CN115536381A - Manganese zinc ferrite material with high saturation magnetic flux density and low loss - Google Patents
Manganese zinc ferrite material with high saturation magnetic flux density and low loss Download PDFInfo
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- CN115536381A CN115536381A CN202211280638.6A CN202211280638A CN115536381A CN 115536381 A CN115536381 A CN 115536381A CN 202211280638 A CN202211280638 A CN 202211280638A CN 115536381 A CN115536381 A CN 115536381A
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- 239000000463 material Substances 0.000 title claims abstract description 55
- 230000004907 flux Effects 0.000 title claims abstract description 42
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 title claims abstract description 31
- 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 31
- 239000000843 powder Substances 0.000 claims abstract description 26
- 238000005245 sintering Methods 0.000 claims abstract description 23
- 238000000280 densification Methods 0.000 claims abstract description 13
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims abstract description 9
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 7
- 229910000859 α-Fe Inorganic materials 0.000 claims description 32
- 238000002156 mixing Methods 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 238000005259 measurement Methods 0.000 claims description 9
- 239000011701 zinc Substances 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000011572 manganese Substances 0.000 claims description 8
- 230000035699 permeability Effects 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 6
- 239000008187 granular material Substances 0.000 claims description 6
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 6
- 239000011118 polyvinyl acetate Substances 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- 239000004576 sand Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000001238 wet grinding Methods 0.000 claims description 4
- 239000002518 antifoaming agent Substances 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000011946 reduction process Methods 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- 239000000853 adhesive Substances 0.000 claims description 2
- 230000001070 adhesive effect Effects 0.000 claims description 2
- 239000011236 particulate material Substances 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 16
- 239000013078 crystal Substances 0.000 abstract description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 13
- 238000009826 distribution Methods 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 238000007792 addition Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 239000011148 porous material Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 3
- 239000013530 defoamer Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 238000003746 solid phase reaction Methods 0.000 description 3
- 229910002548 FeFe Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- WJZHMLNIAZSFDO-UHFFFAOYSA-N manganese zinc Chemical compound [Mn].[Zn] WJZHMLNIAZSFDO-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910001308 Zinc ferrite Inorganic materials 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- WGEATSXPYVGFCC-UHFFFAOYSA-N zinc ferrite Chemical compound O=[Zn].O=[Fe]O[Fe]=O WGEATSXPYVGFCC-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a manganese-zinc ferrite material with high saturation magnetic flux density and low loss, belonging to the technical field of manganese-zinc ferrite materials, comprising a main component and an auxiliary component, wherein the main component comprises Fe 2 O 3 63.0-72.0 mol%, znO 8.0-10.0 mol%, and the balance MnO; the auxiliary component is SiO 2 、CaCO 3 、Nb 2 O 5 、ZrO 2 、MoO 3 ,TiO 2 、V 2 O 5 . The addition amount of the auxiliary components is optimized and combined, the reasonable powder particle size distribution is controlled, the temperature of a sintering condition heating section is optimized, the problems that the manganese-zinc ferrite material with the main component iron oxide content of more than 60mol% is difficult to densify, the crystal grain is large and the distribution is uneven are solved, and the high densification rate of the manganese-zinc ferrite material with the main component iron oxide content of more than 63mol% is realizedHaving a Bs higher than 500mT at a high temperature of 100 ℃ and a loss lower than 1900kW/m 3 And (4) performance.
Description
Technical Field
The invention belongs to the technical field of manganese-zinc ferrite materials, and particularly relates to a manganese-zinc ferrite material with high saturation magnetic flux density and low loss.
Background
The saturation resistance of the magnetic element is mainly determined by the saturation magnetic flux density of the soft magnetic material, and the higher the saturation magnetic flux density of the material is, the higher the current can be resisted under the same condition. The magnetic core with the same current and the same shape can be smaller in volume for the material with higher saturation magnetic flux density. The ferrite material has a lower saturation magnetic flux density than the metal powder core, but has a high permeability and resistivity, and has less loss when used at high frequencies. Therefore, in the high power density power converter, the PFC inductor, the transformer and the power inductor are generally made of high-saturation low-loss ferrite soft magnetic materials.
Along with the development of electronic complete machine equipment towards the direction of light weight and miniaturization, the requirements on the volume of a transformer, a PFC inductor, a filter and a power inductor are smaller and smaller, and the requirements on the initial permeability, the saturation magnetic flux density, the low loss and other properties of the manganese-zinc ferrite material are more and more strict.
In the field of high saturation magnetic flux density and low loss Mn-Zn ferrite material, TDK of Japan reported that saturation magnetic flux density Bs at 100 ℃ is 500mT and loss at 100 ℃ is 500kWm under the condition of adding NiO -3 The materials are left and right, but the addition of NiO causes the price of the ferrite material to be too high; hitachi metals have also been reported in ICF as having a 100 ℃ saturation magnetic flux density Bs at 550mT and a 100 ℃ loss at 1300kWm -3 The material of (a); the commercially available transverse Shandong magnetic DMR28 material has a saturation magnetic flux density Bs of more than or equal to 490mT at 100 ℃, but the 100 ℃ loss is 1350kWm -3 The main component of manganese-zinc ferrite is composed of three components of iron, manganese and zinc, the 100 ℃ saturation magnetic flux density is 510mT,100kHz and 200mT, the 100 ℃ loss reaches 750kWm -3 No report is made.
Disclosure of Invention
In order to solve the technical problems mentioned in the background technology, the invention provides a manganese zinc ferrite material with high saturation magnetic flux density and low loss.
The purpose of the invention can be realized by the following technical scheme:
high saturation magnetic flux density is lowThe loss manganese-zinc ferrite material comprises a main component and an auxiliary component, wherein the main component comprises Fe 2 O 3 63.0-72.0 mol%, znO 8.0-10.0 mol%, and the balance MnO; the auxiliary component is SiO 2 、CaCO 3 、Nb 2 O 5 、ZrO 2 、MoO 3 、TiO 2 、V 2 O 5 。
Further, the total mass percentage of the auxiliary components in the main component is as follows: siO 2 2 :0.005~0.015wt%,CaCO 3 :0.15~0.2wt%,Nb 2 O 5 :0.005~0.03wt%,ZrO 2 :0.005~0.03wt%,V 2 O 5 :0~0.03wt%,MoO 3 :0.005~0.03wt%,TiO 2 :0.05~0.3wt%。
Further, the ferrite material has a saturation magnetic flux density of more than 500mT at 100 ℃ under 1194A/m measurement conditions; the ferrite material has an initial permeability greater than 900 at normal temperature; the ferrite material has the loss of less than 1900kWm at 100 ℃ under the measurement condition of 100kHz and 200mT -3 (ii) a The densification rate of the ferrite material is more than 96%.
Further, the ferrite material has an initial permeability higher than 1400 at normal temperature.
Further, the ferrite material has a loss of less than 750kW/m at 100 ℃ under the measurement conditions of 100kHz,200mT 3 。
Further, the ferrite material has a saturation magnetic flux density of more than 510mT at 100 ℃ under the measurement condition of 1194A/m.
Further, the manganese zinc ferrite material with high saturation magnetic flux density and low loss is prepared by the following steps:
step 1): raw material Fe 2 O 3 、Mn 3 O 4 Wet grinding and mixing the ZnO and the raw materials in a sand mill for 15 to 30min according to a proportion, uniformly mixing the raw materials and drying the raw materials in a drying oven at 120 to 125 ℃;
step 2): pre-burning the powder obtained in the step 1) at 800-1000 ℃ for 1-3 h;
and step 3): adding auxiliary components into the powder obtained in the step 2) in proportion, and then adding 30-80 wt% of deionized water, 0.5-1 wt% of dispersing agent and 0.5-3 wt% of defoaming agent which are measured by the total weight of the main components for ball milling;
step 4): based on the total weight of the powder obtained in the step 3), adding 0.8-1.0 wt% of PVA (polyvinyl acetate) adhesive into the powder obtained in the step 3), and uniformly mixing and granulating to obtain granules;
step 5): using 1-1.5T/cm 2 Pressing the particulate material into a green body sample;
step 6): sintering the green body sample obtained in the step 5) at the sintering temperature of 1250-1350 ℃ for 3-5 h, cooling to below 200 ℃, and discharging, wherein the oxygen partial pressure of the heat preservation section is 0.5-5%, and the balanced oxygen partial pressure is adopted in the temperature reduction process.
Furthermore, the granularity D50 of the powder after ball milling of the main component and the auxiliary component is controlled to be 0.8-1.5 μm.
Further, when the temperature is raised to be 100-200 ℃ lower than the sintering temperature, the temperature is preserved for 2-4 h under the nitrogen atmosphere, and then the temperature is raised to the sintering temperature.
The dispersant and the defoamer can be commonly used in the field, for example, n-octanoic acid can be selected as the defoamer, ammonium citrate can be selected as the dispersant, and the like.
The equilibrium oxygen partial pressure in the cooling section is according to the formula lg (P (O) 2 ) And) = a-b/T to calculate the oxygen partial pressure of different temperature points, wherein a takes 5-10, b takes 10000-15000 and T is absolute temperature.
The invention has the beneficial effects that:
the invention adds six or more than six auxiliary components SiO 2 、CaCO 3 、Nb 2 O 5 、V 2 O 5 、ZrO 2 、TiO 2 、MoO 3 The addition amount is optimized and combined, and the manganese zinc ferrite material with the main component iron oxide content of more than 60mol percent in the manganese zinc ferrite is difficult to densify, has large crystal grains and is divided into different components by combining the optimization design of a sintering condition temperature raising section temperature platform on the basis of controlling reasonable powder particle size distributionThe difficult problem of uneven distribution is realized, the high densification rate of the manganese-zinc ferrite material with the main component of iron oxide content more than 63mol percent is realized, the Bs is higher than 500mT and the loss is lower than 1900kW/m at the high temperature of 100 DEG C 3 And (4) performance.
The content of the main component iron oxide in the invention is more than 63mol percent and is far higher than that of the common manganese-zinc ferrite material. The iron oxide content in the composition is high, which is beneficial to obtaining high saturation magnetic flux density, but in the 1150-1250 ℃ stage of sintering temperature rise, along with Fe 2 O 3 →FeFe 2 O 4 +O 2 The reaction at ↓ proceeds, releasing a large amount of oxygen. According to the solid phase sintering theory, in the middle stage of sintering of ferrite materials, along with the discharge of gas, the movement of a grain boundary is driven, the rapid growth of crystal grains is promoted, and simultaneously, along with the rapid growth of the crystal grains, closed isolated pores are formed in the ferrite. Therefore, the control of the densification rate, the grain size and the uniformity of the manganese-zinc ferrite material with the over-high iron oxide content in the main composition is the difficult problem to be solved for realizing the high performance of the manganese-zinc ferrite.
Nb in the invention 2 O 5 ,ZrO 2 ,MoO 3 ,TiO 2 Adding plasma to FeFe 2 O 4 The spinel generation stage hinders the problem that the grain boundary is too fast caused by gas discharge, and meanwhile, a certain vacancy is formed in the ferrite by adding the high-valence ions, and the solid phase reaction can be promoted through the vacancy, so that the addition amount is optimized through different combinations, the growth speed of crystal grains can be effectively controlled in the temperature rise stage, the gas discharge is promoted, the densification rate of the manganese-zinc ferrite material is improved, the existence of air holes in the ferrite material is reduced, the grain boundary resistance of the ferrite material can be improved, and the loss is reduced.
SiO in the invention 2 ,CaCO 3 ,V 2 O 5 The additives have the fluxing function, and can be distributed in the crystal boundary, so that the resistance of the crystal boundary is effectively improved, and the loss is reduced. The invention combines the design of a constant temperature platform in the sintering temperature rise stage, and can effectively solve the problem of SiO 2 ,CaCO 3 ,V 2 O 5 The addition of a large amount of manganese causes abnormal growth of grains, and the manganese content is increasedThe densification rate and the resistivity of the zinc ferrite have obvious effects of improving the saturation magnetic flux density and reducing the loss.
The sintering condition is set in a constant temperature platform at the temperature rise stage, a part of solid phase reaction can be carried out at a lower temperature, fine powder in the powder particle size is reacted first, the subsequent powder particle size participating in the solid phase reaction at a high temperature is more uniform and larger in particle size, the growth speed of the high-temperature-stage crystal grains is controlled, a large amount of low-temperature cosolvent is added, the rapid crystal grain growth can be avoided, isolated holes and oversized crystal grains are formed, the densification rate of the manganese-zinc ferrite is effectively improved, the size and the particle size distribution of the crystal grains are controlled, and the effects of improving the saturation magnetic flux density of the manganese-zinc ferrite and reducing the loss are obvious.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic view of the structure of an abrasive surface in example 7 of the present invention;
FIG. 2 is a schematic view of the microstructure in example 7 of the present invention;
FIG. 3 is a schematic view showing the structure of an abrasive surface in comparative example 6 of the present invention;
FIG. 4 is a schematic structural view of the microstructure in comparative example 6 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
The manganese zinc ferrite material with high saturation magnetic flux density and low loss is prepared by the following steps:
step 1): comprises a main component and an auxiliary component;
the main component comprising Fe 2 O 3 63.0-72.0 mol%, znO 8.0-10.0 mol%, and the balance MnO.
The auxiliary component is selected from SiO 2 、CaCO 3 、Nb 2 O 5 、ZrO 2 、V 2 O 5 、MoO 3 、TiO 2 (ii) a The total mass percentage of the main components is as follows: siO 2 2 :0.005~0.015wt%,CaCO 3 :0.15~0.2wt%,Nb 2 O 5 :0.005~0.03wt%,ZrO 2 :0.005~0.03wt%,V 2 O 5 :0~0.03wt%,MoO 3 :0.005~0.03wt%,TiO 2 :0.05~0.3wt%;
Mixing Fe 2 O 3 、Mn 3 O 4 Wet-grinding and mixing the ZnO and the ZnO in a sand mill for 15min according to a proportion, uniformly mixing the raw materials, taking out and drying in a drying box;
step 2): presintering the powder obtained in the step 1) for 3 hours at the temperature of 800-1000 ℃;
and step 3): adding auxiliary components into the powder obtained in the step 2) in proportion, adding 30-80 wt% of deionized water, 0.5-1 wt% of dispersing agent and 0.5-3 wt% of defoaming agent which are measured by the total weight of the main components, and carrying out ball milling to ensure that the particle diameter D of the powder after ball milling is 50 Reaching 0.8-1.5 μm;
step 4): based on the total weight of the powder obtained in the step 3), adding PVA liquid with the solid content of 0.8-1.0 wt% into the powder obtained in the step 3), and uniformly mixing and granulating to obtain granules;
step 5): using 1-1.5T/cm 2 Pressing the granules into a T25 standard green body sample;
step 6): sintering the T25 standard green body sample obtained in the step 5) at the sintering temperature of 1250-1350 ℃, and preserving heat for 2-4 h in a nitrogen atmosphere when the temperature is raised to be 100-200 ℃ lower than the sintering temperature, wherein the oxygen partial pressure in a heat preservation section is 0.5-5%, the temperature reduction process adopts balanced oxygen partial pressure, and the temperature is reduced and cooled to be below 200 ℃ and then discharged from the furnace.
Example 1
Preparing a manganese-zinc power ferrite annular magnetic core:
step 1): with commercially available Fe 2 O 3 、Mn 3 O 4 And ZnO as raw material, and proportioning according to the measurement of component raw materials, wherein the main component contains Fe 2 O 3 69.0mol%, znO 9mol%, mnO 22mol%. First of all Fe 2 O 3 、Mn 3 O 4 Wet-grinding and mixing the ZnO and the ZnO in a sand mill for 15min according to a proportion, uniformly mixing the raw materials, taking out and drying in a drying box;
step 2): pre-burning the powder obtained in the step 1) at 900 ℃ for 3h;
and step 3): adding auxiliary components into the powder obtained in the step 2); the auxiliary components account for the total mass percentage of the main components as follows: siO 2 2 In an amount of 0.005 wt.% CaCO 3 Amount 0.06wt%, zrO 2 Amount 0.015wt%, nb 2 O 5 Amount 0.02wt%, tiO 2 Amount 0.15wt%, moO 3 Amount 0.02wt%;
then adding 60wt% of deionized water, 0.8wt% of dispersant and 1wt% of defoamer which are measured by the total weight of the main components, and carrying out ball milling to ensure that the particle size D of the powder after ball milling is 50 Reaching 1.0-1.1 μm;
and step 4): based on the total weight of the powder obtained in the step 3), adding 1.0wt% of PVA liquid based on the solid content into the powder obtained in the step 3), and uniformly mixing and granulating to obtain granules;
step 5): using a 1T/cm 2 Pressing the granules into a T25 standard green body sample;
step 6): sintering the T25 green body sample obtained in the step 5) at the sintering temperature of 1300 ℃, preserving heat for 5 hours, wherein the oxygen partial pressure in the heat preservation section is 2.0%, balancing the oxygen partial pressure in the cooling process, cooling to below 200 ℃, and discharging.
Example 2-example 12
With reference to the conditions of example 1:
fe as the main component 2 O 3 69.0mol% of ZnO, 9mol% of ZnO,MnO accounts for 22mol%;
the auxiliary components account for the total mass percentage of the main components as follows: siO 2 2 In an amount of 0.005 wt.% CaCO 3 In an amount of 0.06 wt.%, without addition of V 2 O 5 (ii) a Adjusting ZrO 2 、Nb 2 O 5 、TiO 2 、MoO 3 High-valence and large-radius ion trace element dosage. The product properties were tested and the results are shown in table 1 below:
TABLE 1
By introducing high-valence large-radius ions and optimizing the addition amount, the densification rate is effectively improved, and the electromagnetic properties such as saturation magnetic flux density, loss, magnetic conductivity and the like are effectively optimized. From the microstructure, the size of the magnetic core grain is 15-25 μm, most of the air holes are positioned at the grain boundary, the internal air holes of the grain are obviously reduced, and the performances such as magnetic conductivity, loss and the like are effectively optimized, but more air holes exist at the grain boundary.
Example 13 example 23
With reference to the conditions of example 1:
fe as the main component 2 O 3 69.0mol%, 9mol% ZnO, 22mol% MnO;
the auxiliary components account for the total mass percentage of the main components as follows: zrO (ZrO) 2 Amount 0.015wt%, nb 2 O 5 Amount 0.02wt%, tiO 2 Amount 0.15wt%, moO 3 Amount 0.02wt%;
by SiO 2 、CaCO 3 、V 2 O 5 Adjusting the addition amount, setting a constant temperature platform at 1150-1185 ℃ in combination with sintering conditions, keeping the temperature for 3 hours in a nitrogen atmosphere, then heating to the sintering heat preservation temperature, and testing the product performance, wherein the test results are shown in the following table 2:
TABLE 2
From the data in table 2, it can be seen that the high saturation magnetic flux density and low loss manganese zinc ferrite prepared in the examples has a densification rate of more than 98.5%, uniform crystal grain size, and an average crystal grain size of about 15 μm to 25 μm, and the magnetic properties thereof are measured as follows:
1. the high saturation magnetic flux density low loss manganese zinc ferrite may have an initial permeability higher than 1400 at normal temperature.
2. The high saturation magnetic flux density low loss manganese zinc ferrite is made into a T25 standard sample ring, the loss characteristics are tested under the conditions of 5Ts,100kHz and 200mT, and the loss at 100 ℃ can be lower than 750kW/m 3 。
3. The high saturation magnetic flux density low loss Mn-Zn ferrite is made into T25 standard ring, and the Bs at 100 ℃ can be higher than 510mT under the conditions of 20Ts, 1194A/m.
From the test results, it is known that SiO passes through a low melting point 2 ,CaCO 3 ,V 2 O 5 And the like, and the setting of a heat preservation platform of the heating part is combined, so that the densification rate can be effectively improved, the saturation magnetic flux density and the magnetic conductivity can be improved, and the loss can be reduced. The microstructure observation of the magnetic core shows that the number of pores at the grain boundary is obviously reduced, the grain size is maintained in the range of 15-25 mu m, and the grain size is not obviously increased.
Comparative examples 1 to 12
With reference to the conditions of example 1, siO alone was added as an auxiliary component 2 In an amount of 0.005 wt.% CaCO 3 Amount 0.06 wt.%, varying Fe 2 O 3 MnO and ZnO, and then subjecting the resulting manganese-zinc-ferrite toroidal core to magnetic property tests, the performance parameters of which are shown in table 3:
TABLE 3
As can be seen from the data in Table 3, the amount of the minor components is reduced and the main composition is accompanied by Fe 2 O 3 The amount increases, the saturation magnetic flux density increases at 100 ℃, but the loss increases at 100 ℃. From the microstructure, as the amount of iron oxide in the main composition increases, the number of voids in the magnetic core increases, and the crystal grains become largeThe grain size is as small as 10-60 μm, and many pores are surrounded by oversized grains, so that the densification rate is reduced (densification rate = magnetic core density/magnetic core theoretical density), and the gas is not discharged in time because the grains are surrounded by the grains due to the high grain generation speed in the sintering process.
As shown in fig. 1-4, when compared with example 7 and comparative example 6, the ground surface of comparative example 6 shows that the manganese-zinc power ferrite toroidal core prepared in example 7 has a large number of air holes and a large volume of the second air holes; in the microstructure of comparative example 6, the number of pores in which pores are located inside the crystal grains is large and also large, and the average crystal grain size is large.
In the description of the specification, reference to the description of "one embodiment," "an example," "a specific example" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (9)
1. The manganese-zinc ferrite material with high saturation magnetic flux density and low loss is characterized by comprising a main component and an auxiliary component, wherein the main component comprises Fe 2 O 3 63.0-72.0 mol%, znO 8.0-10.0 mol%, and the balance MnO; the auxiliary component comprises SiO 2 、CaCO 3 、Nb 2 O 5 、ZrO 2 、MoO 3 、TiO 2 、V 2 O 5 。
2. A shank as set forth in claim 1The manganese-zinc ferrite material with the saturated magnetic flux density and the low loss is characterized in that the total mass percentage of the auxiliary components in the main component is as follows: siO 2 2 :0.005~0.015wt%,CaCO 3 :0.15~0.2wt%,Nb 2 O 5 :0.005~0.03wt%,ZrO 2 :0.005~0.03wt%,V 2 O 5 :0~0.03wt%,MoO 3 :0.005~0.03wt%,TiO 2 :0.05~0.3wt%。
3. The high saturation magnetic flux density low loss Mn-Zn ferrite material according to claim 2, wherein the ferrite material has a saturation magnetic flux density higher than 500mT at 100 ℃ under 1194A/m measurement; the ferrite material has initial permeability greater than 900 at normal temperature; the ferrite material has the loss of less than 1900kWm at 100 ℃ under the measurement condition of 100kHz and 200mT -3 (ii) a The densification rate of the ferrite material is more than 96%.
4. The Mn-Zn ferrite material with high saturation magnetic flux density and low loss of claim 2, wherein the ferrite material has an initial permeability higher than 1400 at normal temperature.
5. The Mn-Zn ferrite material with high saturation magnetic flux density and low loss as claimed in claim 2, wherein the ferrite material has a loss of less than 750kW/m at 100 ℃ under the measurement conditions of 100kHz,200mT 3 。
6. The high saturation magnetic flux density low loss Mn-Zn ferrite material according to claim 2, wherein the saturation magnetic flux density of the ferrite material is higher than 510mT at 1194A/m measurement at 100 ℃.
7. The high saturation flux density low loss manganese zinc ferrite material according to claim 2, wherein said high saturation flux density low loss manganese zinc ferrite material is prepared by the steps of:
step 1): raw material Fe 2 O 3 、Mn 3 O 4 Wet grinding and mixing the ZnO and the raw materials in a sand mill for 15 to 30min according to a proportion, uniformly mixing the raw materials and drying the raw materials in a drying oven at 120 to 125 ℃;
step 2): pre-burning the powder obtained in the step 1) for 1 to 3 hours at a temperature of between 800 and 1000 ℃;
step 3): adding auxiliary components into the powder obtained in the step 2) in proportion, and then adding 30-80 wt% of deionized water, 0.5-1 wt% of dispersing agent and 0.5-3 wt% of defoaming agent which are measured by the total weight of the main components for ball milling;
step 4): based on the total weight of the powder obtained in the step 3), adding 0.8-1.0 wt% of PVA (polyvinyl acetate) adhesive into the powder obtained in the step 3), and uniformly mixing and granulating to obtain granules;
step 5): using 1-1.5T/cm 2 Pressing the particulate material into a green body sample;
step 6): sintering the green body sample obtained in the step 5) at the sintering temperature of 1250-1350 ℃ for 3-5 h, cooling to below 200 ℃, and discharging, wherein the oxygen partial pressure of the heat preservation section is 0.5-5%, and the balanced oxygen partial pressure is adopted in the temperature reduction process.
8. The Mn-Zn ferrite material with high saturation magnetic flux density and low loss as claimed in claim 7, wherein the powder particle size D50 of the main component and the auxiliary component after ball milling is controlled to be 0.8-1.5 μm.
9. The Mn-Zn ferrite material with high saturation magnetic flux density and low loss as claimed in claim 7, wherein the temperature is maintained for 2-4 h under nitrogen atmosphere when the temperature is raised to 100-200 ℃ lower than the sintering temperature, and then the temperature is raised to the sintering temperature.
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