CN114685154A - High-frequency wide-temperature ultralow-loss ferrite material and preparation process thereof - Google Patents

High-frequency wide-temperature ultralow-loss ferrite material and preparation process thereof Download PDF

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CN114685154A
CN114685154A CN202210455385.5A CN202210455385A CN114685154A CN 114685154 A CN114685154 A CN 114685154A CN 202210455385 A CN202210455385 A CN 202210455385A CN 114685154 A CN114685154 A CN 114685154A
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temperature
ferrite material
ball milling
formula
frequency wide
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CN114685154B (en
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黄刚
廖继红
李崇华
刘海
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China Magnetic Electronic Technology Co ltd
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Abstract

The invention provides a high-frequency wide-temperature ultralow-loss ferrite material which comprises a main formula and a dopant formula, wherein the main formula comprises the following components in parts by weight: fe2O370-72 mol%, MnO 20-22 mol% and ZnO 6-10 mol%, wherein the total proportion of the main formula is 100 mol%; relative to the total amount of the main formula, the components and the weight percentages in the dopant formula are respectively as follows: CaCO31～1000PPM、SnO2100～300PPM、Co2O350～80PPM、Bi2O350-100 PPM of nano SiO250 to 100PPM, CCTO 50 to 100 PPM. The invention aims to provide a high-frequency wide-temperature ultralow-loss material with high Bs value and low high-frequency lossA ferrite material.

Description

High-frequency wide-temperature ultralow-loss ferrite material and preparation process thereof
Technical Field
The invention relates to the technical field of soft magnetic ferrite cores, in particular to a high-frequency wide-temperature ultralow-loss ferrite material.
Background
At present, most of domestic enterprises engaged in ferrite material production are in PC95 material level and below. The high-performance low-loss ferrite material products are fewer, and the performance difference with the foreign products of the same type is larger. As for the high-frequency low-loss material capable of being produced in quantity, the market blank is more, so that domestic autonomous power supply manufacturing industry can only produce low-end products, and high-end products depend on the high-frequency ferrite core material of imported foreign well-known enterprises. The situation seriously restricts the development of the electronic information industry in China. More seriously, in recent years, China is continuously subjected to scientific and technological sanctions abroad, and the science and technology sanctions from communication enterprises to scientific research colleges and research institutions all suffer from serious impact. Under such a large environment, the independent high-frequency wide-temperature ultralow-power-loss soft magnetic ferrite material in China is researched and developed, and the method has great significance for the development of the electronic information industry in China.
Therefore, it is necessary to develop a ferrite material having a high Bs value and a low high frequency loss and a wide temperature range.
Disclosure of Invention
The invention aims to provide a ferrite material with high Bs value, high frequency, wide temperature and low loss.
The technical purpose of the invention is realized by the following technical scheme:
the high-frequency wide-temperature ultralow-loss ferrite material is characterized by comprising a main formula and a dopant formula, wherein the main formula comprises the following components in parts by weight:
Fe2O370～72mol％
MnO 20～22mol％
ZnO 6～10mol％
the proportion of each main formula is 100mol percent;
relative to the total amount of the main formula, the components and the weight percentages in the dopant formula are respectively as follows:
CaCO31～1000PPM
SnO2100～300PPM
Co2O350～80PPM
Bi2O350～100PPM
nano SiO250～100PPM
CCTO 50～100PPM。
By adopting the technical scheme, Co is added into the adulterant formula of the invention2O3，Co2O3The metal ion doping in the material can replace Fe at the B site of MnZn ferrite3+And Mn3+Therefore, the exchange effect of the A-B ultrasonic is increased, the heat resistance of the material is improved, the working temperature of the material is widened, the Curie temperature of the material is improved, the density of the sintered ferrite is also improved, and the saturation magnetic induction intensity of the material is effectively improved. And moreover, the CCTO is added in the doping formula, when the CCTO is adopted for doping to prepare the ferrite, the CCTO can be enriched in the crystal boundary of the MnZn power ferrite, and due to the characteristic of high resistivity, the speed of reducing the resistance of crystal grains along with the temperature can be slowed down, so that the increasing speed of high-frequency loss along with the temperature is delayed, and the high-frequency loss energy consumption of the material is effectively reduced.
As a further improvement of the invention, the dopant formula also comprises YBCO 10-50 PPM in percentage by weight.
By adopting the technical scheme, Co2O3Although the saturation flux density of the soft magnet can be improved during doping, the microstructure of the soft magnet is easy to grow discontinuously and the crystal is irregular, and bubbles are generated in each area inside the crystal, so that the initial permeability and the power loss performance of the material are influenced, therefore, when the added YBCO is sintered, the YBCO melting point is low, the YBCO can be preferentially melted and permeated, the connection force among crystal grains is improved, the crystal form of the material grows continuously, the generation of pores in the material is effectively reduced, the hysteresis loss of the material is effectively reduced, and the purpose of improving the connection force between Co and Co2O3The total power loss of the material is reduced under the condition that the guaranteed high Bs value of doping is high.
As a further improvement of the invention, the main formula comprises the following components in percentage by weight:
Fe2O371mol％
MnO 21mol％
ZnO 8mol％
the proportion of each main formula is 100mol percent;
relative to the total amount of the main formula, the components and the weight percentages in the dopant formula are respectively as follows:
CaCO3500PPM
SnO2200PPM
Co2O370PPM
Bi2O380PPM
nano SiO280PPM
CCTO 80PPM
YBCO 30PPM。
The invention also provides a preparation process of the high-frequency wide-temperature ultralow-loss ferrite material, which comprises the following steps of:
step S1: primary burdening: weighing materials according to the proportioning requirement to prepare a main formula raw material Fe2O3MnO and ZnO powder are mixed uniformly;
step S2: primary ball milling: putting the main formula powder which is preliminarily and uniformly mixed in the step S1 into a ball mill, and performing ball milling to obtain primary ball-milled powder;
step S3: pre-burning: heating the powder obtained by ball milling in the step S2 to a certain temperature in the air atmosphere, preserving the heat for 1-3 h, and cooling along with the furnace to obtain pre-sintered powder;
step S4: secondary burdening: addition of CaCO to the presintered powder3、SnO2、Co2O3、Bi2O3Nano SiO2Mixing CCTO and YBCO by stirring to form a mixture, adding polysiloxane into the mixture, and stirring and mixing to form a mixture;
step S5: secondary ball milling: putting the mixture obtained in the step S4 into a ball mill for secondary ball milling;
step S6: and (3) granulation: adding the mixture subjected to secondary ball milling into a binder to form small particles, and sieving;
step S7: and (3) pressing and forming: pressing the granulated small particles into annular raw blanks on pressing equipment;
step S8: and (3) secondary sintering: and sintering and molding the annular raw blank in the air atmosphere to obtain the target high-frequency wide-temperature ultralow-loss ferrite material.
By adopting the technical scheme, when the dopant formula is added for secondary burdening, the polysiloxane is added, and can improve the mixing dispersibility of the main formula and the dopant formula, so that the uniformity of CCTO enriched in the crystal boundary of MnZn power ferrite during the preparation of the ferrite is improved, the increasing effect of the CCTO on the resistivity of the prepared ferrite is improved, the eddy current loss of the material is further reduced, the high-frequency power loss of the material is reduced, in the process of preparing the ferrite material again, the step of rapid heating is also adopted after secondary ball milling, the additive polysiloxane in the ferrite can be removed at high temperature, the purity and density of the sintered ferrite are improved, and the saturation magnetic induction intensity of the material is improved.
As a further refinement of the present invention, the polysiloxane in step S4 is PSX 700.
As a further improvement of the present invention, between step S5 and step S6, there is further included step S5': removing impurities at high temperature: putting the mixture subjected to the secondary ball milling into an oven, and heating for 20-30 min;
as a further improvement of the invention, the mixture is put into an oven to be heated to 400-500 ℃.
As a further improvement of the invention, a PVA solution with 7-10 wt% of adhesive is added during granulation in step S6, and the mixture is formed into small granules by spray drying and then is sieved.
As a further improvement of the invention, the temperature of the pre-burning in the step S3 is 900-1050 ℃.
As a further improvement of the invention, the sintering temperature in the step S8 is 900-1370 ℃.
The invention has the beneficial effects that:
1. co is added into the adulterant formula of the invention2O3，Co2O3The metal ions in the MnZn ferrite are doped with Fe which can replace the B site of the MnZn ferrite3+And Mn3+Therefore, the exchange effect of the A-B ultrasonic is increased, the heat resistance of the material is improved, the working temperature of the material is widened, the Curie temperature of the material is improved, the density of the sintered ferrite is also improved, and the saturation magnetic induction intensity of the material is effectively improved.
2. According to the invention, the CCTO is added in the doping formula, when the CCTO is adopted for doping to prepare the ferrite, the CCTO can be enriched in the crystal boundary of the MnZn power ferrite, and due to the characteristic of high resistivity, the speed of reducing the resistance of crystal grains along with the temperature can be slowed down, so that the increasing speed of high-frequency loss along with the temperature is delayed, and the high-frequency loss energy consumption of the material is effectively reduced.
3. When the main formula and the adulterant adding formula are used for mixing, polysiloxane is added, and the mixing dispersibility of the main formula and the adulterant formula can be improved by the polysiloxane, so that the uniformity of CCTO enriched in the crystal boundary of MnZn power ferrite during the preparation of the ferrite is improved, the increasing effect of the CCTO on the resistivity of the prepared ferrite is improved, the eddy current loss of the material is further reduced, and the high-frequency power loss of the material is reduced.
4. In the preparation process, yttrium barium copper oxide YBCO and Co are added2O3Although the saturation flux density of the soft magnet can be improved during doping, the microstructure of the soft magnet is easy to grow discontinuously and the crystal is irregular, and bubbles are generated in each area inside the crystal, so that the initial permeability and the power loss performance of the material are influenced, therefore, when the added YBCO is sintered, the YBCO melting point is low, the YBCO can be preferentially melted and permeated, the connection force among crystal grains is improved, the crystal form of the material grows continuously, the generation of pores in the material is effectively reduced, the hysteresis loss of the material is effectively reduced, and the purpose of improving the connection force between Co and Co2O3The total power loss of the material is reduced under the condition that the guaranteed high Bs value of doping is high.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to specific embodiments. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments obtained by a person skilled in the art without any inventive work based on the embodiments of the present invention are within the scope of the present invention, and for the sake of experimenting, the samples of the embodiments were prepared as standard rings with a mean outer diameter of 25 × inner diameter of 15 × height of 7.5.
First, an embodiment
Example 1
A high-frequency wide-temperature ultralow-loss ferrite material comprises a main formula and a dopant formula, wherein the main formula comprises the following components in parts by weight:
Fe2O370mol％
MnO 20mol％
ZnO 10mol％
the proportion of each main formula is 100mol percent;
relative to the total amount of the main formula, the components and the weight percentages in the dopant formula are respectively as follows:
CaCO31PPM
SnO2100PPM
Co2O350PPM
Bi2O350PPM
nano SiO250PPM
CCTO 50PPM
YBCO 10PPM。
The invention also provides a preparation process of the high-frequency wide-temperature ultralow-loss ferrite material, which comprises the following steps of:
step S1: primary burdening: weighing the materials according to the proportioning requirement to prepare the main formula raw material Fe2O3MnO and ZnO powder are mixed uniformly;
step S2: primary ball milling: putting the main formula powder which is preliminarily and uniformly mixed in the step S1 into a ball mill, and performing ball milling to obtain primary ball-milled powder;
step S3: pre-burning: heating the powder obtained by ball milling in the step S2 to 900 ℃ in the air atmosphere, preserving the heat for 1h, and cooling along with the furnace to obtain pre-sintered powder;
step S4: secondary burdening: addition of CaCO to the presintered powder3、SnO2、Co2O3、Bi2O3Nano SiO 22Mixing and stirring CCTO and YBCO to form a mixture, adding polysiloxane PSX700 into the mixture, and stirring and mixing to form a mixture;
step S5: secondary ball milling: putting the mixture obtained in the step S4 into a ball mill for secondary ball milling;
step S5': removing impurities at high temperature: putting the mixture subjected to the secondary ball milling into an oven, heating to 400 ℃, and keeping for 20 min;
step S6: and (3) granulation: adding the mixture subjected to secondary ball milling into a PVA solution added with 7 wt% of a binding agent, performing spray drying to form small particles, and sieving;
step S7: and (3) pressing and forming: pressing the granulated small particles into annular raw blanks on pressing equipment;
step S8: and (3) secondary sintering: and sintering and molding the annular raw blank in an air atmosphere at 900 ℃ to obtain the target high-frequency wide-temperature ultralow-loss ferrite material.
Example 2
A high-frequency wide-temperature ultralow-loss ferrite material comprises a main formula and a dopant formula, wherein the main formula comprises the following components in parts by weight:
Fe2O372mol％
MnO 22mol％
ZnO 6mol％
the proportion of each main formula is 100 mol%;
relative to the total amount of the main formula, the components and the weight percentages in the dopant formula are respectively as follows:
CaCO31000PPM
SnO2300PPM
Co2O380PPM
Bi2O3100PPM
nano SiO2100PPM
CCTO 100PPM
YBCO 50PPM。
The invention also provides a preparation process of the high-frequency wide-temperature ultralow-loss ferrite material, which comprises the following steps of:
step S1: primary burdening: weighing the materials according to the proportioning requirement to prepare the main formula raw material Fe2O3MnO and ZnO powder are mixed uniformly;
step S2: primary ball milling: putting the main formula powder which is preliminarily and uniformly mixed in the step S1 into a ball mill, and performing ball milling to obtain primary ball-milled powder;
step S3: pre-burning: heating the powder obtained by ball milling in the step S2 to 1050 ℃ in the air atmosphere, preserving the temperature for 3h, and cooling along with the furnace to obtain pre-sintered powder;
step S4: secondary burdening: addition of CaCO to the presintered powder3、SnO2、Co2O3、Bi2O3Nano SiO2Mixing and stirring CCTO and YBCO to form a mixture, adding polysiloxane PSX700 into the mixture, and stirring and mixing to form a mixture;
step S5: secondary ball milling: putting the mixture obtained in the step S4 into a ball mill for secondary ball milling;
step S5': removing impurities at high temperature: placing the mixture after the secondary ball milling into an oven, heating to 500 ℃, and keeping for 30 min;
step S6: and (3) granulation: adding the mixture subjected to the secondary ball milling into PVA solution added with 10 wt% of adhesive, and sieving after forming small particles by adopting spray drying;
step S7: and (3) pressing and forming: pressing the granulated small particles on pressing equipment into annular raw blanks;
step S8: and (3) secondary sintering: and sintering and molding the annular raw blank in an air atmosphere at 1370 ℃ to obtain the target high-frequency wide-temperature ultralow-loss ferrite material.
Example 3
A high-frequency wide-temperature ultralow-loss ferrite material comprises a main formula and a dopant formula, wherein the main formula comprises the following components in parts by weight:
Fe2O371mol％
MnO 21mol％
ZnO 8mol％
the proportion of each main formula is 100 mol%;
relative to the total amount of the main formula, the components and the weight percentages in the dopant formula are respectively as follows:
CaCO3500PPM
SnO2200PPM
Co2O370PPM
Bi2O380PPM
nano SiO280PPM
CCTO 80PPM
YBCO 30PPM。
The invention also provides a preparation process of the high-frequency wide-temperature ultralow-loss ferrite material, which comprises the following steps of:
step S1: primary burdening: weighing the materials according to the proportioning requirement to prepare the main formula raw material Fe2O3MnO and ZnO powder are mixed uniformly;
step S2: primary ball milling: putting the main formula powder which is preliminarily and uniformly mixed in the step S1 into a ball mill, and performing ball milling to obtain primary ball-milled powder;
step S3: pre-burning: heating the powder obtained by ball milling in the step S2 to 950 ℃ in the air atmosphere, preserving the heat for 2 hours, and cooling along with the furnace to obtain pre-sintered powder;
step S4: secondary burdening: addition of CaCO to the presintered powder3、SnO2、Co2O3、Bi2O3Nano SiO2Mixing and stirring CCTO and YBCO to form a mixture, adding polysiloxane PSX700 into the mixture, and stirring and mixing to form a mixture;
step S5: secondary ball milling: putting the mixture obtained in the step S4 into a ball mill for secondary ball milling;
step S5': removing impurities at high temperature: putting the mixture subjected to the secondary ball milling into an oven, heating to 450 ℃, and keeping for 25 min;
step S6: and (3) granulation: adding the mixture subjected to secondary ball milling into a PVA solution added with 8 wt% of a binding agent, forming small particles by adopting spray drying, and sieving;
step S7: and (3) pressing and forming: pressing the granulated small particles into annular raw blanks on pressing equipment;
step S8: and (3) secondary sintering: and sintering and molding the annular raw blank in an air atmosphere of 1200 ℃ to obtain the target high-frequency wide-temperature ultralow-loss ferrite material.
Comparative example 1
A high-frequency wide-temperature ultralow-loss ferrite material comprises a main formula and a dopant formula, wherein the main formula comprises the following components in parts by weight:
Fe2O371mol％
MnO 21mol％
ZnO 8mol％
the proportion of each main formula is 100mol percent;
relative to the total amount of the main formula, the components and the weight percentages in the dopant formula are respectively as follows:
CaCO3500PPM
SnO2200PPM
Bi2O380PPM
nano SiO280PPM
CCTO 80PPM
YBCO 30PPM。
The invention also provides a preparation process of the high-frequency wide-temperature ultralow-loss ferrite material, which comprises the following steps of:
step S1: primary material preparation: weighing the materials according to the proportioning requirement to prepare the main formula raw material Fe2O3MnO and ZnO powder are mixed uniformly;
step S2: primary ball milling: putting the main formula powder which is preliminarily and uniformly mixed in the step S1 into a ball mill, and performing ball milling to obtain primary ball-milled powder;
step S3: pre-burning: heating the powder obtained by ball milling in the step S2 to 950 ℃ in the air atmosphere, preserving the heat for 2 hours, and cooling along with the furnace to obtain pre-sintered powder;
step S4: secondary burdening: addition of CaCO to the presintered powder3、SnO2、Bi2O3Nano SiO2Mixing and stirring CCTO and YBCO to form a mixture, adding polysiloxane PSX700 into the mixture, and stirring and mixing to form a mixture;
step S5: secondary ball milling: putting the mixture obtained in the step S4 into a ball mill for secondary ball milling;
step S5': removing impurities at high temperature: placing the mixture subjected to the secondary ball milling into an oven, heating to 450 ℃, and keeping for 25 min;
step S6: and (3) granulation: adding the mixture subjected to secondary ball milling into a PVA solution added with 8 wt% of a binding agent, forming small particles by adopting spray drying, and sieving;
step S7: and (3) pressing and forming: pressing the granulated small particles into annular raw blanks on pressing equipment;
step S8: and (3) secondary sintering: and sintering and molding the annular raw blank in an air atmosphere of 1200 ℃ to obtain the target high-frequency wide-temperature ultralow-loss ferrite material.
Comparative example 2
A high-frequency wide-temperature ultralow-loss ferrite material comprises a main formula and a dopant formula, wherein the main formula comprises the following components in parts by weight:
Fe2O371mol％
MnO 21mol％
ZnO 8mol％
the proportion of each main formula is 100mol percent;
relative to the total amount of the main formula, the components and the weight percentages in the dopant formula are respectively as follows:
CaCO3500PPM
SnO2200PPM
Co2O370PPM
Bi2O380PPM
nano SiO280PPM
CCTO 80PPM。
The invention also provides a preparation process of the high-frequency wide-temperature ultralow-loss ferrite material, which comprises the following steps of:
step S1: primary burdening: weighing the materials according to the proportioning requirement to prepare the main formula raw material Fe2O3MnO and ZnO powder are mixed uniformly;
step S2: primary ball milling: putting the main formula powder which is preliminarily and uniformly mixed in the step S1 into a ball mill, and performing ball milling to obtain primary ball-milled powder;
step S3: pre-burning: heating the powder obtained by ball milling in the step S2 to 950 ℃ in the air atmosphere, preserving the heat for 2 hours, and cooling along with the furnace to obtain pre-sintered powder;
step S4: secondary burdening: addition of CaCO to the presintered powder3、SnO2、Co2O3、Bi2O3Nano SiO2Mixing and stirring CCTO to form a mixture, adding polysiloxane PSX700 into the mixture, and stirring and mixing to form a mixture;
step S5: secondary ball milling: putting the mixture obtained in the step S4 into a ball mill for secondary ball milling;
step S5': removing impurities at high temperature: placing the mixture subjected to the secondary ball milling into an oven, heating to 450 ℃, and keeping for 25 min;
step S6: and (3) granulation: adding the mixture subjected to secondary ball milling into a PVA solution added with 8 wt% of a binding agent, forming small particles by adopting spray drying, and sieving;
step S7: and (3) pressing and forming: pressing the granulated small particles into annular raw blanks on pressing equipment;
step S8: and (3) secondary sintering: and sintering and molding the annular raw blank in an air atmosphere of 1200 ℃ to obtain the target high-frequency wide-temperature ultralow-loss ferrite material.
Comparative example 3
A high-frequency wide-temperature ultralow-loss ferrite material comprises a main formula and a dopant formula, wherein the main formula comprises the following components in parts by weight:
Fe2O371mol％
MnO 21mol％
ZnO 8mol％
the proportion of each main formula is 100mol percent;
relative to the total amount of the main formula, the components and the weight percentages in the dopant formula are respectively as follows:
CaCO3500PPM
SnO2200PPM
Bi2O380PPM
nano SiO280PPM
CCTO 80PPM。
The invention also provides a preparation process of the high-frequency wide-temperature ultralow-loss ferrite material, which comprises the following steps of:
step S1: primary burdening: weighing the materials according to the proportioning requirement to prepare the main formula raw material Fe2O3MnO and ZnO powder are mixed uniformly;
step S2: primary ball milling: putting the main formula powder which is preliminarily and uniformly mixed in the step S1 into a ball mill, and performing ball milling to obtain primary ball-milled powder;
step S3: pre-burning: heating the powder obtained by ball milling in the step S2 to 950 ℃ in the air atmosphere, preserving the heat for 2 hours, and cooling along with the furnace to obtain pre-sintered powder;
step S4: secondary burdening: addition of CaCO to the presintered powder3、SnO2、Bi2O3Nano SiO2CCTO is stirred and mixed to form a mixture, and then polysiloxane PSX700 is added into the mixture to be stirred and mixed to form a mixture;
step S5: secondary ball milling: putting the mixture obtained in the step S4 into a ball mill for secondary ball milling;
step S5': removing impurities at high temperature: putting the mixture subjected to the secondary ball milling into an oven, heating to 450 ℃, and keeping for 25 min;
step S6: and (3) granulation: adding the mixture subjected to secondary ball milling into a PVA solution added with 8 wt% of a binding agent, forming small particles by adopting spray drying, and sieving;
step S7: and (3) pressing and forming: pressing the granulated small particles into annular raw blanks on pressing equipment;
step S8: and (3) secondary sintering: and sintering and molding the annular raw blank in an air atmosphere of 1200 ℃ to obtain the target high-frequency wide-temperature ultralow-loss ferrite material.
Comparative example 4
A high-frequency wide-temperature ultralow-loss ferrite material comprises a main formula and a dopant formula, wherein the main formula comprises the following components in parts by weight:
Fe2O371mol％
MnO 21mol％
ZnO 8mol％
the proportion of each main formula is 100mol percent;
relative to the total amount of the main formula, the components and the weight percentages in the dopant formula are respectively as follows:
CaCO3500PPM
SnO2200PPM
Co2O370PPM
Bi2O380PPM
nano SiO 2280PPM
YBCO 30PPM。
The invention also provides a preparation process of the high-frequency wide-temperature ultralow-loss ferrite material, which comprises the following steps of:
step S1: primary burdening: weighing the materials according to the proportioning requirement to prepare the main formula raw material Fe2O3MnO and ZnO powder are mixed evenly in a preliminary way;
step S2: primary ball milling: putting the main formula powder which is preliminarily and uniformly mixed in the step S1 into a ball mill, and performing ball milling to obtain primary ball-milled powder;
step S3: pre-burning: heating the powder obtained by ball milling in the step S2 to 950 ℃ in the air atmosphere, preserving the heat for 2 hours, and cooling along with the furnace to obtain pre-sintered powder;
step S4: secondary burdening: addition of CaCO to the presintered powder3、SnO2、Co2O3、Bi2O3Nano SiO 22Mixing YBCO to form a mixture, adding polysiloxane PSX700 into the mixture, and mixing to form a mixture;
step S5: secondary ball milling: putting the mixture obtained in the step S4 into a ball mill for secondary ball milling;
step S5': removing impurities at high temperature: putting the mixture subjected to the secondary ball milling into an oven, heating to 450 ℃, and keeping for 25 min;
step S6: and (3) granulation: adding the mixture subjected to secondary ball milling into a PVA solution added with 8 wt% of a binding agent, forming small particles by adopting spray drying, and sieving;
step S7: and (3) pressing and forming: pressing the granulated small particles into annular raw blanks on pressing equipment;
step S8: and (3) secondary sintering: and sintering and molding the annular raw blank in an air atmosphere of 1200 ℃ to obtain the target high-frequency wide-temperature ultralow-loss ferrite material.
Comparative example 5
A high-frequency wide-temperature ultralow-loss ferrite material comprises a main formula and a dopant formula, wherein the main formula comprises the following components in parts by weight:
Fe2O371mol％
MnO 21mol％
ZnO 8mol％
the proportion of each main formula is 100mol percent;
relative to the total amount of the main formula, the components and the weight percentages in the dopant formula are respectively as follows:
CaCO3500PPM
SnO2200PPM
Co2O370PPM
Bi2O380PPM
nano SiO 2280PPM
CCTO 80PPM
YBCO 30PPM。
The invention also provides a preparation process of the high-frequency wide-temperature ultralow-loss ferrite material, which comprises the following steps of:
step S1: primary burdening: weighing the materials according to the proportioning requirement to prepare the main formula raw material Fe2O3MnO and ZnO powder are mixed uniformly;
step S2: primary ball milling: putting the main formula powder which is preliminarily and uniformly mixed in the step S1 into a ball mill, and performing ball milling to obtain primary ball-milled powder;
step S3: pre-burning: heating the powder obtained by ball milling in the step S2 to 950 ℃ in the air atmosphere, preserving the heat for 2 hours, and cooling along with the furnace to obtain pre-sintered powder;
step S4: secondary burdening: addition of CaCO to the presintered powder3、SnO2、Co2O3、Bi2O3Nano SiO 22Mixing CCTO and YBCO to form a mixture;
step S5: secondary ball milling: putting the mixture obtained in the step S4 into a ball mill for secondary ball milling;
step S5': removing impurities at high temperature: putting the mixture subjected to the secondary ball milling into an oven, heating to 450 ℃, and keeping for 25 min;
step S6: and (3) granulation: adding the mixture subjected to secondary ball milling into a PVA solution added with 8 wt% of a binding agent, forming small particles by adopting spray drying, and sieving;
step S7: and (3) pressing and forming: pressing the granulated small particles into annular raw blanks on pressing equipment;
step S8: and (3) secondary sintering: and sintering and molding the annular raw blank in an air atmosphere of 1200 ℃ to obtain the target high-frequency wide-temperature ultralow-loss ferrite material.
Comparative example 6
A high-frequency wide-temperature ultralow-loss ferrite material comprises a main formula and a dopant formula, wherein the main formula comprises the following components in parts by weight:
Fe2O371mol％
MnO 21mol％
ZnO 8mol％
the proportion of each main formula is 100 mol%;
relative to the total amount of the main formula, the components and the weight percentages in the dopant formula are respectively as follows:
CaCO3500PPM
SnO2200PPM
Bi2O380PPM
nano SiO280PPM。
The invention also provides a preparation process of the high-frequency wide-temperature ultralow-loss ferrite material, which comprises the following steps of:
step S1: at a timePreparing materials: weighing the materials according to the proportioning requirement to prepare the main formula raw material Fe2O3MnO and ZnO powder are mixed uniformly;
step S2: primary ball milling: putting the main formula powder which is preliminarily and uniformly mixed in the step S1 into a ball mill, and performing ball milling to obtain primary ball-milled powder;
step S3: pre-burning: heating the powder obtained by ball milling in the step S2 to 950 ℃ in the air atmosphere, preserving the heat for 2 hours, and cooling along with the furnace to obtain pre-sintered powder;
step S4: secondary burdening: addition of CaCO to the presintered powder3、SnO2、Bi2O3Nano SiO2Stirring and mixing to form a mixture;
step S5: secondary ball milling: putting the mixture obtained in the step S4 into a ball mill for secondary ball milling;
step S6: and (3) granulation: adding the mixture subjected to secondary ball milling into a PVA solution added with 8 wt% of a binding agent, performing spray drying to form small particles, and sieving;
step S7: and (3) pressing and forming: pressing the granulated small particles into annular raw blanks on pressing equipment;
step S8: and (3) secondary sintering: and sintering and molding the annular raw blank in an air atmosphere of 1200 ℃ to obtain the target high-frequency wide-temperature ultralow-loss ferrite material.
The soft magnetic ferrite materials prepared in examples 1 to 3 and comparative examples 1 to 6 were subjected to a magnetic property test using a standard ring sample having an outer diameter of 25 × an inner diameter of 15 × a height of 7.5, and compared with the properties of TDK PC95 of japan, and the results are as follows:
TABLE 1 magnetic Property results of the respective samples
Figure BDA0003618549150000131
Figure BDA0003618549150000141
The principles and embodiments of the present invention are explained herein using specific examples, which are set forth only to help understand the method and its core ideas of the present invention. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.

Claims (10)

1. The high-frequency wide-temperature ultralow-loss ferrite material is characterized by comprising a main formula and a dopant formula, wherein the main formula comprises the following components in parts by weight:
Fe2O3 70～72mol％
MnO 20～22mol％
ZnO 6～10mol％
the proportion of each main formula is 100mol percent;
relative to the total amount of the main formula, the components and the weight percentages in the dopant formula are respectively as follows:
CaCO3 1～1000PPM
SnO2 100～300PPM
Co2O3 50～80PPM
Bi2O3 50～100PPM
nano SiO2 50～100PPM
CCTO 50～100PPM。
2. The high-frequency wide-temperature ultralow-loss ferrite material as claimed in claim 1, wherein the dopant formulation further comprises YBCO 10-50 PPM in percentage by weight.
3. The high-frequency wide-temperature ultralow-loss ferrite material as claimed in claim 1, wherein the main formula comprises the following components in percentage by weight:
Fe2O3 71mol％
MnO 21mol％
ZnO 8mol％
the proportion of each main formula is 100mol percent;
relative to the total amount of the main formula, the components and the weight percentages in the dopant formula are respectively as follows:
CaCO3 500PPM
SnO2 200PPM
Co2O3 70PPM
Bi2O3 80PPM
nano SiO2 80PPM
CCTO 80PPM
YBCO 30PPM。
4. The preparation process of the high-frequency wide-temperature ultralow-loss ferrite material according to claim 1, characterized by comprising the following steps:
step S1: primary burdening: weighing materials according to the proportioning requirement to prepare a main formula raw material Fe2O3MnO and ZnO powder are mixed uniformly;
step S2: primary ball milling: putting the main formula powder which is preliminarily and uniformly mixed in the step S1 into a ball mill, and performing ball milling to obtain primary ball-milled powder;
step S3: pre-burning: heating the powder obtained by ball milling in the step S2 to a certain temperature in the air atmosphere, preserving the heat for 1-3 h, and cooling along with the furnace to obtain pre-sintered powder;
step S4: secondary burdening: addition of CaCO to pre-sinter powder3、SnO2、Co2O3、Bi2O3Nano SiO2Mixing CCTO and YBCO by stirring to form a mixture, adding polysiloxane into the mixture, and stirring and mixing to form a mixture;
step S5: secondary ball milling: putting the mixture obtained in the step S4 into a ball mill for secondary ball milling;
step S6: and (3) granulation: adding the mixture subjected to the secondary ball milling into a binder to form small particles, and then sieving;
step S7: and (3) pressing and forming: pressing the granulated small particles into annular raw blanks on pressing equipment;
step S8: and (3) secondary sintering: and sintering and molding the annular raw blank in an air atmosphere to obtain the target high-frequency wide-temperature ultralow-loss ferrite material.
5. The high frequency wide temperature ultra low loss ferrite material of claim 4, wherein the polysiloxane in step S4 is PSX 700.
6. The high-frequency wide-temperature ultra-low loss ferrite material of claim 4, further comprising, between step S5 and step S6, step S5': removing impurities at high temperature: and putting the mixture subjected to the secondary ball milling into an oven, and heating for 20-30 min.
7. The high frequency wide temperature ultra low loss ferrite material of claim 6, wherein the mixture is placed in an oven and warmed to 400-500 ℃.
8. The high-frequency wide-temperature ultra-low loss ferrite material as claimed in claim 4, wherein a PVA solution with a binder of 7-10 wt% is added during granulation in step S6, and the mixture is formed into small particles by spray drying and then sieved.
9. The high frequency wide temperature ultra low loss ferrite material of claim 4, wherein the temperature of the pre-firing of step S3 is 900-1050 ℃.
10. The high-frequency wide-temperature ultra-low loss ferrite material of claim 4, wherein the sintering temperature in step S8 is 900 ℃ -1370 ℃.
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