CN113292330A - High-cut-off frequency composite material, preparation method and common-mode inductor - Google Patents
High-cut-off frequency composite material, preparation method and common-mode inductor Download PDFInfo
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- CN113292330A CN113292330A CN202110722760.3A CN202110722760A CN113292330A CN 113292330 A CN113292330 A CN 113292330A CN 202110722760 A CN202110722760 A CN 202110722760A CN 113292330 A CN113292330 A CN 113292330A
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- 239000002131 composite material Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000498 ball milling Methods 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 17
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims description 81
- 238000005245 sintering Methods 0.000 claims description 33
- 239000011347 resin Substances 0.000 claims description 28
- 229920005989 resin Polymers 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 12
- 238000000151 deposition Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 9
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 8
- 229920000178 Acrylic resin Polymers 0.000 claims description 7
- 239000004925 Acrylic resin Substances 0.000 claims description 7
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 6
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 125000003158 alcohol group Chemical group 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 229920003086 cellulose ether Polymers 0.000 claims description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 13
- 229910052681 coesite Inorganic materials 0.000 abstract description 5
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 5
- 239000000377 silicon dioxide Substances 0.000 abstract description 5
- 229910052682 stishovite Inorganic materials 0.000 abstract description 5
- 229910052905 tridymite Inorganic materials 0.000 abstract description 5
- 238000005234 chemical deposition Methods 0.000 abstract description 4
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 18
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 14
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 7
- 239000011787 zinc oxide Substances 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000003466 welding Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000006247 magnetic powder Substances 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- 239000005751 Copper oxide Substances 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
The invention discloses a high-cut-off frequency composite material, a preparation method and a common-mode inductor. Co with refined crystal grains is added into the formula of the invention2O3、SiO2、Sb2O3The growth of crystal grains can be inhibited in the material crystallization process so as to control the size of the crystal grains and effectively refine the crystal grains; the oxides are mixed more uniformly by ball milling, so that the distribution of crystal grains is uniform, the cut-off frequency of the material is improved, uniform nonmagnetic gaps are formed locally by chemical deposition, and the cut-off frequency of the material is further improved. Therefore, the application requirements of the Internet of things and 5G can be fully met.
Description
Technical Field
The invention relates to the technical field of inductors, in particular to a high-cut-off-frequency composite material, a preparation method and a common-mode inductor.
Background
With the development of technologies such as the internet of things and the 5G, the transmission speed of signals is developed from 100Mbps to 1000Mbps or even higher transmission speed, and the frequency band of noise generation is higher and higher, so that a higher requirement is provided for the common mode inductance of the signal end for suppressing noise, that is, the same suppression effect is achieved in the higher frequency band. However, the conventional soft magnetic material has a large grain size due to the design of components and processes, so that resonance occurs at a high frequency to cut off, and a suppression effect cannot be achieved.
Accordingly, the prior art is deficient and needs improvement.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the high-cut-off-frequency composite material, the preparation method and the common-mode inductor are provided, and the application requirements of the Internet of things and 5G are met.
The technical scheme of the invention is as follows: a preparation method of a high-cut-off frequency composite material is provided, and comprises the following steps.
S1: weighing the following substances in proportion: 52-69.3 wt% Fe2O3、8-12wt％ZnO、5-10wt％CuO、17-22wt％NiO、0.1-1.0wt％Co2O3、0.1-0.5wt％SiO2、0.5-2.5wt％Sb2O3And mixing to obtain composite powder.
S2: and performing ball milling on the composite powder for 0.5-8h to obtain ball-milled powder. The ball milling enables the components to be mixed more uniformly.
S3: and (3) carrying out heat treatment on the powder subjected to ball milling for 0.5-6h in the air at the temperature of 700-900 ℃ to obtain first heat-treated powder. The impurities on the surface of the powder after ball milling can be removed at high temperature.
S4: taking first heat treatment powder with the grain diameter of 0.1-10um, and chemically vapor-depositing one or the mixture of at least two of an aluminum oxide layer, a silicon oxide layer and a bismuth oxide layer with the thickness of 0.01-0.3um on the surface of the first heat treatment powder with the grain diameter of 0.1-10um at the vacuum of 140-500 ℃ to obtain deposition powder.
S5: the deposition powder is treated for 0.5 to 6 hours in the air of 700-900 ℃ to obtain the high-cut-off frequency composite material. The high-temperature heat treatment can combine the first heat-treated powder with the aluminum oxide layer, the silicon oxide layer and the bismuth oxide layer on the surface of the first heat-treated powder better.
Added Co2O3、SiO2、Sb2O3Can effectively refine crystal grains and improve the cut-off frequency of the materialAnd a uniform nonmagnetic gap is locally formed through chemical deposition, so that the cut-off frequency of the material is further improved. Therefore, the application requirements of the Internet of things and 5G can be fully met.
Co with refined grains is added into the formula2O3、SiO2、Sb2O3The growth of crystal grains can be inhibited in the material crystallization process so as to control the size of the crystal grains and effectively refine the crystal grains; the oxides are mixed more uniformly by ball milling, so that the used crystal grains are uniformly distributed. The powder after ball milling forms a primary crystalline phase through the pre-sintering of the step S3 and removes impurities in the raw materials to ensure that crystal grains do not grow too large due to the impurities in the subsequent sintering process. In step S4, the nanoscale aluminum oxide layer, silicon oxide layer, and bismuth oxide layer that inhibit the growth of grains are uniformly deposited on the surface of the first heat-treated powder, so as to further control the size and uniformity of grains in the process of subsequent sintering into the common mode inductor, thereby ensuring that the size of grains is controlled at an extremely small level; and the chemically deposited aluminum oxide layer, silicon oxide layer and bismuth oxide layer can be uniformly distributed on the surface of the first heat treatment to form stable and uniform nonmagnetic gaps, so that the cut-off frequency of the material is further improved.
In step S4, the first heat-treated powder is pulverized in advance and then sieved to obtain the first heat-treated powder having a particle size of 0.1 to 10 um.
In step S2, after the ball milling is finished, drying is carried out for 0.5 to 12 hours at the temperature of between 60 and 300 ℃.
The ball milling in the step S2 is wet ball milling, and the solvent is alcohol or acetone or water.
The invention also provides a high-cut-off frequency composite material which is prepared by adopting the preparation method of the high-cut-off frequency composite material.
The invention also provides a common mode inductor, which adopts the high cut-off frequency composite material, uniformly mixes the high cut-off frequency composite material with the sintering resin solution, and dries the mixture for 1 to 20 hours at the temperature of between 70 and 300 ℃ to obtain the sintering material; wherein the weight of the sintering resin in the sintering resin solution is 0.01-0.5% of the weight of the high cut-off frequency composite material; and pressing the sintered material in a mold at the temperature of 50-200 ℃ under the pressure of 150-300 MPa to obtain an inductor blank, and sintering the inductor blank at the temperature of 1000-1600 ℃ for 1-10h to obtain the common mode inductor.
The sintering resin is acrylic resin or cellulose ether or polyvinyl butyral.
By adopting the scheme, the invention provides the high-cut-off-frequency composite material, the preparation method and the common-mode inductor, and Co is added2O3、SiO2、Sb2O3The crystal grains can be effectively refined, the cut-off frequency of the material can be improved, and uniform nonmagnetic gaps are formed locally through chemical deposition, so that the cut-off frequency of the material is further improved. Therefore, the application requirements of the Internet of things and 5G can be fully met.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1
The embodiment provides a preparation method of a high-cut-off frequency composite material, which comprises the following steps.
S1: weighing the following substances in proportion: 69.3 wt% Fe2O3、8wt％ZnO、5wt％CuO、17wt％NiO、0.1wt％Co2O3、0.1wt％SiO2、0.5wt％Sb2O3And mixing to obtain composite powder.
S2: and performing ball milling on the composite powder for 1h to obtain ball-milled powder.
S3: and (3) carrying out heat treatment on the powder subjected to ball milling for 1h in air at 900 ℃ to obtain first heat-treated powder.
S4: taking first heat treatment powder with the grain diameter of 0.1-10um, and chemically vapor depositing an aluminum oxide layer with the thickness of 0.02um on the surface of the first heat treatment powder with the grain diameter of 0.1-10um at the vacuum of 200 ℃ to obtain deposited powder.
S5: the deposited powder was treated in air at 700 ℃ for 3h to obtain a high cut-off frequency composite.
In step S4, the first heat-treated powder is pulverized in advance and then sieved to obtain the first heat-treated powder having a particle size of 0.1 to 10 um.
In step S2, after the completion of the ball milling, the mixture was dried at 120 ℃ for 8 hours.
The ball milling in the step S2 is wet ball milling, and the solvent is alcohol.
The embodiment also provides a common mode inductor, which adopts the high cut-off frequency composite material, uniformly mixes the high cut-off frequency composite material with a sintering resin solution, and dries the mixture at the temperature of 180 ℃ for 5 hours to obtain a sintering material; in the step, the high cut-off frequency composite material and the sintering resin solution are mixed in a mixer for 40 min; wherein the weight of the sintered resin in the sintered resin solution is 0.5% of the weight of the high cut-off frequency composite material; the sintered resin is acrylic resin.
Pressing the sintered material in a mold at the temperature of 150 ℃ under the pressure of 150MPa to prepare an inductor blank, and sintering the inductor blank at the temperature of 1200 ℃ for 4h to obtain the common-mode inductor; the parameters of the spot welding coil contained in the common mode inductor are as follows: and the two wires are wound in parallel, the wire passes through 0.05mm, the winding center post is a square center post, the cross section of the center post is a square post with the length of 1.2mm and the width of 0.6mm, the number of turns is 9.5, and the size of the inductor is 2mm multiplied by 1.2 mm. Testing the common mode inductor; the common mode impedance is tested by using an impedance analyzer E4991, the testing frequency is 100MHz, and the cut-off frequency is tested by using the impedance analyzer E4991. The rated current was measured using a precision electromagnetic analyzer 3260B, measuring frequency 10 MHz. The dc resistance was measured using a milliohm-meter HP 4338A. The test results are shown in Table 1.
Example 2
The embodiment provides a preparation method of a high-cut-off frequency composite material, which comprises the following steps.
S1: weighing the following substances in proportion: 52 wt% Fe2O3、12wt％ZnO、10wt％CuO、22wt％NiO、1.0wt％Co2O3、0.5wt％SiO2、2.5wt％Sb2O3And mixing to obtain composite powder.
S2: and performing ball milling on the composite powder for 1h to obtain ball-milled powder.
S3: and (3) carrying out heat treatment on the powder subjected to ball milling for 3h in the air at 700 ℃ to obtain first heat-treated powder.
S4: taking first heat treatment powder with the grain diameter of 0.1-10um, and chemically vapor depositing a silicon oxide layer with the thickness of 0.2um on the surface of the first heat treatment powder with the grain diameter of 0.1-10um at the vacuum of 300 ℃ to obtain deposited powder.
S5: the deposited powder was treated at 900 ℃ for 1h in air to obtain a high cut-off frequency composite.
In step S4, the first heat-treated powder is pulverized in advance and then sieved to obtain the first heat-treated powder having a particle size of 0.1 to 10 um.
In step S2, after the completion of the ball milling, the mixture was dried at 180 ℃ for 3 hours.
The embodiment also provides a common mode inductor, which adopts the high cut-off frequency composite material, uniformly mixes the high cut-off frequency composite material with a sintering resin solution, and dries the mixture at the temperature of 120 ℃ for 10 hours to obtain a sintering material; in the step, the high cut-off frequency composite material and the sintering resin solution are mixed in a mixer for 40 min; wherein the weight of the sintered resin in the sintered resin solution is 0.01 percent of the weight of the high cut-off frequency composite material; the sintered resin is acrylic resin.
Pressing the sintered material in a mold at the temperature of 80 ℃ under the pressure of 300MPa to prepare an inductor blank, and sintering the inductor blank at the temperature of 1100 ℃ for 5 hours to obtain the common-mode inductor; the parameters of the spot welding coil contained in the common mode inductor are as follows: and the two wires are wound in parallel, the wire passes through 0.05mm, the winding center post is a square center post, the cross section of the center post is a square post with the length of 1.2mm and the width of 0.6mm, the number of turns is 9.5, and the size of the inductor is 2mm multiplied by 1.2 mm. Testing the common mode inductor; the common mode impedance is tested by using an impedance analyzer E4991, the testing frequency is 100MHz, and the cut-off frequency is tested by using the impedance analyzer E4991. The rated current was measured using a precision electromagnetic analyzer 3260B, measuring frequency 10 MHz. The dc resistance was measured using a milliohm-meter HP 4338A. The test results are shown in Table 1.
Example 3
The embodiment provides a preparation method of a high-cut-off frequency composite material, which comprises the following steps.
S1: weighing the following substances in proportion: 59.7 wt% Fe2O3、10wt％ZnO、8wt％CuO、20wt％NiO、0.5wt％Co2O3、0.3wt％SiO2、1.5wt％Sb2O3And mixing to obtain composite powder.
S2: and performing ball milling on the composite powder for 3 hours to obtain ball-milled powder.
S3: and (3) carrying out heat treatment on the powder subjected to ball milling for 2h in air at 800 ℃ to obtain first heat-treated powder.
S4: taking first heat treatment powder with the grain diameter of 0.1-10um, and chemically vapor depositing an aluminum oxide layer with the thickness of 0.08um on the surface of the first heat treatment powder with the grain diameter of 0.1-10um at the vacuum of 250 ℃ to obtain deposited powder.
S5: the deposited powder was treated in air at 800 ℃ for 2h to obtain a high cut-off frequency composite.
In step S4, the first heat-treated powder is pulverized in advance and then sieved to obtain the first heat-treated powder having a particle size of 0.1 to 10 um.
In step S2, after the completion of the ball milling, the mixture was dried at 150 ℃ for 6 hours.
The embodiment also provides a common mode inductor, which adopts the high cut-off frequency composite material, uniformly mixes the high cut-off frequency composite material with a sintering resin solution, and dries the mixture at the temperature of 150 ℃ for 8 hours to obtain a sintering material; in the step, the high cut-off frequency composite material and the sintering resin solution are mixed in a mixer for 40 min; wherein the weight of the sintered resin in the sintered resin solution is 0.05 percent of the weight of the high cut-off frequency composite material; the sintered resin is acrylic resin.
Pressing the sintered material in a mold at the temperature of 120 ℃ under the pressure of 210MPa to prepare an inductor blank, and sintering the inductor blank at the temperature of 1000 ℃ for 7 hours to obtain the common-mode inductor; the parameters of the spot welding coil contained in the common mode inductor are as follows: and the two wires are wound in parallel, the wire passes through 0.05mm, the winding center post is a square center post, the cross section of the center post is a square post with the length of 1.2mm and the width of 0.6mm, the number of turns is 9.5, and the size of the inductor is 2mm multiplied by 1.2 mm. Testing the common mode inductor; the common mode impedance is tested by using an impedance analyzer E4991, the testing frequency is 100MHz, and the cut-off frequency is tested by using the impedance analyzer E4991. The rated current was measured using a precision electromagnetic analyzer 3260B, measuring frequency 10 MHz. The dc resistance was measured using a milliohm-meter HP 4338A. The test results are shown in Table 1.
Example 4
The embodiment provides a preparation method of a high-cut-off frequency composite material, which comprises the following steps.
S1: weighing the following substances in proportion: 60.1 wt% Fe2O3、11wt％ZnO、7wt％CuO、19wt％NiO、0.7wt％Co2O3、0.2wt％SiO2、2.0wt％Sb2O3And mixing to obtain composite powder.
S2: and performing ball milling on the composite powder for 4 hours to obtain ball-milled powder.
S3: and (3) carrying out heat treatment on the powder subjected to ball milling for 1.5h at 850 ℃ in air to obtain first heat-treated powder.
S4: taking first heat treatment powder with the grain diameter of 0.1-10um, and chemically vapor-depositing an aluminum oxide layer with the thickness of 0.1um, a bismuth oxide layer with the thickness of 0.02um and a silicon oxide layer with the thickness of 0.02um on the surface of the first heat treatment powder with the thickness of 0.1-10um at the vacuum of 230 ℃ to obtain deposition powder.
S5: the deposited powder was treated at 850 ℃ for 1.5h in air to obtain a high cut-off frequency composite.
In step S4, the first heat-treated powder is pulverized in advance and then sieved to obtain the first heat-treated powder having a particle size of 0.1 to 10 um.
In step S2, after the completion of the ball milling, the mixture was dried at 160 ℃ for 4 hours.
The embodiment also provides a common mode inductor, which adopts the high cut-off frequency composite material, uniformly mixes the high cut-off frequency composite material with a sintering resin solution, and dries the mixture at the temperature of 170 ℃ for 4 hours to obtain a sintering material; in the step, the high cut-off frequency composite material and the sintering resin solution are mixed in a mixer for 40 min; wherein the weight of the sintered resin in the sintered resin solution is 0.04% of the weight of the high cut-off frequency composite material; the sintered resin is acrylic resin.
Pressing the sintered material in a die at the temperature of 110 ℃ under 190MPa to prepare an inductor blank, and sintering the inductor blank at the temperature of 1500 ℃ for 5 hours to obtain the common-mode inductor; the parameters of the spot welding coil contained in the common mode inductor are as follows: and the two wires are wound in parallel, the wire passes through 0.05mm, the winding center post is a square center post, the cross section of the center post is a square post with the length of 1.2mm and the width of 0.6mm, the number of turns is 9.5, and the size of the inductor is 2mm multiplied by 1.2 mm. Testing the common mode inductor; the common mode impedance is tested by using an impedance analyzer E4991, the testing frequency is 100MHz, and the cut-off frequency is tested by using the impedance analyzer E4991. The rated current was measured using a precision electromagnetic analyzer 3260B, measuring frequency 10 MHz. The dc resistance was measured using a milliohm-meter HP 4338A. The test results are shown in Table 1.
Comparative example 1
Weighing the following substances in proportion: 69.3 wt% Fe2O3、8wt％ZnO、5wt％CuO、17wt％NiO、0.1wt％Co2O3、0.1wt％SiO2、0.5wt％Sb2O3And mixing to obtain composite powder. Mixing the composite powder in a ball mill for 5 hours, and drying at 120 ℃ for 8 hours to obtain ball-milled powder; the ball-milled powder was treated at 900 deg.c for 1 hour under air, and the powder was pulverized to 0.1-10um to obtain a first heat-treated powder. The first heat-treated powder was added with an acrylic resin solution in an amount of 0.05% by weight of the powder, mixed in a mixer for 60min to obtain a mixed powder, and dried at a temperature of 180 ℃ for 5 hours to obtain a composite soft magnetic powder. And pressing the obtained composite soft magnetic powder in a mold at the temperature of 150 ℃ under 200MPa to prepare an inductor blank, and sintering the inductor blank at the temperature of 1400 ℃ for 5h to obtain the common-mode inductor. The composite soft magnetic powder obtained by the embodiment is adopted to prepare the common mode inductor, wherein the parameters of the spot welding coil contained in the common mode inductor are as follows: and the two wires are wound in parallel, the wire passes through 0.05mm, the winding center post is a square center post, the cross section of the center post is a square post with the length of 1.2mm and the width of 0.6mm, the number of turns is 9.5, and the size of the inductor is 2mm multiplied by 1.2 mm. Testing the common mode inductor; the common mode impedance is tested by using an impedance analyzer E4991, the testing frequency is 100MHz, and the cut-off frequency is tested by using the impedance analyzer E4991. The rated current was measured using a precision electromagnetic analyzer 3260B, measuring frequency 10 MHz. The dc resistance was measured using a milliohm-meter HP 4338A. The test results are shown in Table 1.
Comparative example 2
The material components are commercial ferrite materials (wherein, the content of iron oxide is 55-67 wt%, the content of zinc oxide is 6-10 wt%, the content of nickel oxide is 21-25 wt%, and the content of copper oxide is 6-10 wt%). Adding a commercially available ferrite material powder to an epoxy resin solution of 0.07% by weight of the powder, mixing in a mixer for 45min, and drying under vacuum at 70 ℃ for 2.5 hours to obtain a mixed powder, wherein the residual C content of the epoxy resin after burning at 600 ℃ is less than 830 ppm. And pressing the obtained mixed powder in a mold at the temperature of 150 ℃ under 200MPa to obtain an inductor blank, and sintering the blank at the temperature of 1100 ℃ for 2.5 hours to obtain a common-mode inductor sample. The parameters of the spot welding coil contained in the common mode inductor are as follows: and the two wires are wound in parallel, the wire passes through 0.05mm, the winding center post is a square center post, the cross section of the center post is a square post with the length of 1.2mm and the width of 0.6mm, the number of turns is 9.5, and the size of the inductor is 2mm multiplied by 1.2 mm. Testing the common mode inductor; the common mode impedance is tested by using an impedance analyzer E4991, the testing frequency is 100MHz, and the cut-off frequency is tested by using the impedance analyzer E4991. The rated current was measured using a precision electromagnetic analyzer 3260B, measuring frequency 10 MHz. The dc resistance was measured using a milliohm-meter HP 4338A. The test results are shown in Table 1.
TABLE 1
As can be seen from table 1, the common mode inductors made of the materials obtained in the examples and the comparative examples have higher cut-off frequency under the condition that the rated current and the direct current resistance are equivalent, so that the common mode inductor can fully meet the application requirements of the internet of things and 5G.
In summary, the invention provides a high cut-off frequency composite material, a preparation method and a common mode inductor, wherein Co is added2O3、SiO2、Sb2O3Can be effectively refinedThe crystal grains improve the cut-off frequency of the material, and a uniform nonmagnetic gap is formed locally through chemical deposition, so that the cut-off frequency of the material is further improved. Therefore, the application requirements of the Internet of things and 5G can be fully met.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A preparation method of a high cut-off frequency composite material is characterized by comprising the following steps:
s1: weighing the following substances in proportion: 52-69.3 wt% Fe2O3、8-12wt％ZnO、5-10wt％CuO、17-22wt％NiO、0.1-1.0wt％Co2O3、0.1-0.5wt％SiO2、0.5-2.5wt％Sb2O3Mixing to obtain composite powder;
s2: ball-milling the composite powder for 0.5-8h to obtain ball-milled powder;
s3: carrying out heat treatment on the powder subjected to ball milling for 0.5-6h in the air at the temperature of 700-900 ℃ to obtain first heat-treated powder;
s4: taking first heat treatment powder with the particle size of 0.1-10um, and chemically vapor-depositing one or the mixture of at least two of an aluminum oxide layer, a silicon oxide layer and a bismuth oxide layer with the thickness of 0.01-0.3um on the surface of the first heat treatment powder with the particle size of 0.1-10um at the vacuum of 140-500 ℃ to obtain deposition powder;
s5: the deposition powder is treated for 0.5 to 6 hours in the air of 700-900 ℃ to obtain the high-cut-off frequency composite material.
2. The method of claim 1, wherein the first heat-treated powder is pulverized and then sieved to obtain the first heat-treated powder having a particle size of 0.1-10um in step S4.
3. The method of claim 1, wherein the ball-milling is completed and then dried at 60-300 ℃ for 0.5-12 hours in step S2.
4. The method of claim 1, wherein the ball milling in step S2 is wet ball milling, and the solvent is alcohol, acetone or water.
5. A high cut-off frequency composite material, characterized by being produced by the method for producing a high cut-off frequency composite material according to any one of claims 1 to 4.
6. A common mode inductor is characterized in that the high cut-off frequency composite material of claim 5 is adopted, the high cut-off frequency composite material and a sintering resin solution are uniformly mixed, and the mixture is dried for 1 to 20 hours at the temperature of 70 to 300 ℃ to obtain a sintering material; wherein the weight of the sintering resin in the sintering resin solution is 0.01-0.5% of the weight of the high cut-off frequency composite material; pressing the obtained product at a temperature of 50-200 ℃ in a mold at 150-300 MPa to obtain an inductor blank, and sintering the inductor blank at 1000-1600 ℃ for 1-10h to obtain the common mode inductor.
7. A common-mode inductor according to claim 6, characterized in that the sintering resin is acrylic resin or cellulose ether or polyvinyl butyral.
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