CN112299836A - High-frequency low-loss soft magnetic ferrite material and preparation method thereof - Google Patents
High-frequency low-loss soft magnetic ferrite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-frequency low-loss soft magnetic ferrite material and a preparation method thereof, and particularly relates to the technical field of soft magnetic ferrite materials, wherein the soft magnetic ferrite material comprises a main body system A and a doping system B, wherein the main body system A comprises: ferric oxide, zinc oxide, manganic oxide; the doping system B comprises: calcium carbonate, cobaltous oxide, niobium pentoxide, tin dioxide, vanadium pentoxide, boron graphene, nano silicon carbide and nano lanthanum oxide. In the invention, the main body system A and the doping system B are matched with each other to form the high-frequency low-loss soft magnetic ferrite material, in addition, the boron graphene, the nano silicon carbide and the nano lanthanum oxide are matched for use, so that the interaction relation among the boron graphene, the nano silicon carbide and the nano lanthanum oxide can be effectively enhanced, the loss of the soft magnetic ferrite material in a high-frequency working state can be further reduced, the raw material is matched with ultrasonic oscillation irradiation alternate treatment in the ball milling process, the performance of the raw material can be effectively improved, the preparation quality of the soft magnetic ferrite material is better, and the power consumption is reduced.
Description
Technical Field
The invention relates to the technical field of soft magnetic ferrite materials, in particular to a high-frequency low-loss soft magnetic ferrite material and a preparation method thereof.
Background
When magnetization occurs at Hc (coercive force, magnetic field strength at which the magnetic induction is reduced to zero along the saturation hysteresis loop) of not more than 1000A/m, such a material is called a soft magnet. The soft magnetic ferrite is a ferrimagnetic oxide with Fe2O3 as a main component and is produced by a powder metallurgy method. The soft magnetic material has a very low coercive force and can be magnetized repeatedly in a magnetic field, and the magnetism obtained after the external electric field is removed can be completely or mostly disappeared. The soft magnetic ferrite is produced by adopting a powder metallurgy method and comprises Mn-Zn, Cu-Zn, Ni-Zn and the like, wherein the yield and the dosage of the Mn-Zn ferrite are the largest. The magnetic loss of the soft magnetic ferrite material is caused by that the soft magnetic material is magnetized to store energy in a weak alternating field on one hand, and the magnetic induction intensity B lags behind the magnetic field intensity H to generate loss due to various reasons on the other hand, namely, the material absorbs energy from the alternating field and dissipates in the form of heat energy.
The existing soft magnetic ferrite material has high loss when working under a high-frequency state and more energy loss when in use.
Disclosure of Invention
In order to overcome the above defects in the prior art, embodiments of the present invention provide a high-frequency low-loss soft magnetic ferrite material and a preparation method thereof.
In order to achieve the purpose, the invention provides the following technical scheme: a high-frequency low-loss soft magnetic ferrite material comprises a main body system A and a main body system B, wherein the main body system A comprises the following components in percentage by weight: 49.000-53.671 wt% of ferric oxide, 5.0-7.0 wt% of zinc oxide and the balance of manganic manganous oxide; the doping system B is based on the total weight of the main body system A, and comprises: 0.05-0.15 wt% of calcium carbonate, 0.05-0.25 wt% of cobaltous oxide, 0.025-0.05 wt% of niobium pentoxide, 0.20-0.50 wt% of tin dioxide, 0.02-0.05 wt% of vanadium pentoxide, 0.002-0.006 wt% of boron graphene, 0.003-0.005 wt% of nano silicon carbide and 0.30-0.50 wt% of nano lanthanum oxide;
further, the body system a comprises: 49.000 wt% of ferric oxide, 5.0 wt% of zinc oxide and the balance of manganic oxide; the doping system B comprises: 0.05 wt% of calcium carbonate, 0.05 wt% of cobaltous oxide, 0.025 wt% of niobium pentoxide, 0.20 wt% of tin dioxide, 0.02 wt% of vanadium pentoxide, 0.002 wt% of graphene oxide, 0.003 wt% of nano silicon carbide and 0.30 wt% of nano lanthanum oxide.
Further, the body system a comprises: 53.671 wt% of ferric oxide, 7.0 wt% of zinc oxide and the balance of manganic oxide; the doping system B comprises: 0.15 wt% of calcium carbonate, 0.25 wt% of cobaltous oxide, 0.05 wt% of niobium pentoxide, 0.50 wt% of tin dioxide, 0.05 wt% of vanadium pentoxide, 0.006 wt% of graphene oxide, 0.005 wt% of nano silicon carbide and 0.50 wt% of nano lanthanum oxide.
Further, the body system a comprises: 51.38 wt% of ferric oxide, 6.0 wt% of zinc oxide and the balance of manganic oxide; the doping system B comprises: 0.10 wt% of calcium carbonate, 0.15 wt% of cobaltous oxide, 0.0375 wt% of niobium pentoxide, 0.35 wt% of tin dioxide, 0.035 wt% of vanadium pentoxide, 0.004 wt% of graphene oxide, 0.004 wt% of nano silicon carbide and 0.40 wt% of nano lanthanum oxide.
The invention also provides a preparation method of the high-frequency low-loss soft magnetic ferrite material, which comprises the following specific preparation steps:
the method comprises the following steps: selecting raw materials: respectively selecting the main body systems A in the weight ratio according to the purity levels of more than or equal to 99.50% of ferric oxide, more than or equal to 99.85% of zinc oxide and more than or equal to 99.50% of manganic oxide, and respectively selecting the doping systems B in the weight ratio according to the purity of calcium carbonate, cobaltous oxide, niobium pentoxide, tin dioxide, vanadium pentoxide, graphene oxide, nano silicon carbide and nano lanthanum oxide which reach the analytical pure water level;
step two: primary burdening: uniformly mixing the calcium carbonate, the cobaltous oxide, the niobium pentoxide, the tin dioxide and the vanadium pentoxide in the step one, and then equally dividing the mixture into three parts: b1, B2 and B3;
step three: primary planet ball milling: mixing ferric oxide, zinc oxide and manganic oxide in the first step, loading the mixture into stainless steel balls and deionized water, carrying out ball milling for 3-4 h at the rotating speed of 260-280 r/min, carrying out ultrasonic oscillation and irradiation alternative treatment simultaneously, when the particle size is tested to be 0.4-0.5 mu m, carrying out filter pressing to remove water and drying to obtain a mixture C, and then equally dividing the mixture into three parts: c1, C2, and C3;
step four: secondary planetary ball milling: mixing the mixture C1 in the third step, the mixture B1 in the second step and the boron graphene in the first step, filling the mixture into a stainless steel ball and deionized water, carrying out ball milling at a rotating speed of 240-;
step five: and (3) carrying out third planetary ball milling: mixing the mixture C2 in the third step, the mixture B2 in the second step and the nano silicon carbide in the first step, filling the mixture into a stainless steel ball and deionized water, carrying out ball milling at the rotating speed of 240-;
step six: four-time planetary ball milling: mixing the mixture C3 in the third step, the mixture B3 in the second step and the nano lanthanum oxide in the first step, filling the mixture into a stainless steel ball and deionized water, carrying out ball milling at a rotating speed of 240-;
step seven: high-temperature pre-sintering: respectively pre-burning the mixture D in the fourth step, the mixture E in the fifth step and the mixture F in the sixth step, heating for 1h at the heating rate of 3 ℃/min from room temperature, then heating for 2h at the heating rate of 5 ℃/min, finally heating to 900-1000 ℃ at the heating rate of 2 ℃/min, preserving heat for 2-3h, cooling to room temperature along with the furnace, and then discharging;
step eight: and (5) carrying out five-time planetary ball milling: mixing the mixture D, the mixture E and the mixture F subjected to high-temperature pre-sintering in the sixth step, adding the mixture D, the mixture E and the mixture F into a planetary ball mill, adding stainless steel balls and deionized water, carrying out ball milling for 3-4 h at the rotating speed of 260-;
step nine: granulating and forming: carrying out high-pressure spray drying granulation on the ground slurry in the step eight, and forming to obtain a sample blank;
step ten: and sintering the formed blank, adopting a gradient heating mode, and then cooling along with the furnace to obtain the high-frequency low-loss soft magnetic ferrite material.
Further, in the second step, the mixture is subjected to ultrasonic oscillation mixing treatment, the oscillation frequency is 10 megaHz, and the ultrasonic treatment time is 30-40 min.
Further, in the third step, the oscillation frequency of the ultrasonic oscillation mixing treatment is 10 megaHz, the ultrasonic treatment time is 20min each time, and the ultrasonic irradiation treatment is carried out, the irradiation frequency is 40kHz, and the irradiation time is 20min each time.
Further, in the fourth step, the fifth step and the sixth step, the oscillation frequency of the ultrasonic oscillation mixing treatment is 10 megaHz, each ultrasonic treatment time is 20min, and the ultrasonic irradiation treatment is carried out, the irradiation frequency is 40kHz, and each irradiation time is 20 min.
Further, in the step eight, the oscillation frequency of the ultrasonic oscillation mixing treatment is 10 megaHz, each ultrasonic treatment time is 30min, and the ultrasonic irradiation treatment is carried out, wherein the irradiation frequency is 40kHz, and each irradiation time is 30 min.
Further, in the seventh step and the tenth step, cooling treatment is carried out in a liquid cooling mode in the furnace cooling process.
The invention has the technical effects and advantages that:
1. the high-frequency low-loss soft magnetic ferrite material prepared by the raw material formula of the invention has the advantages that a main body system A and a doping system B are mutually matched to form the high-frequency low-loss soft magnetic ferrite material, ferric oxide, zinc oxide and manganic oxide in the main body system A are matched with calcium carbonate, cobaltous oxide, niobium pentoxide, stannic oxide and vanadium pentoxide in the doping system B for use, the loss of the soft magnetic ferrite material in a high-frequency state can be effectively reduced, in addition, boron graphene in the doping system B is formed by a single layer of boron atoms and is a two-dimensional metal material, the structure of the boron graphene is that 36 boron atoms form three mutually connected quasi-planar rings, a hexagonal cavity is left in the middle, the boron graphene has a firm covalent bond, so the boron graphene is more stable than silicone, and has mechanical properties similar to graphene, the boron graphene film has considerable hardness, intersects with three fields of metal, semimetal and nonmetal, and has the characteristic that other two-dimensional materials do not have, and the boron graphene has both metallicity and atomic thickness, is added into the doping system B and is matched with the material in the main body system A to react with the material in the main body system A, so that the electronic performance of the soft magnetic ferrite material can be effectively improved, the loss is reduced, and the safety performance is high; the nano silicon carbide in the doping system B has the characteristics of high forbidden bandwidth, high critical breakdown electric field and thermal conductivity, small dielectric constant, high electronic saturation mobility, strong radiation resistance, good mechanical property and the like, and the one-dimensional nano silicon carbide material has the excellent characteristics of low threshold field intensity, high current density, good high-temperature stability and the like; the nanometer lanthanum oxide in the doping system B can increase the piezoelectric coefficient of the product, improve the electric energy conversion rate of the product, effectively improve the anti-corrosion capability and reduce the electrode loss, and in addition, the cooperation of the boron graphene, the nanometer silicon carbide and the nanometer lanthanum oxide can effectively enhance the interaction relation among the three materials and other raw materials and further reduce the loss of the soft magnetic ferrite material in a high-frequency working state;
2. in the process of preparing the high-frequency low-loss soft magnetic ferrite material, calcium carbonate, cobaltous oxide, niobium pentoxide, tin dioxide and vanadium pentoxide in a doping system B are divided into three parts in the second step, the three parts of raw materials are respectively matched with graphene, nano silicon carbide and nano lanthanum oxide to be ball-milled with three main materials in a main body system A, and finally the mixture after ball milling is ball-milled, so that the raw materials in the doping system B of the main body system A in the raw materials can be effectively enhanced to be fully contacted and mixed, the contact reaction effect among the raw materials is better, the performance of the high-frequency low-loss soft magnetic ferrite material is more stable, the raw materials are matched with ultrasonic oscillation irradiation for alternative treatment in the ball milling process, the ultrasonic oscillation can further enhance the contact effect among the raw materials of each component, and further enhance the stability of the high-frequency low-loss soft magnetic ferrite material, the ultrasonic irradiation treatment can modify the surface of the material, effectively improve the performance of the raw material, better prepare the high-frequency low-loss soft magnetic ferrite material and reduce the power consumption.
Detailed Description
The following will clearly and completely describe the technical solutions 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 embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention provides a high-frequency low-loss soft magnetic ferrite material, which comprises a main body system A and a doping system B, and is characterized in that: the main body system A comprises the following components in percentage by weight: 49.000 wt% of ferric oxide, 5.0 wt% of zinc oxide and the balance of manganic oxide; the doping system B is based on the total weight of the main body system A, and comprises: 0.05 wt% of calcium carbonate, 0.05 wt% of cobaltous oxide, 0.025 wt% of niobium pentoxide, 0.20 wt% of tin dioxide, 0.02 wt% of vanadium pentoxide, 0.002 wt% of graphene oxide, 0.003 wt% of nano silicon carbide and 0.30 wt% of nano lanthanum oxide;
the invention also provides a preparation method of the high-frequency low-loss soft magnetic ferrite material, which comprises the following specific preparation steps:
the method comprises the following steps: selecting raw materials: respectively selecting the main body systems A in the weight ratio according to the purity levels of more than or equal to 99.50% of ferric oxide, more than or equal to 99.85% of zinc oxide and more than or equal to 99.50% of manganic oxide, and respectively selecting the doping systems B in the weight ratio according to the purity of calcium carbonate, cobaltous oxide, niobium pentoxide, tin dioxide, vanadium pentoxide, graphene oxide, nano silicon carbide and nano lanthanum oxide which reach the analytical pure water level;
step two: primary burdening: uniformly mixing the calcium carbonate, the cobaltous oxide, the niobium pentoxide, the tin dioxide and the vanadium pentoxide in the step one, and then equally dividing the mixture into three parts: b1, B2 and B3;
step three: primary planet ball milling: mixing ferric oxide, zinc oxide and manganic oxide in the first step, loading the mixture into stainless steel balls and deionized water, carrying out ball milling for 3-4 h at the rotating speed of 260-280 r/min, carrying out ultrasonic oscillation and irradiation alternative treatment simultaneously, when the particle size is tested to be 0.4-0.5 mu m, carrying out filter pressing to remove water and drying to obtain a mixture C, and then equally dividing the mixture into three parts: c1, C2, and C3;
step four: secondary planetary ball milling: mixing the mixture C1 in the third step, the mixture B1 in the second step and the boron graphene in the first step, filling the mixture into a stainless steel ball and deionized water, carrying out ball milling at a rotating speed of 240-;
step five: and (3) carrying out third planetary ball milling: mixing the mixture C2 in the third step, the mixture B2 in the second step and the nano silicon carbide in the first step, filling the mixture into a stainless steel ball and deionized water, carrying out ball milling at the rotating speed of 240-;
step six: four-time planetary ball milling: mixing the mixture C3 in the third step, the mixture B3 in the second step and the nano lanthanum oxide in the first step, filling the mixture into a stainless steel ball and deionized water, carrying out ball milling at a rotating speed of 240-;
step seven: high-temperature pre-sintering: respectively pre-burning the mixture D in the fourth step, the mixture E in the fifth step and the mixture F in the sixth step, heating for 1h at the heating rate of 3 ℃/min from room temperature, then heating for 2h at the heating rate of 5 ℃/min, finally heating to 900-1000 ℃ at the heating rate of 2 ℃/min, preserving heat for 2-3h, cooling to room temperature along with the furnace, and then discharging;
step eight: and (5) carrying out five-time planetary ball milling: mixing the mixture D, the mixture E and the mixture F subjected to high-temperature pre-sintering in the sixth step, adding the mixture D, the mixture E and the mixture F into a planetary ball mill, adding stainless steel balls and deionized water, carrying out ball milling for 3-4 h at the rotating speed of 260-;
step nine: granulating and forming: carrying out high-pressure spray drying granulation on the ground slurry in the step eight, and forming to obtain a sample blank;
step ten: and sintering the formed blank, adopting a gradient heating mode, and then cooling along with the furnace to obtain the high-frequency low-loss soft magnetic ferrite material.
And in the second step, performing ultrasonic oscillation mixing treatment on the mixture, wherein the oscillation frequency is 10 MHz, and the ultrasonic treatment time is 30-40 min.
In the third step, the oscillation frequency of ultrasonic oscillation mixing treatment is 10 MHz, each ultrasonic treatment time is 20min, and the ultrasonic irradiation treatment is carried out, the irradiation frequency is 40kHz, each irradiation time is 20 min.
In the fourth step, the fifth step and the sixth step, the oscillation frequency of the ultrasonic oscillation mixing treatment is 10 MHz, each ultrasonic treatment time is 20min, and the ultrasonic irradiation treatment is carried out, the irradiation frequency is 40kHz, and each irradiation time is 20 min.
In the step eight, the oscillation frequency of ultrasonic oscillation mixing treatment is 10 MHz, each ultrasonic treatment time is 30min, and ultrasonic irradiation treatment is carried out, the irradiation frequency is 40kHz, each irradiation time is 30 min.
And in the seventh step and the tenth step, cooling treatment is carried out in a liquid cooling mode in the furnace cooling process.
Example 2:
in contrast to example 1, the host system a comprises: 53.671 wt% of ferric oxide, 7.0 wt% of zinc oxide and the balance of manganic oxide; the doping system B comprises: 0.15 wt% of calcium carbonate, 0.25 wt% of cobaltous oxide, 0.05 wt% of niobium pentoxide, 0.50 wt% of tin dioxide, 0.05 wt% of vanadium pentoxide, 0.006 wt% of graphene oxide, 0.005 wt% of nano silicon carbide and 0.50 wt% of nano lanthanum oxide.
Example 3:
unlike examples 1-2, the host system a comprised: 51.38 wt% of ferric oxide, 6.0 wt% of zinc oxide and the balance of manganic oxide; the doping system B comprises: 0.10 wt% of calcium carbonate, 0.15 wt% of cobaltous oxide, 0.0375 wt% of niobium pentoxide, 0.35 wt% of tin dioxide, 0.035 wt% of vanadium pentoxide, 0.004 wt% of graphene oxide, 0.004 wt% of nano silicon carbide and 0.40 wt% of nano lanthanum oxide.
Taking the high-frequency low-loss soft magnetic ferrite materials prepared in the above examples 1-3 and the comparison group of the first soft magnetic ferrite material, the comparison group of the second soft magnetic ferrite material, the comparison group of the third soft magnetic ferrite material, the comparison group of the fourth soft magnetic ferrite material and the comparison group of the fifth soft magnetic ferrite material, respectively, wherein the comparison group of the first soft magnetic ferrite material is the common soft magnetic ferrite material on the market, the comparison group of the second soft magnetic ferrite material is free of graphene compared with the examples, the comparison group of the third soft magnetic ferrite material is free of silicon carbide compared with the examples, the comparison group of the fourth soft magnetic ferrite material is free of lanthanum oxide compared with the examples, the comparison group of the fifth soft magnetic ferrite material is made of common silicon carbide and common lanthanum oxide compared with the examples, the high-frequency low-loss soft magnetic ferrite materials prepared in the three examples and the five comparison group of the soft magnetic ferrite materials are respectively tested in eight groups, and each group of the five, multiple tests were performed to obtain the following data, with the test results shown in table one:
table one:
as can be seen from table one, when the high-frequency low-loss soft magnetic ferrite material comprises the following raw materials in proportion: the main body system A comprises: 51.38 wt% of ferric oxide, 6.0 wt% of zinc oxide and the balance of manganic oxide; the doping system B comprises: 0.10 wt% of calcium carbonate, 0.15 wt% of cobaltous oxide, 0.0375 wt% of niobium pentoxide, 0.35 wt% of tin dioxide, 0.035 wt% of vanadium pentoxide, 0.004 wt% of boron graphene, 0.004 wt% of nano silicon carbide and 0.40 wt% of nano lanthanum oxide, the loss of the soft magnetic ferrite material in high-frequency use can be effectively reduced, the embodiment III is a preferable scheme in the invention, 51.38 wt% of ferric oxide, 6.0 wt% of zinc oxide and the balance of manganic oxide are taken as a main body system A, 0.10 wt% of calcium carbonate, 0.15 wt% of cobaltous oxide, 0.0375 wt% of niobium pentoxide, 0.35 wt% of tin dioxide, 0.035 wt% of vanadium pentoxide, 0.004 wt% of boron graphene, 0.004 wt% of nano silicon carbide and 0.40 wt% of nano lanthanum oxide are taken as doping systems, and the main body system A is taken as a low-loss material of the soft magnetic ferrite material, the doped system B is used as an auxiliary composition raw material of the high-frequency low-loss soft magnetic ferrite material, the main body system A and the doped system B are matched with each other to form the high-frequency low-loss soft magnetic ferrite material, ferric oxide, zinc oxide and manganic oxide in the main body system A are matched with calcium carbonate, cobaltous oxide, niobium pentoxide, tin dioxide and vanadium pentoxide in the doped system B for use, the loss of the soft magnetic ferrite material in a high-frequency state can be effectively reduced, in addition, boron graphene in the doped system B is formed by a single layer of boron atoms and is a two-dimensional metal material, the structure of the boron graphene is that 36 boron atoms form three quasi-planar rings which are connected with each other, a hexagonal cavity is left in the middle, the boron graphene has a firm covalent bond, so that the boron graphene is more stable than silicone, and has mechanical properties similar to graphene, the boron graphene film has considerable hardness, intersects with three fields of metal, semimetal and nonmetal, and has the characteristic that other two-dimensional materials do not have, and the boron graphene has both metallicity and atomic thickness, is added into the doping system B and is matched with the material in the main body system A to react with the material in the main body system A, so that the electronic performance of the soft magnetic ferrite material can be effectively improved, the loss is reduced, and the safety performance is high; the nano silicon carbide in the doping system B has the characteristics of high forbidden bandwidth, high critical breakdown electric field and thermal conductivity, small dielectric constant, high electronic saturation mobility, strong radiation resistance, good mechanical property and the like, and the one-dimensional nano silicon carbide material has the excellent characteristics of low threshold field intensity, high current density, good high-temperature stability and the like; the nanometer lanthanum oxide in the doping system B can increase the piezoelectric coefficient of the product, improve the electric energy conversion rate of the product, effectively improve the anti-corrosion capability and reduce the electrode loss, and in addition, the cooperation of the boron graphene, the nanometer silicon carbide and the nanometer lanthanum oxide can effectively enhance the interaction relation between the boron graphene, the nanometer silicon carbide and other raw materials and further reduce the loss of the soft magnetic ferrite material in a high-frequency working state.
Example 4
In the above preferred technical solution, the present invention provides a high-frequency low-loss soft magnetic ferrite material, which includes a host system a and a doping system B, wherein the host system a includes, by weight: 51.38 wt% of ferric oxide, 6.0 wt% of zinc oxide and the balance of manganic oxide; a dopant system B, based on the total weight of the host system a, comprising: 0.10 wt% of calcium carbonate, 0.15 wt% of cobaltous oxide, 0.0375 wt% of niobium pentoxide, 0.35 wt% of tin dioxide, 0.035 wt% of vanadium pentoxide, 0.004 wt% of graphene oxide, 0.004 wt% of nano silicon carbide and 0.40 wt% of nano lanthanum oxide.
The invention also provides a preparation method of the high-frequency low-loss soft magnetic ferrite material, which comprises the following specific preparation steps:
the method comprises the following steps: selecting raw materials: respectively selecting the main body systems A in the weight ratio according to the purity levels of more than or equal to 99.50% of ferric oxide, more than or equal to 99.85% of zinc oxide and more than or equal to 99.50% of manganic oxide, and respectively selecting the doping systems B in the weight ratio according to the purity of calcium carbonate, cobaltous oxide, niobium pentoxide, tin dioxide, vanadium pentoxide, graphene oxide, nano silicon carbide and nano lanthanum oxide which reach the analytical pure water level;
step two: primary burdening: uniformly mixing the calcium carbonate, the cobaltous oxide, the niobium pentoxide, the tin dioxide and the vanadium pentoxide in the step one, and then equally dividing the mixture into three parts: b1, B2 and B3;
step three: primary planet ball milling: mixing ferric oxide, zinc oxide and manganic oxide in the first step, loading the mixture into stainless steel balls and deionized water, carrying out ball milling for 3-4 h at the rotating speed of 260-280 r/min, carrying out ultrasonic oscillation and irradiation alternative treatment simultaneously, when the particle size is tested to be 0.4-0.5 mu m, carrying out filter pressing to remove water and drying to obtain a mixture C, and then equally dividing the mixture into three parts: c1, C2, and C3;
step four: secondary planetary ball milling: mixing the mixture C1 in the third step, the mixture B1 in the second step and the boron graphene in the first step, filling the mixture into a stainless steel ball and deionized water, carrying out ball milling at a rotating speed of 240-;
step five: and (3) carrying out third planetary ball milling: mixing the mixture C2 in the third step, the mixture B2 in the second step and the nano silicon carbide in the first step, filling the mixture into a stainless steel ball and deionized water, carrying out ball milling at the rotating speed of 240-;
step six: four-time planetary ball milling: mixing the mixture C3 in the third step, the mixture B3 in the second step and the nano lanthanum oxide in the first step, filling the mixture into a stainless steel ball and deionized water, carrying out ball milling at a rotating speed of 240-;
step seven: high-temperature pre-sintering: respectively pre-burning the mixture D in the fourth step, the mixture E in the fifth step and the mixture F in the sixth step, heating for 1h at the heating rate of 3 ℃/min from room temperature, then heating for 2h at the heating rate of 5 ℃/min, finally heating to 900-1000 ℃ at the heating rate of 2 ℃/min, preserving heat for 2-3h, cooling to room temperature along with the furnace, and then discharging;
step eight: and (5) carrying out five-time planetary ball milling: mixing the mixture D, the mixture E and the mixture F subjected to high-temperature pre-sintering in the sixth step, adding the mixture D, the mixture E and the mixture F into a planetary ball mill, adding stainless steel balls and deionized water, carrying out ball milling for 3-4 h at the rotating speed of 260-;
step nine: granulating and forming: carrying out high-pressure spray drying granulation on the ground slurry in the step eight, and forming to obtain a sample blank;
step ten: and sintering the formed blank, adopting a gradient heating mode, and then cooling along with the furnace to obtain the high-frequency low-loss soft magnetic ferrite material.
And in the second step, performing ultrasonic oscillation mixing treatment on the mixture, wherein the oscillation frequency is 10 MHz, and the ultrasonic treatment time is 30-40 min.
In the third step, the oscillation frequency of ultrasonic oscillation mixing treatment is 10 MHz, each ultrasonic treatment time is 20min, and the ultrasonic irradiation treatment is carried out, the irradiation frequency is 40kHz, each irradiation time is 20 min.
In the fourth step, the fifth step and the sixth step, the oscillation frequency of the ultrasonic oscillation mixing treatment is 10 MHz, each ultrasonic treatment time is 20min, and the ultrasonic irradiation treatment is carried out, the irradiation frequency is 40kHz, and each irradiation time is 20 min.
In the step eight, the oscillation frequency of ultrasonic oscillation mixing treatment is 10 MHz, each ultrasonic treatment time is 30min, and ultrasonic irradiation treatment is carried out, the irradiation frequency is 40kHz, each irradiation time is 30 min.
And in the seventh step and the tenth step, cooling treatment is carried out in a liquid cooling mode in the furnace cooling process.
Example 5
Different from the embodiment 4, in the sixth step, the temperature is always raised to 900-1000 ℃ at a temperature raising rate of 5 ℃/min during the temperature raising process.
Example 6
Different from the embodiments 4-5, in the seventh step and the tenth step, the temperature reduction treatment is carried out by adopting a natural cooling mode.
Respectively taking the high-frequency low-loss soft magnetic ferrite materials prepared in the above examples 4-6, and a contrast group six soft magnetic ferrite material, a contrast group seven soft magnetic ferrite material, a contrast group eight soft magnetic ferrite material, a contrast group nine soft magnetic ferrite material and a contrast group ten soft magnetic ferrite material to perform experiments, wherein the contrast group six soft magnetic ferrite material is not subjected to ultrasonic oscillation and irradiation treatment in the third step, the fourth step, the fifth step, the sixth step and the eighth step compared with the examples, the contrast group seven soft magnetic ferrite material is not subjected to ultrasonic oscillation treatment in the third step, the fourth step, the fifth step, the sixth step and the eighth step compared with the examples, the contrast group eight soft magnetic ferrite material is not subjected to ultrasonic irradiation treatment in the third step, the fourth step, the fifth step, the sixth step and the eighth step compared with the examples, and the contrast group nine soft magnetic ferrite material is subjected to the third step, the fourth step, the fifth step, the sixth step and the eighth step compared with the examples, Step four, step five, step six and step eight, do not carry on the alternative treatment to the ultrasonic oscillation radiation, compare ten soft magnetic ferrite materials of group with embodiment directly carry on ball-milling treatment to all main body systems A and all doping systems B, then mix ball-milling treatment; the high-frequency low-loss soft magnetic ferrite materials prepared in the three examples and five control groups of soft magnetic ferrite materials were tested in eight groups, 30 samples were randomly selected for each group, and a plurality of tests were performed to obtain the following data, with the test results shown in table two:
table two:
as can be seen from table two, in the process of preparing the soft magnetic ferrite material, when the preparation method in the fourth embodiment is the preferred scheme of the present invention, in the second step, calcium carbonate, cobalt oxide, niobium pentoxide, tin dioxide and vanadium pentoxide in the doping system B are divided into three parts, the three parts of raw materials are respectively matched with graphene, nano silicon carbide and nano lanthanum oxide to be ball-milled with three main materials in the main body system a, and finally, the mixture after ball milling is ball-milled, so that the raw materials in the doping system B of each component in the main body system a in the raw materials can be effectively and sufficiently contacted and mixed, the contact reaction effect between the raw materials is better, the performance of the high-frequency low-loss soft magnetic ferrite material is more stable, the raw materials are matched with the ultrasonic oscillation irradiation alternate treatment in the ball milling process, and the ultrasonic oscillation can further enhance the contact effect between the raw materials of each component, the stability of the high-frequency low-loss soft magnetic ferrite material is further enhanced, the surface of the material can be modified through ultrasonic irradiation treatment, the performance of the raw material can be effectively improved, the ultrasonic oscillation and the ultrasonic irradiation are alternately performed, the treatment effect on the raw material can be further enhanced, the preparation quality of the high-frequency low-loss soft magnetic ferrite material is better, and the power consumption is reduced.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A high-frequency low-loss soft magnetic ferrite material comprises a main body system A and a doping system B, and is characterized in that: the main body system A comprises the following components in percentage by weight: 49.000-53.671 wt% of ferric oxide, 5.0-7.0 wt% of zinc oxide and the balance of manganic manganous oxide; the doping system B is based on the total weight of the main body system A, and comprises: 0.05-0.15 wt% of calcium carbonate, 0.05-0.25 wt% of cobaltous oxide, 0.025-0.05 wt% of niobium pentoxide, 0.20-0.50 wt% of tin dioxide, 0.02-0.05 wt% of vanadium pentoxide, 0.002-0.006 wt% of boron graphene, 0.003-0.005 wt% of nano silicon carbide and 0.30-0.50 wt% of nano lanthanum oxide.
2. A high frequency low loss soft magnetic ferrite material according to claim 1, characterized in that: the main body system A comprises: 49.000 wt% of ferric oxide, 5.0 wt% of zinc oxide and the balance of manganic oxide; the doping system B comprises: 0.05 wt% of calcium carbonate, 0.05 wt% of cobaltous oxide, 0.025 wt% of niobium pentoxide, 0.20 wt% of tin dioxide, 0.02 wt% of vanadium pentoxide, 0.002 wt% of graphene oxide, 0.003 wt% of nano silicon carbide and 0.30 wt% of nano lanthanum oxide.
3. A high frequency low loss soft magnetic ferrite material according to claim 1, characterized in that: the main body system A comprises: 53.671 wt% of ferric oxide, 7.0 wt% of zinc oxide and the balance of manganic oxide; the doping system B comprises: 0.15 wt% of calcium carbonate, 0.25 wt% of cobaltous oxide, 0.05 wt% of niobium pentoxide, 0.50 wt% of tin dioxide, 0.05 wt% of vanadium pentoxide, 0.006 wt% of graphene oxide, 0.005 wt% of nano silicon carbide and 0.50 wt% of nano lanthanum oxide.
4. A high frequency low loss soft magnetic ferrite material according to claim 1, characterized in that: the main body system A comprises: 51.38 wt% of ferric oxide, 6.0 wt% of zinc oxide and the balance of manganic oxide; the doping system B comprises: 0.10 wt% of calcium carbonate, 0.15 wt% of cobaltous oxide, 0.0375 wt% of niobium pentoxide, 0.35 wt% of tin dioxide, 0.035 wt% of vanadium pentoxide, 0.004 wt% of graphene oxide, 0.004 wt% of nano silicon carbide and 0.40 wt% of nano lanthanum oxide.
5. The method for preparing a high-frequency low-loss soft magnetic ferrite material according to any one of claims 1 to 4, wherein: the preparation method comprises the following specific steps:
the method comprises the following steps: selecting raw materials: respectively selecting the main body systems A in the weight ratio according to the purity levels of more than or equal to 99.50% of ferric oxide, more than or equal to 99.85% of zinc oxide and more than or equal to 99.50% of manganic oxide, and respectively selecting the doping systems B in the weight ratio according to the purity of calcium carbonate, cobaltous oxide, niobium pentoxide, tin dioxide, vanadium pentoxide, graphene oxide, nano silicon carbide and nano lanthanum oxide which reach the analytical pure water level;
step two: primary burdening: uniformly mixing the calcium carbonate, the cobaltous oxide, the niobium pentoxide, the tin dioxide and the vanadium pentoxide in the step one, and then equally dividing the mixture into three parts: b1, B2 and B3;
step three: primary planet ball milling: mixing ferric oxide, zinc oxide and manganic oxide in the first step, loading the mixture into stainless steel balls and deionized water, carrying out ball milling for 3-4 h at the rotating speed of 260-280 r/min, carrying out ultrasonic oscillation and irradiation alternative treatment simultaneously, when the particle size is tested to be 0.4-0.5 mu m, carrying out filter pressing to remove water and drying to obtain a mixture C, and then equally dividing the mixture into three parts: c1, C2, and C3;
step four: secondary planetary ball milling: mixing the mixture C1 in the third step, the mixture B1 in the second step and the boron graphene in the first step, filling the mixture into a stainless steel ball and deionized water, carrying out ball milling at a rotating speed of 240-;
step five: and (3) carrying out third planetary ball milling: mixing the mixture C2 in the third step, the mixture B2 in the second step and the nano silicon carbide in the first step, filling the mixture into a stainless steel ball and deionized water, carrying out ball milling at the rotating speed of 240-;
step six: four-time planetary ball milling: mixing the mixture C3 in the third step, the mixture B3 in the second step and the nano lanthanum oxide in the first step, filling the mixture into a stainless steel ball and deionized water, carrying out ball milling at a rotating speed of 240-;
step seven: high-temperature pre-sintering: respectively pre-burning the mixture D in the fourth step, the mixture E in the fifth step and the mixture F in the sixth step, heating for 1h at the heating rate of 3 ℃/min from room temperature, then heating for 2h at the heating rate of 5 ℃/min, finally heating to 900-1000 ℃ at the heating rate of 2 ℃/min, preserving heat for 2-3h, cooling to room temperature along with the furnace, and then discharging;
step eight: and (5) carrying out five-time planetary ball milling: mixing the mixture D, the mixture E and the mixture F subjected to high-temperature pre-sintering in the sixth step, adding the mixture D, the mixture E and the mixture F into a planetary ball mill, adding stainless steel balls and deionized water, carrying out ball milling for 3-4 h at the rotating speed of 260-;
step nine: granulating and forming: carrying out high-pressure spray drying granulation on the ground slurry in the step eight, and forming to obtain a sample blank;
step ten: and sintering the formed blank, adopting a gradient heating mode, and then cooling along with the furnace to obtain the high-frequency low-loss soft magnetic ferrite material.
6. The method for preparing a high-frequency low-loss soft magnetic ferrite material according to claim 5, wherein the method comprises the following steps: and in the second step, performing ultrasonic oscillation mixing treatment on the mixture, wherein the oscillation frequency is 10 MHz, and the ultrasonic treatment time is 30-40 min.
7. The method for preparing a high-frequency low-loss soft magnetic ferrite material according to claim 5, wherein the method comprises the following steps: in the third step, the oscillation frequency of ultrasonic oscillation mixing treatment is 10 MHz, each ultrasonic treatment time is 20min, and the ultrasonic irradiation treatment is carried out, the irradiation frequency is 40kHz, each irradiation time is 20 min.
8. The method for preparing a high-frequency low-loss soft magnetic ferrite material according to claim 7, wherein the method comprises the following steps: in the fourth step, the fifth step and the sixth step, the oscillation frequency of the ultrasonic oscillation mixing treatment is 10 MHz, each ultrasonic treatment time is 20min, and the ultrasonic irradiation treatment is carried out, the irradiation frequency is 40kHz, and each irradiation time is 20 min.
9. The method for preparing a high-frequency low-loss soft magnetic ferrite material according to claim 8, wherein the method comprises the following steps: in the step eight, the oscillation frequency of ultrasonic oscillation mixing treatment is 10 MHz, each ultrasonic treatment time is 30min, and ultrasonic irradiation treatment is carried out, the irradiation frequency is 40kHz, each irradiation time is 30 min.
10. The method for preparing a high-frequency low-loss soft magnetic ferrite material according to claim 5, wherein the method comprises the following steps: and in the seventh step and the tenth step, cooling treatment is carried out in a liquid cooling mode in the furnace cooling process.
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