CN111039666A - Manganese zinc ferrite material with ultrahigh saturation magnetic flux density and preparation method thereof - Google Patents

Manganese zinc ferrite material with ultrahigh saturation magnetic flux density and preparation method thereof Download PDF

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CN111039666A
CN111039666A CN201911363158.4A CN201911363158A CN111039666A CN 111039666 A CN111039666 A CN 111039666A CN 201911363158 A CN201911363158 A CN 201911363158A CN 111039666 A CN111039666 A CN 111039666A
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heat preservation
magnetic flux
flux density
oxygen content
saturation magnetic
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张强原
邢冰冰
缪思敏
宋岩岩
焦帅帅
张志新
李小龙
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TDG Holding Co Ltd
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TDG Holding Co Ltd
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Priority to PCT/CN2020/070794 priority patent/WO2021128477A1/en
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Abstract

The invention discloses a manganese-zinc ferrite material with ultrahigh saturation magnetic flux density, which consists of a main component and an auxiliary component, wherein the main component is calculated by Fe through oxides2O3:55.25~56.25mol%,ZnO:2.5~3.5mol%,Co2O30.10 to 0.20mol%, and the balance being MnO; the minor component comprising Nb by weight of the major component2O5:0.01~0.06wt%、CaCO3:0.05~0.15wt%、NiO:0~0.05wt%,V2O5:0.01~0.04wt%、SiO2:0~0.01wt%、TiO2:0~0.05wt%、Ta2O50 to 0.05 wt%. The power consumption of the manganese-zinc material prepared by the invention is less than 250kW/m at 25 ℃ and 100 ℃ under 3MHz and 30mT3The saturation magnetic flux density at 100 ℃ reaches more than 460mT, so that the manganese-zinc ferrite material is suitable for high-frequency transformersAnd the need for server inductance.

Description

Manganese zinc ferrite material with ultrahigh saturation magnetic flux density and preparation method thereof
Technical Field
The invention relates to a manganese-zinc ferrite material and a preparation method thereof, in particular to a manganese-zinc ferrite material with ultrahigh saturation magnetic flux density and a preparation method thereof.
Background
As an important component of modern electronic devices, switching power supplies are widely used in various fields of industrial, civil and military electronic devices, and the miniaturization development of electronic products requires small size, light weight and high reliability. The volume and the weight of a main transformer of a core component of the power supply occupy a significant part of the power supply, according to the working principle of the transformer, the output voltage is in direct proportion to the frequency (V = KfBmAN), K is a form factor, Bm is the working magnetic induction intensity, f is the switching frequency, A is the sectional area of a magnetic core, and N is the number of turns of a winding, so that the working frequency of the power supply is required to be improved by reducing the volume and the weight, the soft magnetic ferrite material of a DC-DC module of the power supply has the characteristic of high frequency and low loss, and the popularization of a semiconductor GaN on the power supply accelerates the requirement of the high frequency material; on the other hand, as the electronic transformer needs to output higher energy density and output voltage is lower and lower, output current is higher and higher, so that the soft magnetic material is required to have higher saturation magnetic flux density to meet the requirement that the magnetic core is not saturated under high current.
The server is a high-performance computer in a network environment, the cloud computing technology is mature gradually, and a most suitable platform is provided for the rise of the server market. The new IT era marked by cloud computing and big data has pushed the revolution of server technology and market. With the development of application hot spot fields such as virtualization, cloud computing, desktop cloud, big data, memory database application, high-performance operation and the like in the future, the development of a high-temperature energy-saving high-density server is further promoted, and the high-temperature energy-saving high-density server has high saturation magnetic flux density and low high-frequency loss for ferrite materials using the high-temperature energy-saving high-density server.
In order to meet the requirements of high frequency, integration and miniaturization of the inductance of the electronic transformer and the server, the requirements of the materials are also improved: on one hand, the high-frequency loss is low; and on the other hand, has higher saturation magnetic flux density. However, the traditional materials are mainly concentrated below 500kHz, and the saturation magnetic flux density is low, so that the development requirement of modern technology is difficult to meet.
Disclosure of Invention
The invention provides a manganese-zinc ferrite material with ultrahigh saturation magnetic flux density and a preparation method thereof, aiming at overcoming the defects of the prior art, wherein the cut-off frequency can reach 8MHz, and the power consumption of the prepared manganese-zinc ferrite material is less than 250kW/m at 25 ℃ and 100 ℃ under 3MHz and 30mT3And the saturation magnetic flux density at 100 ℃ reaches more than 460mT, so that the manganese-zinc ferrite material meets the requirements of high-frequency transformers and server inductors.
The technical scheme adopted by the invention for solving the technical problem is as follows: a Mn-Zn ferrite material with ultrahigh saturation magnetic flux density is composed of main component (Fe calculated by oxide) and auxiliary component(s)2O3:55.25~56.25mol%,ZnO:2.5~3.5mol%,Co2O30.10 to 0.20mol%, and the balance being MnO; the minor component comprising Nb by weight of the major component2O5:0.01~0.06wt%、CaCO3:0.05~0.15wt%、NiO:0~0.05wt%,V2O5:0.01~0.04wt%、SiO2:0~0.01wt%、TiO2:0~0.05wt% 、Ta2O5:0~0.05wt%。
The preparation method of the manganese-zinc ferrite material with the ultrahigh saturation magnetic flux density comprises the following steps:
1) preparing materials: according to the main formula Fe2O3、ZnO 、Co2O3Weighing the mixture according to the proportion of MnO, mixing and sanding for 15-30 min;
2) pre-burning: pre-burning the mixed powder at 850-1050 ℃;
3) sanding: and adding the additive into the pre-sintered material for secondary mixing treatment, wherein the sanding time is 80-140 min, and the particle size is 0.3-0.6 mu m.
4) And (3) granulation: drying the ground slurry and then granulating;
5) molding: pressing the granulated particles into blanks T12.7 x 8 x 7;
6) and (3) sintering: a two-stage heat preservation equilibrium oxygen partial pressure sintering method is adopted for the blank in a kiln, the first-stage sintering temperature is 1200-1240 ℃, the heat preservation time is 4-8 hours, wherein the oxygen content in the first 0-1 hour is 3.5-4%, and the oxygen content in the later heat preservation time is 2.0-3.0%; the temperature of the first section in the cooling section is 1050-1100 ℃, the heat preservation time is 30-100 min, and the oxygen content is 0.3-1.0%.
The preparation method has the beneficial effects that the power consumption of the prepared manganese-zinc material is less than 250kW/m at 25 ℃ and 100 ℃ under 3MHz 30mT by controlling the composition and content of the main component and the auxiliary component and optimizing the sintering process3And the saturation magnetic flux density at 100 ℃ reaches more than 460mT, so that the manganese-zinc ferrite material meets the requirements of high-frequency transformers and server inductors.
Detailed Description
Example 1: the manganese-zinc ferrite material with ultrahigh saturation magnetic flux density comprises a main component and an auxiliary component, wherein the main component is Fe2O3:55.25mol%,ZnO:3.2mol% ,Co2O3: 0.20mol% and the balance MnO; subcomponent Nb2O5:0.02wt%、CaCO3:0.05wt%、NiO:0.02wt%,V2O5:0.02wt%、SiO2:0.008wt%、TiO2:0.01wt%,Ta2O50.02wt%, the above-mentioned secondary components being Fe2O3ZnO, MnO and Co2O3The total weight percent of (c) is calculated.
A preparation method for preparing the manganese-zinc ferrite material with high frequency, wide temperature, low loss and ultrahigh saturation magnetic flux density in the embodiment 1 comprises the following steps:
1) preparing materials: according to the main formula Fe2O3、ZnO、Co2O3Weighing the MnO in proportion, mixing and sanding for 15 min;
2) pre-burning: presintering the mixed powder, presintering at 900 ℃, and keeping the temperature for 2 h;
3) sanding: adding the additive into the pre-sintered material, performing vibration grinding, and then performing secondary mixing treatment, wherein the sand grinding time is 80 min; the grain size is 0.52 um;
4) and (3) granulation: drying the ground slurry and then granulating;
5) molding: pressing the granulated particles into blanks T12.7 x 8 x 7;
6) and (3) sintering: and sintering the blank in a kiln by adopting balanced oxygen partial pressure, wherein the first-stage sintering temperature is 1240 ℃, the heat preservation time is 4 hours, the heat preservation oxygen content in the first 1 hour is 3.5 percent, the heat preservation oxygen content in the later 3 hours is 2.8 percent, and the first-stage temperature is 1060 ℃, the heat preservation time is 60 minutes, and the oxygen content is 0.6 percent.
Example 2: a Mn-Zn ferrite material with ultrahigh saturation magnetic flux density is composed of main component (Fe) and auxiliary component (Fe)2O3:55.5mol%,ZnO:3.5mol% ,Co2O3: 0.15mol% and the balance MnO; subcomponent Nb2O5:0.04wt%、CaCO3:0.05wt%、NiO:0.03wt%,V2O5:0.03wt%、SiO2:0.01wt%、TiO2:0.03wt%、Ta2O50.01wt% and the above-mentioned secondary components are Fe2O3ZnO, MnO and Co2O3The total weight percent of (c) is calculated.
A method for preparing the manganese-zinc ferrite material with ultrahigh saturation magnetic flux density according to embodiment 2, comprising the following steps:
1) preparing materials: according to the main formula Fe2O3、ZnO、Co2O3Weighing MnO in proportion, mixing and sanding for 25 min;
2) pre-burning: pre-burning the mixed powder, wherein the pre-burning temperature is 1000 ℃, and keeping the temperature for 2 h;
3) sanding: adding the additive into the pre-sintered material, performing vibration grinding, and then performing secondary mixing treatment, wherein the sand grinding time is 100min, and the particle size is 0.46 mu m;
4) and (3) granulation: drying the ground slurry and then granulating;
5) molding: pressing the granulated particles into blanks T12.7 x 8 x 7;
6) and (3) sintering: sintering the blank in a kiln by adopting two-stage heat preservation and balanced oxygen partial pressure, wherein the first-stage sintering temperature is 1220 ℃, the heat preservation time is 6 hours, the heat preservation oxygen content in the first 1 hour is 4.0%, and the heat preservation oxygen content in the next 5 hours is 2.6%; one section is insulated for 100min at the temperature of 1100 ℃ in the cooling section, and the oxygen content is 0.4 percent.
Example 3: the manganese-zinc ferrite material with ultrahigh saturation magnetic flux density comprises a main component and auxiliary components, wherein the main component is Fe2O3:56.2mol%,ZnO:2.5mol% ,Co2O3:0.10 mol% and the balance MnO; subcomponent Nb2O5:0.01wt%、NiO:0.05wt%,CaCO3:0.08wt%、V2O5:0.01wt%、SiO20.005wt%, TiO2:0.05wt%、Ta2O50.02wt%, and the above-mentioned secondary components are Fe2O3ZnO, MnO and Co2O3The total weight percent of (c) is calculated.
A preparation method of the manganese zinc ferrite material with the ultrahigh saturation magnetic flux density in the embodiment 3 comprises the following steps:
1) preparing materials: according to the main formula Fe2O3、ZnO、Co2O3Weighing the MnO in proportion, mixing and sanding for 15 min;
2) pre-burning: presintering the mixed powder, wherein the presintering temperature is 1050 ℃, and keeping the temperature for 2 hours;
3) sanding: adding the additive into the pre-sintered material, performing vibration grinding, and then performing secondary mixing treatment, wherein the sand grinding time is 140min, and the particle size is 0.32 mu m;
4) and (3) granulation: drying the ground slurry and then granulating;
5) molding: pressing the granulated particles into blanks T12.7 x 8 x 7;
6) and (3) sintering: sintering the blank in a kiln by adopting two-stage heat preservation and balanced oxygen partial pressure, wherein the first-stage sintering temperature is 1240 ℃, the heat preservation time is 4 hours, the heat preservation oxygen content in the first 0.5 hour is 3.5 percent, and the heat preservation oxygen content in the later 3.5 hours is 2.4 percent; one section is kept at the temperature of 1070 ℃ for 100min in a cooling section, and the oxygen content is 1.0 percent.
Example 4: a Mn-Zn ferrite material with ultrahigh saturation magnetic flux density is composed of main component and auxiliary componentThe main component is Fe2O3:55.6mol%,ZnO:2.8mol% ,Co2O3: 0.20wt% and the balance MnO; subcomponent Nb2O5:0.04wt%、CaCO3:0.10wt%、NiO:0.01wt%,V2O5:0.03wt%、SiO2:0.01wt%wt%、Ta2O5:0.02wt%、TiO20.05wt%, and the above-mentioned secondary components are Fe2O3ZnO, MnO and Co2O3The total weight percent of (c) is calculated.
A method for preparing the manganese-zinc ferrite material with ultrahigh saturation magnetic flux density of embodiment 4 comprises the following steps:
1) preparing materials: according to the main formula Fe2O3Weighing ZnO and MnO in proportion, mixing and sanding for 30 min;
2) pre-burning: pre-burning the mixed powder, wherein the pre-burning temperature is 950 ℃, and keeping the temperature for 2 hours;
3) sanding: adding the additive into the pre-sintered material, performing vibration grinding, and then performing secondary mixing treatment, wherein the sand grinding time is 80min, and the particle size is 0.55 mu m;
4) and (3) granulation: drying the ground slurry and then granulating;
5) molding: pressing the granulated particles into blanks T12.7 x 8 x 7;
6) and (3) sintering: sintering the blank in a kiln by adopting two-stage heat preservation and balanced oxygen partial pressure, wherein the first-stage sintering temperature is 1200 ℃, the heat preservation time is 8 hours, the heat preservation oxygen content in the first 1 hour is 3.8%, and the heat preservation oxygen content in the next 7 hours is 2.0%; the temperature of the cooling section of the first section is 1100 ℃, the temperature is kept for 60min, and the oxygen content is calculated according to the equilibrium oxygen partial pressure.
Comparative example 1
Comparative example 1 procedure and method, selection of Fe as the principal component2O3:55mol%,ZnO:4mol% ,Co2O3:0.05 mol% and the balance MnO; nb as a subcomponent2O5:0.04wt%、CaCO3:0.05wt%、V2O5:0.02wt%、TiO2:0.01wt%,Ta2O50.01wt%, the above minor ingredientsIs divided by Fe2O3ZnO, MnO and Co2O3The total weight percent of (c) is calculated. The test was carried out according to the following procedure.
1) Preparing materials: according to the main formula Fe2O3、ZnO、Co2O3Weighing the MnO in proportion, mixing and sanding for 15 min;
2) pre-burning: pre-burning the mixed powder, wherein the pre-burning temperature is 950 ℃, and keeping the temperature for 2 hours;
3) sanding: adding the additive into the pre-sintered material, performing vibration grinding, and mixing for the second time, wherein the grinding time is 80min, and the particle diameter is 0.58um
4) And (3) granulation: drying the ground slurry and then granulating;
5) molding: pressing the granulated particles into blanks T12.7 x 8 x 7;
6) and (3) sintering: and sintering the blank in a kiln by adopting balanced oxygen partial pressure, wherein the sintering temperature is 1240 ℃, the heat preservation time is 4 hours, the heat preservation oxygen content in the first 1 hour is 4 percent, the heat preservation oxygen content in the later 3 hours is 3.0 percent, and the blank is subjected to heat preservation at 1060 ℃ for 60min in a cooling section, and the oxygen content is 0.6 percent.
Comparative example 2
Comparative example 4, Fe as the main component2O3:55.6mol%,ZnO:2.8mol% ,Co2O3: 0.20wt% of MnO in balance, and Nb as an accessory component2O5:0.04wt%、CaCO3:0.0.03wt%、NiO:0.06wt%,V2O5:0.03wt%、SiO2:0.01wt%、Ta2O5:0.02wt%、TiO20.05wt%, the above-mentioned secondary components being Fe2O3ZnO, MnO and Co2O3The total weight percent of (a) was calculated and tested according to the following procedure.
1) Preparing materials: according to the main formula Fe2O3、ZnO、Co2O3Weighing the MnO in proportion, mixing and sanding for 15 min;
2) pre-burning: presintering the mixed powder, wherein the presintering temperature is 1050 ℃, and keeping the temperature for 2 hours;
3) sanding: adding the additive into the pre-sintered material, performing vibration grinding, and then performing secondary mixing treatment, wherein the sand grinding time is 100min, and the particle size is 0.55 um;
4) and (3) granulation: drying the ground slurry and then granulating;
5) molding: pressing the granulated particles into blanks T12.7 x 8 x 7;
6) and (3) sintering: and sintering the blank in a kiln at the sintering temperature of 1200 ℃, keeping the temperature for 4 hours, wherein the oxygen content is 3.8 percent, and the oxygen content at the cooling section of 1100 ℃ is 0.5 percent.
The results of the performance testing of the standard rings prepared in the above four examples and two comparative examples are as follows:
Figure 632244DEST_PATH_IMAGE001
the manganese-zinc ferrite material provided by the invention can improve the working frequency of the transformer, meets the miniaturization requirement, has ultrahigh saturation magnetic flux density, and meets the requirement of high power density.
The foregoing is a preferred embodiment of the present invention, and it should be noted that it is obvious to those skilled in the art that modifications can be made without departing from the preparation method of the present invention, and these modifications are also considered to be within the protection scope of the present invention.

Claims (3)

1. The manganese-zinc ferrite material with ultrahigh saturation magnetic flux density comprises a main component and an auxiliary component, and is characterized in that: the main component is calculated by oxide, and the main component is calculated by Fe2O3:55.25~56.25mol%,ZnO:2.5~3.5mol%,Co2O30.10 to 0.20mol%, and the balance being MnO; the minor component comprising Nb by weight of the major component2O5:0.01~0.06wt%、CaCO3:0.05~0.15wt%、NiO:0~0.05wt%,V2O5:0.01~0.04wt%、SiO2:0~0.01wt%、TiO2:0~0.05wt% 、Ta2O5:0~0.05wt%。
2. The preparation method of the manganese zinc ferrite material with ultrahigh saturation magnetic flux density as claimed in claim 1, characterized by comprising the following steps:
1) preparing materials: according to the main formula Fe2O3、ZnO 、Co2O3Weighing the mixture according to the proportion of MnO, mixing and sanding for 15-30 min;
2) pre-burning: pre-burning the mixed powder at 850-1050 ℃;
3) sanding: adding the additive into the pre-sintered material, performing vibration grinding and then performing secondary mixing treatment, wherein the sand grinding time is 80-140 min, and the particle size is 0.3-0.6 mu m;
4) and (3) granulation: drying the ground slurry and then granulating;
5) molding: pressing the granulated particles into blanks T12.7 x 8 x 7;
6) and (3) sintering: a two-stage heat preservation equilibrium oxygen partial pressure sintering method is adopted for the blank in a kiln, the first-stage sintering temperature is 1200-1240 ℃, the heat preservation time is 4-8 hours, wherein the oxygen content in the first 0-1 hour is 3.5-4%, and the oxygen content in the later heat preservation time is 2.0-3.0%; the temperature of the first section in the cooling section is 1050-1100 ℃, the heat preservation time is 30-100 min, and the oxygen content is 0.3-1.0%.
3. The preparation method of the manganese zinc ferrite material with the ultrahigh saturation magnetic flux density as claimed in claim 2, wherein the preparation method comprises the following steps: the sintering temperature in the step 6) is 1210-1230 ℃, the heat preservation is carried out for 4-8 hours, wherein the oxygen content in the first 0-1 hour is 3.5-4%, the oxygen content in the later heat preservation time is 2.0-3.0%, the secondary heat preservation is carried out in the temperature reduction section at 1050-1100 ℃, the heat preservation time is 30-80 min, and the oxygen content is 0.3-1.0%.
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