CN114773047B - Broadband high-impedance manganese zinc ferrite material and preparation method and application thereof - Google Patents
Broadband high-impedance manganese zinc ferrite material and preparation method and application thereof Download PDFInfo
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- CN114773047B CN114773047B CN202210443170.1A CN202210443170A CN114773047B CN 114773047 B CN114773047 B CN 114773047B CN 202210443170 A CN202210443170 A CN 202210443170A CN 114773047 B CN114773047 B CN 114773047B
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- 239000000463 material Substances 0.000 title claims abstract description 67
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 title claims abstract description 48
- 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 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000843 powder Substances 0.000 claims description 45
- 238000000498 ball milling Methods 0.000 claims description 21
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 19
- 239000001301 oxygen Substances 0.000 claims description 19
- 229910052760 oxygen Inorganic materials 0.000 claims description 19
- 230000036961 partial effect Effects 0.000 claims description 19
- 239000007864 aqueous solution Substances 0.000 claims description 18
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 16
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 15
- 239000002270 dispersing agent Substances 0.000 claims description 12
- 230000002829 reductive effect Effects 0.000 claims description 12
- 239000011572 manganese Substances 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000004321 preservation Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 8
- 229920002125 Sokalan® Polymers 0.000 claims description 7
- 238000004590 computer program Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 7
- 239000008187 granular material Substances 0.000 claims description 7
- 229910052748 manganese Inorganic materials 0.000 claims description 7
- 239000004584 polyacrylic acid Substances 0.000 claims description 7
- 238000011946 reduction process Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 230000001939 inductive effect Effects 0.000 claims 1
- 230000035699 permeability Effects 0.000 abstract description 19
- 229910000859 α-Fe Inorganic materials 0.000 abstract description 19
- 239000011701 zinc Substances 0.000 abstract description 6
- 239000000696 magnetic material Substances 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 14
- 238000005245 sintering Methods 0.000 description 9
- 238000001816 cooling Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 4
- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000002075 main ingredient Substances 0.000 description 2
- 238000004804 winding Methods 0.000 description 2
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- 229910004762 CaSiO Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 1
- RGHNJXZEOKUKBD-SQOUGZDYSA-N Gluconic acid Natural products OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000000174 gluconic acid Substances 0.000 description 1
- 235000012208 gluconic acid Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- WJZHMLNIAZSFDO-UHFFFAOYSA-N manganese zinc Chemical compound [Mn].[Zn] WJZHMLNIAZSFDO-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 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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Abstract
The invention belongs to the technical field of magnetic materials, and provides a broadband high-impedance manganese-zinc ferrite material, a preparation method and application thereof, wherein the manganese-zinc ferrite material comprises a main component and an auxiliary component, and the main component is prepared from Fe in a certain proportion 2 O 3 ZnO and Mn 3 O 4 The auxiliary component comprises Co 2 O 3 、CaCO 3 、Nb 2 O 5 、V 2 O 5 The invention can make the Mn-Zn ferrite material obtain high initial permeability, high Curie temperature and high DC resistivity by reasonably adjusting the formula, and has high impedance characteristics in a wide frequency range of 1MHz-500MHz, wherein the initial permeability is more than or equal to 6000 at 25 ℃, the Curie temperature is more than or equal to 120 ℃, the DC resistivity is more than or equal to 1000Ω.m, and the impedance of 1MHz, 25MHz, 100MHz and 500MHz is respectively more than or equal to 20Ω, 65Ω, 125Ω and 1000Ω.
Description
Technical Field
The invention relates to the technical field of magnetic materials, in particular to a broadband high-impedance manganese zinc ferrite material, a preparation method and application thereof.
Background
An effective way to reduce electromagnetic pollution and improve the anti-electromagnetic interference capability of electronic devices is to use electromagnetic compatibility (EMC) design, in which a large amount of anti-electromagnetic interference (EMI) materials are required, and soft magnetic ferrite has become an integral part of modern military electronic devices, industrial and civil electronic instruments due to the development of miniaturization, flattening and high frequency of electronic devices.
Common electromagnetic interference (EMI) resistant materials include manganese zinc ferrite and nickel zinc ferrite, and compared with nickel zinc ferrite, manganese zinc ferrite has low direct current resistivity, high dielectric constant and the like, so that the manganese zinc ferrite is difficult to adapt to high frequency above 1 MHz; the nickel zinc ferrite has low-frequency impedance, high manufacturing cost and certain limit on application.
The manganese zinc ferrite material with impedance characteristics in the prior art has low initial permeability, is unfavorable for improving low-frequency impedance, or has low Curie temperature and limited practicability, and even if CuO, niO and other components are added in a main formula, the use frequency is improved, but the low-frequency impedance is low, and the cost is high. In addition, although the manganese zinc ferrite material with high frequency and high impedance has high initial permeability, the manganese zinc ferrite material with high frequency and high impedance has a Curie temperature below 40 ℃ and cannot be used in working environments with high Curie temperature requirements (more than 120 ℃) such as 5G communication, automobile electronics and the like, and has limited practicability.
Therefore, it is difficult to combine the high initial permeability, the high curie temperature and the high dc resistivity with the high impedance characteristic in a wide frequency range, and therefore, it is highly desirable to develop a ferrite material which combines the high initial permeability, the high curie temperature and the high dc resistivity with the high impedance characteristic in a wide frequency range.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the prior art described above. Therefore, the invention provides a broadband high-impedance manganese-zinc ferrite material, a preparation method and application thereof, and the provided manganese-zinc ferrite material has the characteristics of high initial permeability, high Curie temperature and high direct current resistivity, and has the characteristics of high impedance in a broadband range, wherein the initial permeability is more than or equal to 6000 at 25 ℃, the Curie temperature is more than or equal to 120 ℃, the direct current resistivity is more than or equal to 1000 Ω & m, and the impedance of the manganese-zinc ferrite material in 1MHz, 25MHz, 100MHz and 500MHz is respectively more than or equal to 20Ω, 65Ω, 125Ω and 1000Ω.
The first aspect of the invention provides a broadband high-impedance manganese zinc ferrite material.
Specifically, a broadband high-impedance manganese-zinc ferrite material is prepared from the raw materials including a main component and an auxiliary component; the main components comprise the following components in percentage by mass: 63.5 to 66.5wt% of Fe 2 O 3 12.5-16.0wt% ZnO, 18-24wt% Mn 3 O 4 The method comprises the steps of carrying out a first treatment on the surface of the According to the total content of the main componentsThe auxiliary components comprise one or more of the following components in percentage by weight: co (Co) 2 O 3 0.60-1.20wt％、CaCO 3 0.01-0.03wt％、Nb 2 O 5 0.01-0.03wt％、V 2 O 5 0.01-0.025wt％。
The Mn-Zn ferrite material provided by the invention is prepared by adjusting Fe in main components 2 O 3 ZnO and Mn 3 O 4 Is effective in inhibiting Fe 2+ Ion generation, fe is reduced 2+ -Fe 3+ The electron migration between the two electrodes improves the direct current resistivity of the material, so that the use frequency of the material is greatly improved; general ferrite magnetocrystalline anisotropy constant K 1 Is negative, and the auxiliary component is added with proper amount of Co 2 O 3 By Co 2+ To compensate K 1 Not only has the function of improving the initial permeability temperature characteristic, but also can lead K 1 The temperature curve of the value becomes flat, the initial permeability of normal temperature is improved, and the impedance characteristic of a wide frequency range is improved; caCO in raw materials 3 With Fe 2 O 3 Contains SiO as an impurity 2 Reaction takes place, ca 2+ And Si (Si) 4+ Diffusion to grain boundary to form CaSiO 1-10nm thick in the grain boundary layer 3 The insulating layer improves the direct current resistivity of the material and plays a role in improving broadband impedance characteristics; nb (Nb) 2 O 5 The magnetic material exists in a crystal boundary, plays a role in preventing crystal grains from growing, so that a fine and uniform microstructure of the crystal grains is formed, the crystal grains become uniform and compact, the porosity is reduced, the resistance of domain wall displacement and magnetization vector rotation is reduced, the initial permeability of the magnetic material is not reduced and is reversely increased, and the impedance of broadband is improved; adding V 2 O 5 Mainly plays roles of reducing melting point and densification, is beneficial to liquid phase sintering, and promotes grain growth at a lower sintering temperature, thereby obtaining a uniform and compact microstructure.
Preferably, the initial permeability at 25 ℃ is 6000 or more, the curie temperature is 120 ℃ or more, and the direct current resistivity is 1000Ω·m or more.
Preferably, the impedance at 1MHz, 25MHz, 100MHz and 500MHz is equal to or greater than 20Ω, 65Ω, 125Ω and 1000Ω, respectively.
Preferably, the raw materials for preparing the manganese-zinc ferrite material further comprise water, a dispersing agent and an aqueous solution of an organic binder.
The second aspect of the invention provides a preparation method of the broadband high-impedance manganese zinc ferrite material.
The invention discloses a preparation method for protecting the manganese-zinc ferrite material, which comprises the following steps:
and (3) presintering the components of the main component, adding the auxiliary component, performing ball milling, granulating, pressing into a green body sample, sintering, and cooling to obtain the manganese-zinc ferrite material.
Preferably, the ball milling process further comprises adding water and a dispersing agent, and after ball milling, the ball milling process further comprises adding an aqueous solution of an organic binder, mixing and granulating.
Preferably, the presintering temperature is 750-850 ℃, and the presintering time is 2-3h.
Preferably, the mass of the water is 40-60% of the total mass of the main component.
Preferably, the mass of the dispersant is 0.5 to 3% of the total mass of the main component.
Preferably, the dispersing agent is one or more of the group consisting of the poly propionic acid, the gluconic acid and the citric acid.
Preferably, each component of the main ingredient further comprises a step of drying before pre-firing.
Preferably, the ball milling time is 20-60min.
Preferably, the average particle size of the powder after ball milling is less than 1.0 μm.
Preferably, the mass of the aqueous solution of the organic binder is 5-8% by weight of the mass of the powder.
Preferably, the organic binder is polyvinyl alcohol.
Preferably, the green sample has a density of 3.0.+ -. 0.2g/cm 3 。
Preferably, the sintering temperature is 1280-1360 ℃, and the sintering time is 4-8h.
Preferably, the sintering comprises three stages, namely a heating stage, a heat preservation stage and a cooling stage, wherein the heating stage adopts air sintering, the temperature is raised to 1280-1360 ℃ from normal temperature, the oxygen partial pressure of the heat preservation stage is 1-6%, and the cooling stage adopts nitrogen protection.
Preferably, the equilibrium oxygen partial pressure P of the cooling stage O2 Calculated according to the following formula:
log(P O2 )＝(a–b)/T；
wherein a is 7-9,b and is 12000-15000, and T is absolute temperature.
Preferably, the normal temperature is 25-30 ℃.
Preferably, the cooling is to 170-190 ℃.
The third aspect of the invention provides an application of the wide-band high-impedance manganese zinc ferrite material.
The invention protects the application of the manganese-zinc ferrite material in preparing an inductance device.
A fourth aspect of the present invention provides an electromagnetic interference resistant material.
The raw materials for preparing the anti-electromagnetic interference material comprise the manganese zinc ferrite material.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention provides a broadband high-impedance Mn-Zn ferrite material, which is prepared by taking main components and auxiliary components as main raw materials, wherein the main components are prepared from Fe with a certain proportion 2 O 3 ZnO and Mn 3 O 4 The auxiliary component comprises Co 2 O 3 、CaCO 3 、Nb 2 O 5 、V 2 O 5 The invention reasonably adjusts the formula so that the initial magnetic conductivity of the manganese-zinc ferrite material at 25 ℃ is not lower than 6000, the Curie temperature is not lower than 120 ℃, the direct current resistivity is not lower than 1000 omega-m, and the manganese-zinc ferrite material has high impedance characteristics in a wide frequency range of 1-500MHz, wherein the impedance of the manganese-zinc ferrite material at 1MHz, 25MHz, 100MHz and 500MHz is not lower than 20 omega, 65 omega, 125 omega and 1000 omega respectively, and the manganese-zinc ferrite material provided by the invention has high initial magnetic conductivity and high initial magnetic conductivityThe characteristic of Curie temperature and high direct current resistivity, and has high impedance characteristic in a wide frequency range;
(2) The manganese-zinc ferrite material is prepared by adopting a method of presintering, ball milling and sintering, and the sintering temperature and atmosphere parameters are optimized, so that the activity of powder is improved, the density is increased, the crystal grains are increased, the structure is promoted to be uniform, and the purpose of improving the initial magnetic conductivity is achieved;
(3) The manganese-zinc ferrite material provided by the invention can be further used for preparing an inductance device, the inductance device can reduce the number of turns of a coil, the process is simplified, the cost is reduced, and the prepared product can meet the electromagnetic interference resistance requirements of 5G communication, automobile electronics and the like, so that the market demand is better met.
Drawings
FIG. 1 is a graph showing initial permeability vs. temperature for a broadband high-impedance ferrite prepared in example 2 of the present invention and a general high-impedance ferrite of comparative example 11.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples will be presented. It should be noted that the following examples do not limit the scope of the invention.
The starting materials, reagents or apparatus used in the following examples are all available from conventional commercial sources or may be obtained by methods known in the art unless otherwise specified.
Example 1
A kind of wide band high impedance manganese zinc ferrite material, the raw materials for preparing manganese zinc ferrite material include principal component and auxiliary component; the main component comprises Fe 2 O 3 、Mn 3 O 4 ZnO, the components and contents of the main components are shown in the following table 1; the auxiliary component is Co accounting for 1.00 weight percent of the total weight of the main component 2 O 3 0.02wt% CaCO 3 V0.015 wt% 2 O 5 。
The preparation method of the broadband high-impedance manganese zinc ferrite material comprises the following steps:
placing the components of the main components into a ball mill, mixing for 0.5 hour, taking out and drying to obtain powder, and presintering the powder at 830 ℃ for 2.0 hours by using a box-type resistance furnace; then placing the presintered powder into a ball mill, and adding auxiliary components into the obtained powder; adding 50wt% of deionized water based on the total mass of the main component and 1.5wt% of polyacrylic acid dispersing agent based on the total mass of the main component, and performing ball milling until the average granularity is 1.0 mu m; adding an aqueous solution of polyvinyl alcohol into the powder, wherein the addition amount of the aqueous solution of the polyvinyl alcohol is 7 weight percent of the total mass of the powder after ball milling, uniformly mixing and granulating, and pressing the granules into an annular sample of OR25 (outer diameter) x 8 (height) x 15 (inner diameter) mm; finally, the temperature is kept for 5 hours in a bell jar furnace controlled by a computer program at 1320 ℃, and then the temperature is slowly reduced and cooled to 180 ℃ for discharging; wherein the oxygen partial pressure of the heat preservation section is 4.0%, and the temperature reduction process adopts the equilibrium oxygen partial pressure.
Equilibrium oxygen partial pressure formula log (P) O2 ) In = (a-b)/T, a is 7.73, b is 14540, and T is absolute temperature.
Examples 2 to 3
Examples 2 to 3 differ from example 1 in the content of each component of the main ingredient, and the preparation method is the same, as shown in Table 1.
Example 4
A broadband high-impedance Mn-Zn ferrite material is prepared from main component (65.1 wt.%) and auxiliary component (65.1 wt.%) 2 O 3 20.4wt% Mn 3 O 4 And 14.5wt% ZnO, the auxiliary components are shown in Table 2 below.
The preparation method of the broadband high-impedance manganese zinc ferrite material comprises the following steps:
placing the components of the main components into a ball mill, mixing for 0.5 hour, taking out and drying to obtain powder, and presintering the powder at 800 ℃ for 2.5 hours by using a box-type resistance furnace; then placing the presintered powder into a ball mill, and adding auxiliary components into the obtained powder; adding 50wt% of deionized water based on the total mass of the main component and 1.5wt% of polyacrylic acid dispersing agent based on the total mass of the main component, and performing ball milling until the average granularity is 1.0 mu m; adding an aqueous solution of polyvinyl alcohol into the powder, wherein the addition amount of the aqueous solution of the polyvinyl alcohol is 7 weight percent of the total mass of the powder after ball milling, uniformly mixing and granulating, and pressing the granules into an annular sample of OR25 (outer diameter) x 8 (height) x 15 (inner diameter) mm; finally, the temperature is kept for 6 hours in a bell jar furnace controlled by a computer program at 1300 ℃, and then the temperature is slowly reduced and cooled to 180 ℃ for discharging; wherein the oxygen partial pressure of the heat preservation section is 3.0%, and the temperature reduction process adopts the equilibrium oxygen partial pressure.
Equilibrium oxygen partial pressure formula log (P) O2) In = (a-b)/T, a is 7.73, b is 14540, and T is absolute temperature.
Examples 5 to 7
Examples 5 to 7 differ from example 4 in the content of each component of the auxiliary ingredient, specifically as shown in Table 2, and the preparation method was the same.
Comparative examples 1 to 2
Comparative examples 1 to 2 are different from example 1 in the content of each component of the main component, and the preparation method is the same as shown in Table 1.
Comparative examples 3 to 10
Comparative examples 3 to 10 are different from example 4 in the content of each component of the auxiliary ingredient, and the preparation method is the same, as shown in Table 2.
Comparative example 11
Comparative example 11 is a conventional high-resistance ferrite (conventional high-resistance material), the raw materials for preparing the conventional high-resistance ferrite include a main component, an auxiliary component, water, a dispersant, and an aqueous solution of polyvinyl alcohol, and the main component is 61.8wt% of Fe in terms of mass percent 2 O 3 22.9wt% Mn 3 O 4 And 15.3wt% ZnO; the auxiliary components are calculated according to the mass percentage of the total weight of the main components: 0.03wt% Co 2 O 3 0.04wt% CaCO 3 V0.03 wt% 2 O 5 。
The preparation method of the common high-impedance ferrite comprises the following steps:
placing the components of the main components into a ball mill, mixing for 0.5 hour, taking out and drying to obtain powder, and presintering the powder at 800 ℃ for 2.5 hours by using a box-type resistance furnace; then placing the presintered powder into a ball mill, and adding auxiliary components into the obtained powder; adding 50wt% of deionized water based on the total mass of the main component and 1.5wt% of polyacrylic acid dispersing agent based on the total mass of the main component, and performing ball milling until the average granularity is 1.0 mu m; adding an aqueous solution of polyvinyl alcohol into the powder, wherein the addition amount of the aqueous solution of the polyvinyl alcohol is 7 weight percent of the total mass of the powder after ball milling, uniformly mixing and granulating, and pressing the granules into an annular sample of OR25 (outer diameter) x 8 (height) x 15 (inner diameter) mm; finally, the temperature is kept for 6 hours in a bell jar furnace controlled by a computer program at 1300 ℃, and then the temperature is slowly reduced and cooled to 180 ℃ for discharging; wherein the oxygen partial pressure of the heat preservation section is 3.0%, and the temperature reduction process adopts the equilibrium oxygen partial pressure.
Equilibrium oxygen partial pressure formula log (P) O2 ) In = (a-b)/T, a is 7.73, b is 14540, and T is absolute temperature.
TABLE 1 Main Components of examples 1-3 and comparative examples 1-2 and their contents
TABLE 2 auxiliary Components of examples 4-7 and comparative examples 3-10 in mass percent based on the total weight of the main component
Application example
The raw material components for preparing the anti-electromagnetic interference material comprise the manganese zinc ferrite material prepared in the embodiment 1.
Product effect test
1. Test method
The prepared annular sample with the diameter of OR25 (outer diameter) multiplied by 8 (height) multiplied by 15 (inner diameter) is measured by an Agilent4287A tester at the normal temperature of 25 ℃, and the inductance L (winding 10 turns) of the sample at 10kHz and the impedance Z (winding single turns) of 1MHz, 25MHz, 100MHz and 500MHz are measured, and the initial permeability is calculated by the corresponding inductance L. The inductance is slightly increased near the Curie temperature, then is suddenly decreased, and the temperature extrapolated to zero inductance along the largest part of the curve descent slope is the Curie temperature Tc (DEG C). The two surfaces of the sample are firstly polished, the sample is clamped by two copper plates, the direct current resistance of the sample is measured by a universal meter, and the direct current resistivity (omega.m) of the sample is calculated.
2. Test results
TABLE 3 electromagnetic physical property test result data for each of examples and comparative examples
As is clear from Table 3 above, the Mn-Zn ferrite materials prepared in examples 1 to 7 have high impedance characteristics in a wide frequency range of 1MHz to 500MHz, in which the initial permeability (. Mu.i) at 25℃is not lower than 6000, the Curie temperature (Tc) is not lower than 120℃and the DC resistivity is not lower than 1000Ω.m, and in which the impedances of 1MHz, 25MHz, 100MHz and 500MHz are not lower than 20Ω, 65Ω, 125Ω and 1000Ω, respectively.
While the main component of the manganese-zinc-ferrite material of comparative example 1 is Fe 2 O 3 The content is excessive, the impedance at 25MHz is only 3 omega, the impedance characteristic is not provided at higher frequency, the direct current resistivity is only 5 omega-m, and the high direct current resistivity characteristic is not provided; fe in the main component of the manganese-zinc-ferrite material of comparative example 2 2 O 3 The content is too small, the impedance at 1MHz is only 4Ω, the impedance at 25-500MHz is also significantly lower than in examples 1-3, and the Curie temperature Tc is only 107 ℃. Whereas the manganese zinc ferrites of comparative examples 3-10The material has the auxiliary components and the content thereof regulated, and cannot obtain the material with high initial permeability, high Curie temperature, high direct current resistivity and high impedance in a wide frequency range. Therefore, the main component and the auxiliary component and the content thereof need to be matched with each other, the prepared Mn-Zn ferrite material can obtain excellent broadband high-impedance characteristics, any component exceeds the range defined by the invention, and the prepared material can not obtain good performance.
In addition, as can be seen from fig. 1, the broadband high-impedance ferrite prepared in the embodiment 2 of the present invention has high activity through reasonably adjusting the formulation and optimizing the preparation method thereof, and the initial permeability of the prepared material is significantly higher than that of the common high-impedance ferrite prepared in the comparative example 11 at the temperature of about 25 ℃ at normal temperature, so that the broadband high-impedance ferrite in the embodiment 2 of the present invention can exhibit higher impedance characteristics, higher curie temperature and higher practical value in the frequency band of 1-100MHz compared with the common high-impedance ferrite. In fig. 1, temperature is Temperature, and μi is initial permeability.
The results prove that the manganese-zinc ferrite material with high initial permeability, high Curie temperature and high direct current resistivity and high impedance characteristic in a wide frequency range is obtained by reasonably adjusting the formulas of the main components and the auxiliary components of the manganese-zinc ferrite material.
Claims (6)
1. The manganese-zinc ferrite material is characterized in that raw materials for preparing the manganese-zinc ferrite material comprise a main component and an auxiliary component; the main component comprises Fe 2 O 3 、Mn 3 O 4 ZnO, wherein the main component is 64.2wt% of Fe 2 O 3 23.3wt% Mn 3 O 4 And 12.5wt% ZnO;
or, the main component is 63.5wt% of Fe 2 O 3 22.3wt% Mn 3 O 4 And 14.2wt% ZnO;
or, the main component is 66.5wt% of Fe 2 O 3 18.3wt% Mn 3 O 4 And 15.2wt% ZnO;
based on the total weight of the main componentsThe auxiliary component is Co 1.00wt% 2 O 3 0.02wt% CaCO 3 V0.015 wt% 2 O 5 ；
The preparation method of the manganese zinc ferrite material comprises the following steps:
placing the components of the main components into a ball mill, mixing for 0.5 hour, taking out and drying to obtain powder, and presintering the powder at 830 ℃ for 2.0 hours by using a box-type resistance furnace; then placing the presintered powder into a ball mill, and adding auxiliary components into the obtained powder; adding 50wt% of deionized water based on the total mass of the main component and 1.5wt% of polyacrylic acid dispersing agent based on the total mass of the main component, and performing ball milling until the average granularity is 1.0 mu m; adding an aqueous solution of polyvinyl alcohol into the powder, wherein the addition amount of the aqueous solution of the polyvinyl alcohol is 7wt% of the total mass of the powder after ball milling, uniformly mixing and granulating, and pressing the granules into an annular sample with the outer diameter of OR25mm, the height of 8mm and the inner diameter of 15 mm; finally, the temperature is kept for 5 hours in a bell jar furnace controlled by a computer program at 1320 ℃, and then the temperature is slowly reduced and cooled to 180 ℃ for discharging; wherein the oxygen partial pressure of the heat preservation section is 4.0%, and the temperature reduction process adopts the equilibrium oxygen partial pressure.
2. The method for preparing the manganese-zinc-ferrite material according to claim 1, comprising the steps of:
placing the components of the main components into a ball mill, mixing for 0.5 hour, taking out and drying to obtain powder, and presintering the powder at 830 ℃ for 2.0 hours by using a box-type resistance furnace; then placing the presintered powder into a ball mill, and adding auxiliary components into the obtained powder; adding 50wt% of deionized water based on the total mass of the main component and 1.5wt% of polyacrylic acid dispersing agent based on the total mass of the main component, and performing ball milling until the average granularity is 1.0 mu m; adding an aqueous solution of polyvinyl alcohol into the powder, wherein the addition amount of the aqueous solution of the polyvinyl alcohol is 7wt% of the total mass of the powder after ball milling, uniformly mixing and granulating, and pressing the granules into an annular sample with the outer diameter of OR25mm, the height of 8mm and the inner diameter of 15 mm; finally, the temperature is kept for 5 hours in a bell jar furnace controlled by a computer program at 1320 ℃, and then the temperature is slowly reduced and cooled to 180 ℃ for discharging; wherein the oxygen partial pressure of the heat preservation section is 4.0%, and the temperature reduction process adopts the equilibrium oxygen partial pressure.
3. A manganese-zinc ferrite material is characterized in that raw materials for preparing the manganese-zinc ferrite material comprise a main component and an auxiliary component, wherein the main component is 65.1 weight percent of Fe according to the mass percent 2 O 3 20.4wt% Mn 3 O 4 And 14.5wt% ZnO;
the auxiliary component is Co accounting for 0.80wt percent of the total weight of the main component 2 O 3 0.03wt% CaCO 3 ；
Or, the auxiliary component is Co accounting for 0.80wt% of the total weight of the main component 2 O 3 0.01wt% CaCO 3 0.01wt% Nb 2 O 5 ；
Or, the auxiliary component is Co accounting for 1.20wt% of the total weight of the main component 2 O 3 0.02wt% CaCO 3 0.02wt% Nb 2 O 5 V0.01 wt% 2 O 5 ；
Or, the auxiliary component is Co accounting for 0.60 weight percent of the total weight of the main component 2 O 3 0.03wt% CaCO 3 V0.02 wt% 2 O 5 ；
The preparation method of the manganese zinc ferrite material comprises the following steps:
placing the components of the main components into a ball mill, mixing for 0.5 hour, taking out and drying to obtain powder, and presintering the powder at 800 ℃ for 2.5 hours by using a box-type resistance furnace; then placing the presintered powder into a ball mill, and adding auxiliary components into the obtained powder; adding 50wt% of deionized water based on the total mass of the main component and 1.5wt% of polyacrylic acid dispersing agent based on the total mass of the main component, and performing ball milling until the average granularity is 1.0 mu m; adding an aqueous solution of polyvinyl alcohol into the powder, wherein the addition amount of the aqueous solution of the polyvinyl alcohol is 7wt% of the total mass of the powder after ball milling, uniformly mixing and granulating, and pressing the granules into an annular sample with the outer diameter of OR25mm, the height of 8mm and the inner diameter of 15 mm; finally, the temperature is kept for 6 hours in a bell jar furnace controlled by a computer program at 1300 ℃, and then the temperature is slowly reduced and cooled to 180 ℃ for discharging; wherein the oxygen partial pressure of the heat preservation section is 3.0%, and the temperature reduction process adopts the equilibrium oxygen partial pressure.
4. A method of preparing a manganese zinc ferrite material according to claim 3, comprising the steps of:
placing the components of the main components into a ball mill, mixing for 0.5 hour, taking out and drying to obtain powder, and presintering the powder at 800 ℃ for 2.5 hours by using a box-type resistance furnace; then placing the presintered powder into a ball mill, and adding auxiliary components into the obtained powder; adding 50wt% of deionized water based on the total mass of the main component and 1.5wt% of polyacrylic acid dispersing agent based on the total mass of the main component, and performing ball milling until the average granularity is 1.0 mu m; adding an aqueous solution of polyvinyl alcohol into the powder, wherein the addition amount of the aqueous solution of the polyvinyl alcohol is 7wt% of the total mass of the powder after ball milling, uniformly mixing and granulating, and pressing the granules into an annular sample with the outer diameter of OR25mm, the height of 8mm and the inner diameter of 15 mm; finally, the temperature is kept for 6 hours in a bell jar furnace controlled by a computer program at 1300 ℃, and then the temperature is slowly reduced and cooled to 180 ℃ for discharging; wherein the oxygen partial pressure of the heat preservation section is 3.0%, and the temperature reduction process adopts the equilibrium oxygen partial pressure.
5. Use of a manganese-zinc-ferrite material according to claim 1 or 3 for the manufacture of an inductive device.
6. An anti-electromagnetic interference material, characterized in that the raw materials for preparing the anti-electromagnetic interference material comprise the manganese-zinc ferrite material as claimed in claim 1 or 3.
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