changed into Mn3O4，
2MnO2→Mn2O3+1/2O2
3Mn2O3→2Mn3O4+1/2O2
Both reactions release oxygen, which can be promotedThe chlorine ions and the sulfate ions are oxidized and volatilized, so that the harm caused by the impurity atoms is reduced, the temperature rise time can be shortened, and the production efficiency and the qualification rate of the MnZn ferrite are effectively improved. Therefore, the invention provides a method for utilizing industrial MnO2Mn-Zn ferrite material prepared by using the raw material and a preparation method thereof.
Disclosure of Invention
In view of the above, the present invention is directed to providing a method for utilizing industrial MnO2Compared with the traditional method of preparing high-performance high-frequency low-power-consumption MnZn ferrite material by using Mn as a raw material3O4The method for preparing the MnZn ferrite by using the raw materials has the advantages of low cost, high quality, high production efficiency and qualification rate and obvious microstructure and performance advantages.
In order to achieve the purpose, the invention adopts the following technical scheme:
an Mn-Zn ferrite material comprising a main component and an auxiliary component, the main component comprising Fe2O3、MnO2And ZnO; the auxiliary components comprise CaO and SiO2、Nb2O5、Co2O3、TiO2And SnO2。
Preferably, the mole percentage of each component in the main component is as follows: fe2O350-57%, ZnO 4-12%, and the balance being MnO2。
Preferably, the content of each component in the auxiliary components is as follows according to the weight of the main component: CaO0.03-0.2%, SiO20.01-0.03％、Nb2O50.01-0.06％、Co2O30.05-0.3％、TiO20.05-0.2% and SnO20.05-0.3％。
The preparation method of the Mn-Zn ferrite material comprises the following steps:
(1) accurately weighing iron oxide red and MnO according to the formula2And ZnO, putting into a sand mill, adding water, mixing, and drying at 200 ℃ for 2h to obtain a dried material;
(2) putting the dried material into a muffle furnace for presintering at the presintering temperature of 800-950 ℃ for 1-4h to obtain a presintering material;
(3) after the pre-sintered material is cooled, weighing each component in the auxiliary components according to the total weight of the main components, mixing the components with the pre-sintered material, adding water for sanding for 1-5 hours to obtain a sand abrasive, wherein the sanding material D50 is 0.8-1.2 mu m;
(4) adding polyvinyl alcohol accounting for 0.1-0.5% of the weight of the pre-sintered material into the sand grinding material, and performing spray granulation;
(5) and (3) granulating, performing compression molding to obtain a Mn-Zn ferrite blank, and sintering the pressed Mn-Zn ferrite blank in an atmosphere protection bell jar furnace to obtain the Mn-Zn ferrite material.
Preferably, the amount of water added in step (1) is the same as the total weight of the main components.
Preferably, the Mn-Zn ferrite ingot in the step (5) has a density of 2.8 to 3.0kg/cm3。
Preferably, the sintering process of the sintering in the step (5) is as follows:
firstly, raising the temperature to 200 ℃ at the speed of 2-5 ℃/min in the air, and then raising the temperature to 300 ℃ at the speed of 0.5-1 ℃/min;
PVA added in the granulation process can be decomposed and volatilized at the temperature of 200-300 ℃, and if the PVA is volatilized violently at the too high temperature rise in the stage, the blank is easy to crack, so that the temperature needs to be raised slowly at the temperature of 200-300 ℃, and the PVA can be ensured to have sufficient time to volatilize;
secondly, the temperature is continuously and directly increased to 1100-1250 ℃ at the speed of 5-10 ℃/min, the oxygen content of the sintering atmosphere is reduced to 0.5-5.0 percent, and the temperature is preserved for 300 min;
due to the use of MnO2In place of Mn3O4Does not form MnFe after pre-sintering2O4So that MnFe does not exist in the temperature rising section2O4And the blank is cracked due to oxidation. Simultaneous MnO2Release of O by decomposition reaction2And the volatilization of chlorine radical and sulfate radical impurities in the blank is promoted, so that the harm caused by acid radical ions is avoided. Therefore, the temperature of the temperature rising section can be rapidly raised, and the production efficiency is effectively improved. For MnZn ferrite material with high Bs, high frequency and low power consumption, the microstructure crystal grains must be small, the air holes are few, the density is high, so the sintering temperature cannot be too high, and the sintering temperature is 1100-1250 DEG CThe comparison between them is moderate. The reduction of the oxygen content of the sintering atmosphere is favorable for promoting the elimination of pores and the microcosmic densification of the material, and the oxygen content of the sintering heat-preservation atmosphere is reduced to 0.5-5.0 percent, which can be matched with the heat-preservation time of 150-plus-material for 300min, the magnetic permeability of the material can be controlled to be 1000-plus-material 1500, and the density is controlled to be 4.8-4.9g/cm3The power consumption characteristic of the material 500K-3M is better;
thirdly, after the heat preservation is finished, the temperature is reduced to 1000 ℃ at the speed of 0.3-1.5 ℃/min, the oxygen content is controlled to be 0.5-1.0% at 1100 ℃, 0.1-0.3% at 1050 ℃ and 0.02-0.05% at 1000 ℃;
in the MnZn ferrite sintering heat preservation stage, impurities such as doped Ca, Si and the like are dissolved in MnZn spinel in a solid solution mode, in the cooling stage, the impurities can move and segregate to grain boundaries, and after cooling is finished, a high-resistivity insulating layer is formed on the grain boundaries, so that the grain boundary resistivity is improved, and the high-frequency power consumption characteristic of the material is reduced. By slowly cooling at the temperature of heat preservation-cooling of 1000 ℃, impurities such as Ca, Si and the like can be guaranteed to have sufficient time to move and segregate towards the grain boundary, so that the thickness of the grain boundary layer of the material is increased, and the high-frequency power consumption characteristic of the material is improved. The oxygen content of the sintering atmosphere is reduced at 1050 ℃ and 1000 ℃ mainly to avoid the oxidation of MnFe2O4 and Fe3O4 formed in the heat preservation stage, so that the performance of the material is deteriorated;
fourthly, the temperature is finally reduced to 200 ℃ at the speed of 3-10 ℃/min, and the oxygen content is controlled to be less than 50 ppm;
the purpose of reducing the temperature of the low-oxygen atmosphere at the stage is to protect MnFe formed at the heat preservation stage2O4And Fe3O4And the material performance is prevented from being damaged.
According to the technical scheme, compared with the prior art, the invention has the following beneficial effects:
(1)MnO2the pre-sintering stage does not react with Fe2O3Ferrite reaction is carried out, and MnFe does not exist in the secondary sintering stage2O4The problem of blank cracking is caused, so that the heating sintering can be carried out at a higher speed, the sintering time is shortened, and the production efficiency is improved;
(2)MnO2decomposing and releasing oxygen in the temperature rising stageThe method is beneficial to oxidizing and removing acid radicals and other impurities in the blank, thereby improving the quality and the qualification rate of the sintered product;
(3)MnO2the pre-sintering stage does not react with the raw material Fe2O3The ferrite reaction is carried out, so that crystal nuclei required by the growth of the secondary sintered ferrite can not be formed, the uniform growth of secondary sintered crystal grains is facilitated, and a microstructure with uniform crystal grain size and few pores is formed, thereby improving the high-frequency power consumption characteristic of the material.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The Mn-Zn ferrite material provided by the embodiment comprises a main component and an auxiliary component, wherein the mol percentage of each component in the main component is Fe2O357%, ZnO 12%, the balance being MnO2(ii) a The contents of the components in the auxiliary components are as follows according to the weight of the main components: CaO0.2%, SiO20.03％、Nb2O50.06％、Co2O30.3％、TiO20.2% and SnO20.3％。
This example prepares an Mn-Zn ferrite material as follows:
(1) accurately weighing iron oxide red (Fe)2O3)、MnO2And ZnO, putting into a sand mill, adding water, mixing, and drying to obtain a dried material;
(2) putting the dried material into a muffle furnace for presintering at 950 ℃ for 1h to obtain a presintering material;
(3) after the pre-sintered material is cooled, weighing each component in the auxiliary components according to the total weight of the main components, mixing the components with the pre-sintered material, adding water for sanding for 5 hours to obtain a sanding material, wherein the sanding material D50 is 1.2 mu m;
(4) adding polyvinyl alcohol accounting for 0.5 percent of the weight of the pre-sintered material into the sand grinding material, and performing spray granulation;
(5) and (2) after granulation, performing compression molding to obtain a Mn-Zn ferrite blank, and sintering the pressed Mn-Zn ferrite blank in an atmosphere protection bell jar furnace, wherein the sintering process comprises the following steps:
firstly, raising the temperature to 200 ℃ at the speed of 2 ℃/min in the air, and then raising the temperature to 300 ℃ at the speed of 0.5 ℃/min;
secondly, the temperature is directly raised to 1100 ℃ at the speed of 5 ℃/min, the oxygen content of the sintering atmosphere is reduced to 2.5 percent, and the temperature is preserved for 150 min;
thirdly, after the heat preservation is finished, the temperature is reduced to 1000 ℃ at the speed of 0.3 ℃/min, the oxygen content is controlled to be 0.5% at 1100 ℃, 0.1% at 1050 ℃ and 0.02% at 1000 ℃;
fourthly, the temperature is finally reduced to 200 ℃ at the speed of 10 ℃/min, and the oxygen content is controlled to be less than 50 ppm.
Example 2
The Mn-Zn ferrite material provided by the embodiment comprises a main component and an auxiliary component, wherein the mol percentage of each component in the main component is Fe2O350 percent of ZnO4 percent and the balance of MnO2(ii) a The contents of the components in the auxiliary components are as follows according to the weight of the main components: CaO0.03%, SiO20.01％、Nb2O50.01％、Co2O30.05％、TiO20.052% and SnO20.05％。
This example prepares an Mn-Zn ferrite material as follows:
(1) accurately weighing iron oxide red (Fe)2O3)、MnO2And ZnO, putting into a sand mill, adding water, mixing, and drying to obtain a dried material;
(2) putting the dried material into a muffle furnace for presintering at 800 ℃ for 4 hours to obtain a presintering material;
(3) after the pre-sintered material is cooled, weighing each component in the auxiliary components according to the total weight of the main components, mixing the components with the pre-sintered material, adding water for sanding for 1h to obtain a sanding material, wherein the sanding material D50 is 0.8 mu m;
(4) adding polyvinyl alcohol accounting for 0.5 percent of the weight of the pre-sintered material into the sand grinding material, and performing spray granulation;
(5) and (2) after granulation, performing compression molding to obtain a Mn-Zn ferrite blank, and sintering the pressed Mn-Zn ferrite blank in an atmosphere protection bell jar furnace, wherein the sintering process comprises the following steps:
firstly, raising the temperature to 200 ℃ at the speed of 5 ℃/min in the air, and then raising the temperature to 300 ℃ at the speed of 1 ℃/min;
secondly, the temperature is directly raised to 1100-1250 ℃ at the speed of 10 ℃/min, the oxygen content of the sintering atmosphere is reduced to 5.0 percent, and the temperature is maintained for 300 min;
thirdly, after the heat preservation is finished, the temperature is reduced to 1000 ℃ at the speed of 1.5 ℃/min, the oxygen content is controlled to be 1.0% at 1100 ℃, 0.3% at 1050 ℃ and 0.05% at 1000 ℃;
fourthly, the temperature is finally reduced to 200 ℃ at the speed of 3 ℃/min, and the oxygen content is controlled to be less than 50 ppm.
Example 3
The Mn-Zn ferrite material provided by the embodiment comprises a main component and an auxiliary component, wherein the mol percentage of each component in the main component is Fe2O3:52 mol% ZnO, 6 mol% ZnO, and the balance MnO2(ii) a The contents of the components in the auxiliary components are as follows according to the weight of the main components: 0.08 percent of CaO and SiO2:0.015％、Nb2O5:0.02％、Co2O30.1％、TiO20.08% and SnO20.08％。
This example prepares an Mn-Zn ferrite material as follows:
(1) accurately weighing iron oxide red (Fe)2O3)、MnO2And ZnO, putting into a sand mill, adding water, mixing, and drying to obtain a dried material;
(2) putting the dried material into a muffle furnace for presintering at 800 ℃ for 4 hours to obtain a presintering material;
(3) after the pre-sintered material is cooled, weighing each component in the auxiliary components according to the total weight of the main components, mixing the components with the pre-sintered material, adding water for sanding for 1h to obtain a sanding material, wherein the sanding material D50 is 0.8 mu m;
(4) adding polyvinyl alcohol accounting for 0.5 percent of the weight of the pre-sintered material into the sand grinding material, and performing spray granulation;
(5) and (2) after granulation, performing compression molding to obtain a Mn-Zn ferrite blank, and sintering the pressed Mn-Zn ferrite blank in an atmosphere protection bell jar furnace, wherein the sintering process comprises the following steps:
firstly, raising the temperature to 200 ℃ at a speed of 3 ℃/min in the air, and then raising the temperature to 300 ℃ at a speed of 1 ℃/min;
secondly, the temperature is directly raised to 1250 ℃ at the speed of 10 ℃/min, the oxygen content of the sintering atmosphere is reduced to 5.0 percent, and the temperature is preserved for 200 min;
thirdly, after the heat preservation is finished, the temperature is reduced to 1000 ℃ at the speed of 1.5 ℃/min, the oxygen content is controlled to be 1.0% at 1100 ℃, 0.3% at 1050 ℃ and 0.02% at 1000 ℃;
fourthly, the temperature is finally reduced to 200 ℃ at the speed of 10 ℃/min, and the oxygen content is controlled to be less than 50 ppm.
Performance testing
The initial permeability of the Mn-Zn ferrite-like ring prepared in example 3 was tested at 1000-1500, and the specific properties of the sintered density at 4.7-4.9kg/cm3 are shown in Table 1:
TABLE 1
As can be seen from the above table, the present invention uses MnO2In place of Mn3O4The Mn-Zn ferrite material with high Bs, high frequency and low power consumption is prepared.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. An Mn-Zn ferrite material characterized by comprising a main component and an auxiliary component, the main component comprising Fe2O3、MnO2And ZnO; the auxiliary components comprise CaO and SiO2、Nb2O5、Co2O3、TiO2And SnO2。
2. A Mn-Zn ferrite material according to claim 1, wherein the main component comprises the following components in mol%: fe2O350-57 mol%, ZnO4-12 mol%, and the balance being MnO2。
3. An Mn-Zn ferrite material as claimed in claim 2, wherein the contents of the components in the auxiliary component are, by weight based on the main component: CaO0.03-0.2%, SiO20.01-0.03％、Nb2O50.01-0.06％、Co2O30.05-0.3％、TiO20.05-0.2% and SnO20.05-0.3％。
4. A method of producing an Mn-Zn ferrite material according to claim 3, characterized by comprising the steps of:
(1) accurately weighing iron oxide red and MnO according to the formula2Mixing with ZnO, adding water, and drying at 200 deg.C for 2 hr to obtain dried material;
(2) pre-burning the dried material at the temperature of 800-950 ℃ for 1-4h to obtain a pre-burned material;
(3) after the pre-sintered material is cooled, weighing each component in the auxiliary components according to the total weight of the main components, mixing the components with the pre-sintered material, and then adding water for sanding for 1-5 hours to obtain a sand abrasive;
(4) adding polyvinyl alcohol accounting for 0.1-0.5% of the weight of the pre-sintered material into the sand grinding material, and performing spray granulation;
(5) and (3) granulating, performing compression molding to obtain a Mn-Zn ferrite blank, and sintering the pressed Mn-Zn ferrite blank in an atmosphere protection bell jar furnace to obtain the Mn-Zn ferrite material.
5. A method of producing an Mn-Zn ferrite material as claimed in claim 4, wherein the amount of water added in the step (1) is the same as the total weight of the main components.
6. A Mn-Zn ferrite material production method as claimed in claim 4, wherein the density of the Mn-Zn ferrite material in the step (5) is 2.8 to 3.0kg/cm3。
7. A method of producing an Mn-Zn ferrite material according to claim 4, wherein the sintering process of the sintering in the step (5) is:
firstly, raising the temperature to 200 ℃ at the speed of 2-5 ℃/min in the air, and then raising the temperature to 300 ℃ at the speed of 0.5-1 ℃/min;
secondly, the temperature is continuously and directly increased to 1100-1250 ℃ at the speed of 5-10 ℃/min, the oxygen content of the sintering atmosphere is reduced to 0.5-5.0 percent, and the temperature is preserved for 300 min;
thirdly, after the heat preservation is finished, the temperature is reduced to 1000 ℃ at the speed of 0.3-1.5 ℃/min, the oxygen content is controlled to be 0.5-1.0% at 1100 ℃, 0.1-0.3% at 1050 ℃ and 0.02-0.05% at 1000 ℃;
fourthly, the temperature is reduced to 200 ℃ at the cooling speed of 3 to 10 ℃/min, and the oxygen content is controlled to be less than 50 ppm.
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