CN117776700A - High-permeability Mn-Zn ferrite broadband material KAH150 material and preparation method thereof - Google Patents
High-permeability Mn-Zn ferrite broadband material KAH150 material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 101
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 31
- 230000035699 permeability Effects 0.000 claims abstract description 26
- 238000005469 granulation Methods 0.000 claims abstract description 9
- 230000003179 granulation Effects 0.000 claims abstract description 9
- 239000007921 spray Substances 0.000 claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000004576 sand Substances 0.000 claims description 23
- 238000003801 milling Methods 0.000 claims description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- 239000001301 oxygen Substances 0.000 claims description 12
- 230000000630 rising effect Effects 0.000 claims description 10
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 9
- 239000008187 granular material Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 238000012360 testing method Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000002002 slurry Substances 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims 6
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 claims 2
- 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 claims 2
- 239000002994 raw material Substances 0.000 abstract description 5
- 239000000843 powder Substances 0.000 description 10
- 238000004321 preservation Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 235000013619 trace mineral Nutrition 0.000 description 3
- 239000011573 trace mineral Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
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Abstract
The embodiment of the invention discloses a high-permeability Mn-Zn ferrite broadband material KAH150 material and a preparation method thereof, wherein the material has a permeability ui within the range of 10000-15000 +/-25% under the frequency condition of 10-200 KHZ; the Curie temperature Tc of the material is more than 130 ℃; the method comprises the following steps: according to Fe 2 O 3 51.2 to 54.5mol percent, 19.1 to 22.40mol percent of ZnO and the balance of MnO are proportioned to obtain raw materials; and sequentially performing ball milling, presintering, secondary sanding, spray granulation, blank preparation and sintering treatment on the raw materials to obtain the high-permeability Mn-Zn ferrite broadband material KAH 150. Through the combination adjustment of the fixed formula and the doping, the permeability of the material can be kept at more than or equal to 10000 at 200KHZ, and the high-frequency performance is greatly improved.
Description
Technical Field
The invention relates to the technical field of electronic material preparation, in particular to a high-permeability Mn-Zn ferrite broadband material KAH150 material and a preparation method thereof.
Background
For the broadband material KAH150 of the Mn-Zn ferrite, the current material with the permeability ui reaching 15000 generally starts to decline at the frequency point of 50KHZ, the frequency characteristic is poor, the frequency point ui reaching 200KHZ is reduced below 6000ui, the broadband characteristic is poor, and the requirement that customers need ui=15000 and broadband characteristics is not met. At present, the material with the magnetic permeability ui reaching 15000 can only reach 100 ℃, and can not meet the requirements of part of vehicle-mounted products and new energy products, namely, the requirement of high magnetic permeability and the requirement of high Curie temperature.
1. With the increasing requirements of electronic products, the high magnetic permeability of Mn-Zn reaches over 12000, not only can the number of turns be reduced and the cost be lowered, but also the product has the impedance effect with higher frequency. At present, although the current product with the ui reaching 15000 has the magnetic permeability ui reaching the level of 10KHZ, the ui falls seriously after 100KHZ, and the requirement of high-frequency characteristics after 100KHZ cannot be met.
2. The Curie temperature TC of the material with ui=15000 in the current market can only reach 100-105 ℃, and the Curie temperature of the material reaches 130 ℃ (the main component is different from the existing material).
3. According to the invention, through the average particle size control of powder ball milling, the addition of trace elements and the effective matching of a sintering process, the material with ui=15000 can reach a frequency permeability ui of 200KHZ of more than 10000.
4. The product of the invention can enable the design of the customer product, reduce the number of turns (reduce cost), improve the impedance, and has higher performance and market competitiveness.
1. The prior art has the following defects:
1) At present, although the magnetic permeability ui of 10KHZ reaches the level, the ui falls below 60% after 100KHZ, and the magnetic permeability of 200KHZ falls below 30%;
2) At present, the Curie temperature of the product with ui reaching 15000 is only 100-105 ℃, and the product has limitation on part of application fields.
The purpose of the invention is that: 1) The product design of customers can reduce the number of turns (reduce cost), improve impedance and realize higher performance and market competitiveness of the EMI product by using the product of the invention. 2) The problem that the Curie temperature Tc of the material with ui=15000 is lower is solved.
Disclosure of Invention
Aiming at the defects of the current material, the embodiment of the application provides a high-permeability Mn-Zn ferrite broadband material KAH150 material and a preparation method thereof, which are used for solving the problem that the current material cannot meet the requirements of high Curie temperature and high permeability.
The invention provides a high-permeability Mn-Zn ferrite broadband material KAH150 material, wherein the permeability ui is in the range of 10000-15000+/-25% under the frequency condition of 10-200 KHZ.
In one possible implementation, the curie temperature Tc of the material is > 130 ℃.
The high-permeability Mn-Zn ferrite broadband material KAH150 material comprises a main component and an auxiliary component; the main component is Fe 2 O 3 The auxiliary component is added doping material MoO 3 、Bi 2 O 3 、CaCO 3 、V 2 O 5 、CuO、TiO 2 、CO 2 O 3 、WO 3 Is a mixed material of the above materials.
In one possible implementation, the main component is according to Fe 2 O 3 51.2 to 54.5mol percent, 19.1 to 22.40mol percent of ZnO and 23.5 to 26.7mol percent of MnO.
In one possible implementation, the subcomponents are doped materials added respectively as follows: moO (MoO) 3 0.01-0.05wt% Bi 2 O 3 0.01 to 0.04 percent by weight of CaCO 3 0.005-0.04 wt% of V 2 O 5 0.01 to 0.04wt percent of CuO, 0.02 to 0.05wt percent of TiO 2 0.01-0.05wt% of CO 2 O 3 0.01-0.04wt%, WO 3 0.01 to 0.05wt%.
The invention provides a preparation method of a high-permeability Mn-Zn ferrite broadband material KAH150 material, which comprises the following steps:
step 1: ball milling for the first time: proportioning the main components, adding the materials and deionized water into a sand mill, and performing ball milling;
step 2: presintering: drying and granulating the materials in the step 1, and then placing the materials into a presintering furnace for presintering;
step 3: secondary ball milling: adding the pre-sintered material and the prepared auxiliary components in the step 2 into a sand mill, adding deionized water for secondary sand milling, and adding 8% PVA solution 10 minutes before the secondary sand milling is finished to prepare secondary slurry with the average particle size of 0.80-0.90 mu m;
step 4: granulating: carrying out spray granulation on the material in the step 3 to obtain particles with 80-120 meshes;
step 5: pressing the granules into a T25-15-8 blank by a press, wherein the density of the blank is 3.00-3.15g/cm < 3 >;
step 6: sintering the T25-15-8 blank in a bell jar kiln, keeping the sintering temperature at 1360-1440 ℃ for 5-8 hours, cooling the kiln to 120 ℃ to lower the kiln, taking out a sample, keeping the temperature at 22-27 ℃ for 3 hours, and testing.
In one possible implementation, the presintering in step 2 is performed at 870-960 ℃ for 1-3 hours.
In one possible implementation, the sintering of the step 6 is performed at the temperature rising section of 900-1150 ℃ and the temperature rising speed of 1.0 degree/min, and the oxygen content is controlled to be 0.1-1.0%.
In a possible implementation manner, in the step 6, the oxygen content of the rest of the heat preservation period except for 8% of the oxygen content of the last 1 hour is 20%, namely air sintering.
In one possible implementation, the sintered T25-15-8 sample of step 6 has a test density of not less than 5.0g/cm 3 。
The invention has the following beneficial effects:
(1) The high-permeability Mn-Zn ferrite broadband material KAH150 is prepared by adopting unique doping combination, grinding, pressing and sintering, wherein the main component determines that the Curie temperature reaches 130 ℃. The proper doping combination promotes better liquid phase sintering, promotes grain growth, grows more uniform grains, reduces the porosity of grain boundaries, and forms the characteristic of higher finished product density, so that the permeability of the material can be kept to more than 10000 at high frequency of 200KHZ, and a unique and excellent new material is formed.
(2) The common high magnetic permeability material has mixed trace elements of about 5 kinds, 8 kinds of trace elements are added, and the high frequency characteristic of the material is improved through the effective combination of the mixing amount.
(3) The material of the invention has the ui reaching the 15000 median level under the frequency of 10KHZ, but the magnetic permeability ui of the frequency point of 200KHZ is more than 2 times of that of the traditional material, and the high-frequency characteristic has obvious advantages.
(4) The material of the invention can reduce the number of turns of the coil of the EMI product and reduce the cost when a customer designs the product, and simultaneously obtains better high-frequency high-impedance characteristics, thereby being suitable for being applied to the field of vehicle-mounted and new energy with continuously improved requirements.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the present application and do not constitute a limitation on the invention.
In the drawings:
FIG. 1 is a flow chart of a preparation method of a high permeability Mn-Zn ferrite broadband material KAH150 material.
Fig. 2 is a graph comparing data of example 1 with those of comparative examples 1 and 2.
Detailed Description
In order to better understand the technical solutions in the present application, the following description will clearly and completely describe the technical solutions in the embodiments of the present application with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments herein without making any inventive effort, shall fall within the scope of the present application.
At present, the permeability ui reaches 15000, usually, the frequency point of 50KHZ begins to decrease, the frequency characteristic is poor, the frequency point ui reaches 200KHZ to below 6000ui, the broadband characteristic is poor, and the requirements of customers that the requirement ui=15000 and the broadband characteristic are needed to be obtained cannot be met.
At present, the material with the magnetic permeability ui reaching 15000 can only reach 100 ℃, and can not meet the requirements of part of vehicle-mounted products and new energy products, namely, the requirement of high magnetic permeability and the requirement of high Curie temperature.
The high-permeability Mn-Zn ferrite broadband material KAH150 material can achieve the magnetic permeability ui within 10000-15000 + -25% under the frequency condition of 10-200 KHZ. Compared with the prior art, the method has obvious improvement.
The Curie temperature Tc of the material is more than 130 ℃. The material is improved by 30 degrees compared with the existing material with the same ui, and the requirements of products in the fields of vehicle-mounted and new energy are met.
The material comprises a main component and an auxiliary component; the main component is Fe 2 O 3 The auxiliary component is added doping material MoO 3 、Bi 2 O 3 、CaCO 3 、V 2 O 5 、CuO、TiO 2 、CO 2 O 3 、WO 3 Is a mixed material of the above materials.
The main component of the invention is according to Fe 2 O 3 51.2 to 54.5mol percent, 19.1 to 22.40mol percent of ZnO and 23.5 to 26.7mol percent of MnO.
The auxiliary components of the invention are doped materials which are respectively as follows: moO (MoO) 3 0.01-0.05wt% Bi 2 O 3 0.01 to 0.04 percent by weight of CaCO 3 0.005-0.04 wt% of V 2 O 5 0.01 to 0.04wt percent of CuO, 0.02 to 0.05wt percent of TiO 2 0.01-0.05wt% of CO 2 O 3 Is 0.01-0.0.04wt％、WO 3 0.01 to 0.05wt%.
The key point of the invention is to effectively combine the doping type and the tragic amount, so that the internal crystal grains of the magnetic core are uniform, the porosity is reduced, and a novel material with high density and more reasonable microstructure is formed. The sintering densification arrangement of the invention also plays a great role in uniform crystallization inside the product. The high-permeability Mn-Zn ferrite broadband material KAH150 material needs to adopt a densification mode during sintering, so that grains can be uniformly grown, pores are reduced, and ui is improved.
Example 1:
as shown in figure 1, the preparation method of the high-permeability Mn-Zn ferrite broadband material KAH150 material comprises the following steps:
1) According to Fe 2 O 3 52.34mol%, znO 22.03mol% and MnO 25.63mol% to obtain raw materials; then adding proper deionized water into a sand mill for primary sand milling for 45 minutes, and then carrying out primary spray granulation.
2) Spraying the above materials, pre-sintering in a pre-sintering furnace at 860 deg.C for 3 hr;
3) Adding minor elements into the presintered granular material, wherein the adding amount of minor elements is as follows relative to the total weight of the main components:
MoO 3 0.02wt%, bi 2 O 3 0.02wt% CaCO 3 0.01wt%. V (V) 2 O 5 0.015wt% TiO 2 0.03wt% of CuO, 0.02wt% of Co 2 O 3 0.015wt%, WO 3 0.02 wt.%; 8 microelements are added.
4) Placing the powder containing the main component and the auxiliary component into a sand mill, performing secondary sand milling for 105 minutes, controlling the average grain diameter to be 0.80-0.85 mu m, adding PVA solution with the percentage concentration of 8% for 20 minutes before the secondary sand milling is finished, wherein the addition amount is 10% of the weight of the powder, then performing spray granulation, and sieving the powder by 60 meshes and 180 meshes.
5) Pressing the above granule into T25-15-8 blank, and compacting the blankThe degree is controlled to be 3.00-3.10 g/cm 3 。
6) Sintering the T25-15-8 blank in a bell kiln, wherein the sintering heat preservation temperature is 1360-1440 ℃, and the heat preservation time is 5-8 hours; in the temperature rising section 900-1150 ℃, the temperature rising speed is 1.0 degree/min, the oxygen content is controlled to be 0.1-1.0%, and the rest is air sintering except 8% of the oxygen content in the last 1 hour.
Comparative example 1:
the preparation method of the high-permeability Mn-Zn ferrite broadband material KAH150 material comprises the following steps:
1) According to Fe 2 O 3 52.34mol%, znO 22.03mol% and MnO 25.63mol% to obtain raw materials; then adding proper deionized water into a sand mill for primary sand milling for 45 minutes, and then carrying out primary spray granulation.
2) Spraying the above materials, pre-sintering in a pre-sintering furnace at 860 deg.C for 3 hr;
3) Adding minor elements into the presintered granular material, wherein the adding amount of minor elements is as follows relative to the total weight of the main components:
MoO 3 0.02wt%, bi 2 O 3 0.02wt% CaCO 3 0.01wt%. V (V) 2 O 5 0.01wt% of TiO 2 0.01 to 0.05wt%; 5 microelements are added.
4) Placing the powder containing the main component and the auxiliary component into a sand mill, performing secondary sand milling for 105 minutes, controlling the average grain diameter to be 0.80-0.85 mu m, adding PVA solution with the percentage concentration of 8% for 20 minutes before the secondary sand milling is finished, wherein the addition amount is 10% of the weight of the powder, then performing spray granulation, and sieving the powder by 60 meshes and 180 meshes.
5) Pressing the above granule material into T25-15-8 blank with blank density controlled at 3.00-3.10 g/cm 3 。
6) Sintering the T25-15-8 blank in a bell kiln, wherein the sintering heat preservation temperature is 1360-1440 ℃, and the heat preservation time is 5-8 hours; in the temperature rising section 900-1150 ℃, the temperature rising speed is 1.0 degree/min, the oxygen content is controlled to be 0.1-1.0%, and the rest is air sintering except 8% of the oxygen content in the last 1 hour.
Comparative example 2:
the preparation method of the high-permeability Mn-Zn ferrite broadband material KAH150 material comprises the following steps:
1) According to Fe 2 O 3 52.34mol%, znO 22.03mol% and MnO 25.63mol% to obtain raw materials; then adding proper deionized water into a sand mill for primary sand milling for 45 minutes, and then carrying out primary spray granulation.
2) Spraying the above materials, pre-sintering in a pre-sintering furnace at 860 deg.C for 3 hr;
3) Adding minor elements into the presintered granular material, wherein the adding amount of minor elements is as follows relative to the total weight of the main components:
MoO 3 0.02wt%, bi 2 O 3 0.02wt% CaCO 3 0.01wt%. V (V) 2 O 5 0.01wt% of TiO 2 0.02wt% of CuO and 0.02wt%; 6 microelements are added.
4) Placing the powder containing the main component and the auxiliary component into a sand mill, performing secondary sand milling for 105 minutes, controlling the average grain diameter to be 0.80-0.85 mu m, adding PVA solution with the percentage concentration of 8% for 20 minutes before the secondary sand milling is finished, wherein the addition amount is 10% of the weight of the powder, then performing spray granulation, and sieving the powder by 60 meshes and 180 meshes.
5) Pressing the above granule material into T25-15-8 blank with blank density controlled at 3.00-3.10 g/cm 3 。
6) Sintering the T25-15-8 blank in a bell kiln, wherein the sintering heat preservation temperature is 1360-1440 ℃, and the heat preservation time is 5-8 hours; in the temperature rising section 900-1150 ℃, the temperature rising speed is 1.0 degree/min, the oxygen content is controlled to be 0.1-1.0%, and the rest is air sintering except 8% of the oxygen content in the last 1 hour.
T25-15-8 of the above three schemes was kept at room temperature of 25℃for 3 hours and then tested, and the results are shown in FIG. 2.
The above results illustrate:
1) The material of the invention has the ui reaching the 15000 median level under the frequency of 10KHZ, but the magnetic permeability ui of the frequency point of 200KHZ is more than 2 times of that of the traditional material, and the high-frequency characteristic has obvious advantages.
2) The material adopts the main component proportion with the Curie temperature reaching 130 degrees, which is 30 degrees higher than the material with the current ui=15000 (Tc=100 degrees).
3) The material of the invention can reduce the number of turns of the coil of the EMI product and reduce the cost when a customer designs the product, and simultaneously obtains better high-frequency high-impedance characteristics, thereby being suitable for being applied to the field of vehicle-mounted and new energy with continuously improved requirements.
It is to be understood that, based on the several embodiments provided in the present application, those skilled in the art may combine, split, reorganize, etc. the embodiments of the present application to obtain other embodiments, where none of the embodiments exceed the protection scope of the present application.
The foregoing detailed description of the embodiments of the present application has further described the objects, technical solutions and advantageous effects thereof, and it should be understood that the foregoing is merely a specific implementation of the embodiments of the present application, and is not intended to limit the scope of the embodiments of the present application, and any modifications, equivalent substitutions, improvements, etc. made on the basis of the technical solutions of the embodiments of the present application should be included in the scope of the embodiments of the present application.
Claims (8)
1. The high-permeability Mn-Zn ferrite broadband material KAH150 material is characterized by comprising a main component and an auxiliary component; the main component is Fe 2 O 3 The auxiliary component is added doping material MoO 3 、Bi 2 O 3 、CaCO 3 、V 2 O 5 、CuO、TiO 2 、CO 2 O 3 、WO 3 Is a mixed material of the above materials.
2. The high permeability Mn-Zn ferrite broadband material KAH150 according to claim 1, wherein theThe main component is according to Fe 2 O 3 51.2 to 54.5mol percent, 19.1 to 22.40mol percent of ZnO and 23.5 to 26.7mol percent of MnO.
3. The high permeability manganese zinc ferrite broadband material KAH150 material according to claim 1, wherein the subcomponents are doped materials respectively: moO (MoO) 3 0.01-0.05wt% Bi 2 O 3 0.01 to 0.04 percent by weight of CaCO 3 0.005-0.04 wt% of V 2 O 5 0.01 to 0.04wt percent of CuO, 0.02 to 0.05wt percent of TiO 2 0.01-0.05wt% of CO 2 O 3 0.01 to 0.04wt%, WO 3 0.01 to 0.05wt%.
4. A method for preparing a high permeability manganese zinc ferrite broadband material KAH150 material according to claims 1-3, comprising the steps of:
step 1: ball milling for the first time: proportioning the main components, adding the materials and deionized water into a sand mill, and performing ball milling;
step 2: presintering: drying and granulating the materials in the step 1, and then placing the materials into a presintering furnace for presintering;
step 3: secondary ball milling: adding the pre-sintered material and the prepared auxiliary components in the step 2 into a sand mill, adding deionized water for secondary sand milling, and adding 8% PVA solution 10 minutes before the secondary sand milling is finished to prepare secondary slurry with the average particle size of 0.80-0.90 mu m;
step 4: granulating: carrying out spray granulation on the material in the step 3 to obtain particles with 80-120 meshes;
step 5: pressing the above granule material into T25-15-8 blank with density of 3.00-3.15g/cm 3 ；
Step 6: sintering the T25-15-8 blank in a bell jar kiln, keeping the sintering temperature at 1360-1440 ℃ for 5-8 hours, cooling the kiln to 120 ℃ to lower the kiln, taking out a sample, keeping the temperature at 22-27 ℃ for 3 hours, and testing.
5. The method for preparing the high-permeability Mn-Zn ferrite broadband material KAH150 according to claim 4, wherein the pre-sintering temperature in the step 2 is 870-960 ℃, and the pre-sintering time is 1-3 hours.
6. The method for preparing the high-permeability Mn-Zn ferrite broadband material KAH150 according to claim 4, wherein the sintering in the step 6 is performed at a temperature rising period of 900-1150 ℃ and a temperature rising rate of 1.0 degree/min, and the oxygen content is controlled to be 0.1-1.0%.
7. The method of preparing high permeability Mn-Zn ferrite broadband material KAH150 according to claim 4, wherein in step 6, the oxygen content in the rest of the heat-preserving period is 20% except 8% of the oxygen content in the last 1 hour, i.e. air sintering.
8. The method for preparing high permeability Mn-Zn ferrite broadband material KAH150 according to claim 4, wherein the test density of the sintered T25-15-8 sample in step 6 is not lower than 5.0g/cm 3 。
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