CN113185275A - Preparation method of ultrahigh Bs low-loss manganese-zinc ferrite material for cloud computing - Google Patents

Preparation method of ultrahigh Bs low-loss manganese-zinc ferrite material for cloud computing Download PDF

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CN113185275A
CN113185275A CN202110442165.4A CN202110442165A CN113185275A CN 113185275 A CN113185275 A CN 113185275A CN 202110442165 A CN202110442165 A CN 202110442165A CN 113185275 A CN113185275 A CN 113185275A
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sintering
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陈旭彬
刘志坚
尉晓东
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Emicore Corp
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Abstract

The application provides a preparation method of an ultrahigh Bs low-loss manganese-zinc ferrite material for cloud computing, which comprises the step of adding Fe2O3、ZnO、Mn3O4Mixing to obtain a precursor material, mixing the precursor material, water and a binder, and performing wet ball milling to obtain first slurry; carrying out spray granulation on the first slurry to obtain a first granular material; pre-sintering the first particle material to obtain a second particle material; mixing the second particle material, water, a binder and an additive, and then carrying out wet ball milling to obtain a second slurry; performing spray granulation on the second slurry to obtain a third granular material, and pressing the third granular material into an annular magnetic core green body; and carrying out sectional sintering on the annular magnetic core green body. The preparation method provided by the embodiment of the application can improveThe Mn-Zn ferrite material has saturated magnetic induction and reduced loss.

Description

Preparation method of ultrahigh Bs low-loss manganese-zinc ferrite material for cloud computing
Technical Field
The application relates to the technical field of soft magnetic ferrite, in particular to a preparation method of an ultrahigh Bs low-loss manganese-zinc ferrite material for cloud computing.
Background
With the rapid development of electronic information technology, cloud computing data centers will become larger and larger in the future, and a lot of new requirements such as space saving, energy consumption reduction and the like are also provided for servers. In order to meet new requirements of space saving, energy consumption reduction and the like of a server, electronic elements formed by the server are developed towards miniaturization and low loss. The DC-DC converter is used for the nuclear voltage of the multimedia coprocessor and is an important component of a server element. Under the condition that the working condition of the element is not changed, the magnetic ferrite material with high saturation magnetic induction intensity is beneficial to reducing the volume of the magnetic core and is beneficial to ensuring that the element is in an optimal working state under the high-temperature condition.
At present, the mainstream manganese-zinc ferrite materials are all produced by adopting an iron formula, although the characteristic requirement of high saturation magnetic induction intensity of the materials can be ensured due to the increased iron content. On one hand, as the iron content increases, the resistivity of the material decreases, and thus the loss increases; on the other hand, as the content of iron increases, closed oxygen vacancies are easily caused in the manganese zinc ferrite crystal grains in the sintering process, so that the sintering density of the product is low, and the improvement of the saturation magnetic induction intensity of the product is not facilitated.
Therefore, how to reduce the loss of the manganese-zinc ferrite material while improving the saturation magnetic induction of the manganese-zinc ferrite material is a problem to be solved at present.
Disclosure of Invention
In view of this, the application provides a preparation method of the ultrahigh Bs low-loss manganese-zinc ferrite material for cloud computing, which can improve the saturation magnetic induction intensity of the manganese-zinc ferrite material and reduce the loss.
In a first aspect, the application provides a preparation method of an ultrahigh Bs low-loss manganese zinc ferrite material for cloud computing, which comprises the following steps:
mixing: mixing Fe2O3、ZnO、Mn3O4Mixing to obtain a precursor material, wherein the precursor material comprises 62.0 mol% -66.0 mol% of Fe2O317.0 mol% -19.0 mol% of ZnO and the balance of Mn3O4(ii) a And the precursor material is mixed,Mixing water and a binder, and then performing wet ball milling to obtain first slurry;
granulation and pre-sintering: carrying out spray granulation on the first slurry to obtain a first granular material, and carrying out pre-sintering treatment on the first granular material to obtain a second granular material;
and (3) remixing: mixing the second particle material, water, a binder and an additive, and performing wet ball milling to obtain a second slurry, wherein the additive comprises the following components in percentage by mass: 0.015 to 0.04 wt% CaO, 0.008 to 0.025 wt% SiO20.02 to 0.06 wt% of V2O50.02-0.045 wt% of SnO2And 0.01 to 0.035 wt% of TiO2；
And (3) granulation and forming: performing spray granulation on the second slurry to obtain a third granular material, and pressing the third granular material into an annular magnetic core green body;
and (3) sintering: and sintering the annular magnetic core green body.
In a possible embodiment, the method comprises at least one of the following features a to c:
a. the precursor material, water and the adhesive are mixed according to the mass ratio of 100: (50-80) and (5-10) mixing;
b. the diameter of zirconium balls adopted by the first slurry in wet ball milling is 2-10 mm, and the wet ball milling time is controlled to be 45-60 min;
c. the average particle diameter of the particles in the first slurry was controlled to be 3.5 μm. + -. 0.1. mu.m.
In one possible embodiment, the bulk density of the second particulate material is 1.2 ± 0.3g/cm3。
In a possible embodiment, the method comprises at least one of the following features a to b:
a. the pre-sintering temperature is 900-980 ℃, and the heat preservation time is 2-3 h;
b. and in the temperature reduction section of the pre-sintering treatment, the oxygen content is controlled to be 21-25% by adopting an oxidizing atmosphere rapid temperature reduction mode at the temperature of 800-600 ℃.
In a possible embodiment, the method comprises at least one of the following features a to c:
a. the second granular material, water and the adhesive are mixed according to the mass ratio of 8: (2-4) mixing (1-3);
b. the diameter of zirconium balls adopted by the second slurry in wet ball milling is 1-5 mm, and the wet ball milling time is controlled to be 60-120 min;
c. the average particle diameter of the particles in the second slurry was controlled to be 1.5 μm. + -. 0.2. mu.m.
In one possible embodiment, the bulk density of the third particulate material is controlled to be 1.45. + -. 0.1g/cm3。
In a possible embodiment, the sintering is a step-by-step sintering process, specifically including:
air sintering is adopted, the temperature of the first temperature rise section is controlled to be 25-500 ℃, and the temperature rise rate is 0.5-2 ℃/min;
adopting nitrogen for sintering, controlling the temperature of the second temperature rising section to be 850-1000 ℃, controlling the oxygen concentration in the second temperature rising section to be 3-5%, and controlling the temperature rising rate to be 1-4 ℃/min;
mixing and sintering nitrogen and reducing gas, controlling the temperature of a third temperature rise section to be 1000-1150 ℃, preserving the heat at 1050 ℃ for 30-90 min, controlling the oxygen concentration in the third temperature rise section to be 0-0.5%, and controlling the temperature rise rate to be 1-4 ℃/min;
adopting nitrogen for sintering, controlling the temperature of the fourth temperature rising section to be 1150-1360 ℃, controlling the oxygen concentration in the fourth temperature rising section to be 3-5%, and controlling the temperature rising rate to be 1-4 ℃/min;
and (3) cooling under the protection of nitrogen, wherein the cooling rate is controlled to be 1-3 ℃/min, and the concentration of oxygen in the cooling section is controlled to be 500ppm less.
In one possible embodiment, the reducing gas comprises at least one of methane, ethane, ethylene, carbon monoxide, hydrogen.
In one possible embodiment, the degree of magnetization of the second particulate material after the pre-sintering treatment is 8% or less.
The technical scheme of the application has at least the following beneficial effects:
the preparation method of the ultrahigh Bs low-loss manganese-zinc ferrite material for cloud computing provided by the application comprises the steps of doping oxides in the material, and passing through CaO and SiO2With TiO2The synergistic effect of the components is beneficial to the growth of manganese-zinc ferrite grains, the sintering temperature is reduced, the thickness of a grain boundary is increased, and the resistivity of the material is improved; by adding SnO2And V2O5The crystal grains are refined, the sintering temperature is reduced, and the loss of materials can be effectively reduced; the problem of oxygen release during ferrite sintering can be solved by introducing gas for sintering in the sintering process, the sintering density of the ferrite material is obviously improved, and the volume and the loss of the magnetic core are reduced.
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For a clearer explanation of the embodiments or technical solutions of the prior art of the present application, the drawings needed for the description of the embodiments or prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is a flowchart of a preparation method of a manganese-zinc ferrite material provided in an embodiment of the present application.
Detailed Description
While the following is a description of the preferred embodiments of the present invention, it should be noted that those skilled in the art can make various modifications and improvements without departing from the principle of the embodiments of the present invention, and such modifications and improvements are considered to be within the scope of the embodiments of the present invention.
In a first aspect, an embodiment of the present application further provides a preparation method of the ultrahigh Bs low-loss manganese zinc ferrite material for cloud computing, as shown in fig. 1, including the following steps:
step S10, mixing Fe2O3、ZnO、Mn3O4Mixing to obtain a precursor material, wherein the precursor material comprises 62.0 mol% >, E66.0 mol% Fe2O317.0 mol% -19.0 mol% of ZnO and the balance of Mn3O4(ii) a Mixing the precursor material, water and a binder, and then carrying out wet ball milling to obtain first slurry;
step S20, performing spray granulation on the first slurry to obtain a first granular material;
step S30, pre-sintering the first particle material to obtain a second particle material;
step S40, mixing the second particulate material, water, a binder, and an additive, and performing wet ball milling to obtain a second slurry, wherein the additive comprises, by mass: 0.015 to 0.04 wt% CaO, 0.008 to 0.025 wt% SiO20.02 to 0.06 wt% of V2O50.02-0.045 wt% of SnO2And 0.01 to 0.035 wt% of TiO2；
Step S50, performing spray granulation on the second slurry to obtain a third granular material, and pressing the third granular material into an annular magnetic core green body;
and step S60, sintering the green annular magnetic core in a sectional mode.
In the scheme, the material is doped with oxide through CaO and SiO2With TiO2The synergistic effect of the components is beneficial to the growth of manganese-zinc ferrite grains, the sintering temperature is reduced, the thickness of a grain boundary is increased, and the resistivity of the material is improved; by adding SnO2And V2O5The crystal grains are refined, the sintering temperature is reduced, and the loss of materials can be effectively reduced; the problem of oxygen release during ferrite sintering can be solved by introducing gas for sintering in a sectional sintering process, the sintering density of the ferrite material is obviously improved, and the volume and the loss of the magnetic core are reduced.
The preparation method of the manganese-zinc ferrite material of the present application is explained in detail as follows:
step S10, mixing Fe2O3、ZnO、Mn3O4Mixing to obtain a precursor material, wherein the precursor material comprises 62.0 mol% -66.0 mol% of Fe2O317.0 mol% -19.0 mol% of ZnO and the balance of Mn3O4(ii) a And mixing the precursor material, water and the adhesive, and then carrying out wet ball milling to obtain first slurry.
In a specific embodiment, before step S10, the method further includes:
carrying out a compounding process, wherein the components are measured in mole fractions, and the Fe2O3The content of (A) is 62.0 mol% -66.0 mol%, the content of ZnO is 17.0 mol% -19.0 mol%, and the balance is Mn3O4。
Illustratively, mixing Fe in the slurry2O3The molar percentage of (b) may be, for example, 62.0 mol%, 62.5 mol%, 63.0 mol%, 63.5 mol%, 64.0 mol%, 64.5 mol%, 65.0 mol%, 65.5 mol%, or 66.0 mol%, etc., but is not limited to the recited values, and other values not recited in the numerical range are also applicable. Understandably, the saturation magnetic induction intensity of the material can be effectively improved by increasing the iron content in the material by a proper amount.
Illustratively, the molar percentage of ZnO in the mixed slurry may be, for example, 17.0 mol%, 17.3 mol%, 17.5 mol%, 17.8 mol%, 18.0 mol%, 18.3 mol%, 18.5 mol%, 18.8 mol%, or 19.0 mol%, etc., but is not limited to the recited values, and other values not recited in the range are also applicable.
After charging Fe2O3、Mn3O4In the process of ZnO, half of Fe can be added firstly2O3After that, Mn is added3O4ZnO, and finally adding the other half of Fe2O3This can make the above three materials mixed more uniformly.
Specifically, the precursor material, water and the binder are mixed according to a mass ratio of 100: (50-80): (5-10), and wet ball milling and/or sanding can be used to mix the materials uniformly. Illustratively, the precursor material, the water and the binder are mixed according to a mass ratio of 100: 50: 5. 100, and (2) a step of: 60: 8. 100, and (2) a step of: 70: 8. 100, and (2) a step of: 80: 10, etc., without limitation thereto.
As an optional technical scheme of the application, a proper amount of purified water and a proper amount of a binder can be added into the precursor material, the diameter of zirconium balls adopted in wet ball milling is 2-10 mm, and the wet ball milling time is controlled to be 45-60 min. Specifically, the diameter of the zirconium balls may be 2mm, 2.5mm, 2.8mm, 3mm, 3.5mm, 4mm, 5mm, 10mm, or the like, but is not limited to the recited values, and other values not recited in the numerical range are also applicable.
The wet ball milling time may be 45min, 48min, 50min, 52min, 55min or 60min, but is not limited to the listed values, and other values not listed in the range of the values are also applicable. In the ball milling time range, the particle size of the metal oxide powder can be smaller, and the uniformity of the mixed powder is improved.
As an optional technical solution of the present application, the average particle size of the particles in the first slurry after wet ball milling is controlled to be 3.5 μm ± 0.1 μm, specifically, 3.4 μm, 3.5 μm, 3.6 μm, and the like.
Step S20, performing spray granulation on the first slurry to obtain a first granular material.
It is understood that the first slurry is subjected to spray granulation to form spherical granular material, and the spherical granular material is beneficial to improving the sintering uniformity of the material.
Step S30, performing pre-sintering treatment on the first particle material to obtain a second particle material.
Specifically, the pre-sintering treatment comprises a temperature rising stage and a temperature reducing stage.
In the temperature raising stage, the pre-sintering temperature is controlled to be 900-980 ℃, and can be 900 ℃, 920 ℃, 950 ℃, 960 ℃ or 980 ℃. The holding time is controlled to be 2 to 3 hours, for example, 2 hours, 2.2 hours, 2.5 hours, 2.8 hours or 3 hours, but the holding time is not limited to the listed values, and other values not listed in the numerical range are also applicable. In this example, the pre-sintering was performed under air.
In the cooling stage, the temperature is controlled to be 800-600 ℃, and the oxygen content is controlled to be 21-25% in a rapid cooling mode in an oxidizing atmosphere.
Understandably, the metal oxide powder can be subjected to preliminary solid-phase reaction through pre-sintering treatment, and partial ferrite is performed, wherein the valence change of Mn and Fe can be ensured by adopting oxidizing atmosphere sintering at 800-600 ℃, so that the material can fully absorb oxygen, the degree of magnetization of the pre-sintered second particle material is controlled to be less than or equal to 8%, and the purpose of controlling the material shrinkage is achieved.
As an alternative solution, the bulk density of the second particulate material is 1.2. + -. 0.3g/cm3。
Step S40, mixing the second particulate material, water, a binder, and an additive, and performing wet ball milling to obtain a second slurry, wherein the additive comprises, by mass: 0.015 to 0.04 wt% CaO, 0.008 to 0.025 wt% SiO20.02 to 0.06 wt% of V2O50.02-0.045 wt% of SnO2And 0.01 to 0.035 wt% of TiO2。
In the process of preparing the second slurry, the second granular material, water and the binder are mixed according to the mass ratio of 8: (2-4) mixing (1-3), specifically, the mass ratio of the second particulate material, water and the binder may be 8:2:1, 8:3:2, 8:2:3, 8:4:3, etc., but not limited to the listed values, and other values not listed in the range of the values are also applicable.
The diameter of zirconium balls adopted by the second slurry in wet ball milling is 1-5 mm, and the wet ball milling time is controlled to be 60-120 min; specifically, the diameter of the zirconium balls may be 1mm, 2.5mm, 2.8mm, 3mm, 3.5mm, 4mm, 5mm, or the like, but is not limited to the listed values, and other values not listed in the numerical range are also applicable.
The wet ball milling time may be 60min, 70min, 80min, 90min, 100min or 120min, but is not limited to the listed values, and other values not listed in the range of the values are also applicable. In the ball milling time range, the particle sizes of the doped oxide and the second particle material in the slurry are smaller, so that the doped oxide has larger specific surface area and stronger adhesive force, the main material and the doped oxide are mixed more uniformly, and the slurry is finer and smoother.
In a specific embodiment, the average particle size of the particles in the second slurry is controlled to be 1.5 μm ± 0.2 μm, and may be, for example, 1.3 μm, 1.35 μm, 1.4 μm, 1.5 μm, 1.6 μm, or 1.7 μm, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable. In the present embodiment, the particle size of the particles can be adjusted by increasing the grinding time, and in general, the longer the grinding time, the smaller the particle size.
Further, the second slurry can be screened to remove large particles in the second slurry, so that the slurry is more uniform and fine.
In this embodiment, the binder includes at least one of polyvinyl alcohol, paraffin wax, and methyl cellulose.
And step S50, performing spray granulation on the second slurry to obtain a third granular material, and pressing the third granular material into an annular magnetic core green body.
Specifically, the sieved second slurry may be poured into a spray granulation apparatus to obtain a third granular material, i.e., a manganese-zinc ferrite material after the doped oxide is compounded. Specifically, the apparent density of the third particulate material is controlled to 1.45. + -. 0.1g/cm3。
And pouring the material into a pressing grinding tool, and pressing to obtain an annular magnetic core green body. In this example, the green toroidal core had dimensions of 25mm 15mm 8mm and the density of the green core was 3.0 ± 0.05g/cm3。
Further, the green annular magnetic core is subjected to segmented sintering, and the segmented sintering comprises the following steps:
air sintering is adopted, the temperature of the first temperature rise section is controlled to be 25-500 ℃, and the temperature rise rate is 0.5-2 ℃/min;
adopting nitrogen for sintering, controlling the temperature of the second temperature rising section to be 850-1000 ℃, controlling the oxygen concentration in the second temperature rising section to be 3-5%, and controlling the temperature rising rate to be 1-4 ℃/min;
mixing and sintering nitrogen and reducing gas, controlling the temperature of a third temperature rise section to be 1000-1150 ℃, preserving the heat at 1050 ℃ for 30-90 min, controlling the oxygen concentration in the third temperature rise section to be 0-0.5%, and controlling the temperature rise rate to be 1-4 ℃/min;
adopting nitrogen for sintering, controlling the temperature of the fourth temperature rising section to be 1150-1360 ℃, controlling the oxygen concentration in the fourth temperature rising section to be 3-5%, and controlling the temperature rising rate to be 1-4 ℃/min;
and (3) cooling under the protection of nitrogen, wherein the cooling rate is 1-3 ℃/min, and the concentration of oxygen in the cooling section is controlled to be 500ppm less.
Specifically, in the first temperature-raising section, the temperature may be 25 ℃, 50 ℃, 100 ℃, 150 ℃, 200 ℃, 300 ℃, 400 ℃, 500 ℃ or the like. The temperature rise rate may be, for example, 0.5 ℃/min, 1.0 ℃/min, 1.5 ℃/min, 1.8 ℃/min, 2.0 ℃/min, or the like, but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
In the second temperature raising section, the temperature may be 850 ℃, 880 ℃, 900 ℃, 920 ℃, 950 ℃, 980 ℃, 1000 ℃ or the like. The oxygen concentration in the second temperature rise section may be, in particular, 3%, 3.5%, 4%, 4.5% or 5%, etc., but is not limited to the recited values, and other values not recited in the range of values are equally applicable. It should be noted that only nitrogen gas is introduced into the sintering furnace in the first temperature rising section. The temperature rise rate of the second temperature rise section may be 1.0 ℃/min, 2 ℃/min, 2.5 ℃/min, 3 ℃/min or 4 ℃/min, but is not limited to the listed values, and other values not listed in the numerical range are also applicable.
In the third temperature raising section, the temperature may be 1000 ℃, 1050 ℃, 1080 ℃, 1100 ℃, 1150 ℃ or the like. The oxygen concentration in the third temperature rise section may specifically be 0%, 0.1%, or 0.3%, and so on; the temperature rise rate of the third temperature rise section may be 1.0 ℃/min, 2 ℃/min, 2.5 ℃/min, 3 ℃/min or 4 ℃/min, but is not limited to the listed values, and other values not listed in the numerical range are also applicable.
In the third temperature rising section, a mixed gas composed of nitrogen and reducing gas is introduced into the sintering furnace.
In this embodiment, in the third temperature rising section, the volume ratio of the nitrogen gas is 98.5% to 99%, and the volume ratio of the reducing gas is 1% to 1.5%. It is understood that by adding a small amount of reducing gas to the nitrogen gas, the reducing gas easily reacts with oxygen evolved from the valence change of iron, consuming the oxygen, thereby accelerating the valence change rate of iron.
It is understood that the reaction formula of iron during the temperature rise is as follows: fe3++1/2O2-→Fe2++1/4O2If the oxygen can not be discharged in time, closed oxygen vacancies are easily caused in the manganese-zinc ferrite crystal grains, ferrous ions obtained by valence change of iron are reduced, the porosity of the final magnetic core material is increased, and the sintering density of the product is reduced. The decrease in product density in turn can also affect the saturation induction of the product.
In this embodiment, the reducing gas includes at least one of methane, ethane, ethylene, carbon monoxide, and hydrogen.
More specifically, in the third stage, the temperature is raised from 1000 ℃ to 1050 ℃, the temperature is kept for 30-90 min, the oxygen concentration reaches 0.3%, the temperature is raised from 1050 ℃ to 1150 ℃, and the oxygen concentration is controlled to gradually rise to 0.5%.
In the fourth temperature rising section, nitrogen is adopted for sintering, the temperature of the fourth temperature rising section is controlled to be 1150-1360 ℃, and the oxygen concentration in the third temperature rising section is controlled to be 3-5%. The temperature may be 1150 deg.C, 1180 deg.C, 1200 deg.C, 1250 deg.C, 1300 deg.C or 1360 deg.C. The oxygen concentration in the fourth temperature rise section may be, in particular, 3%, 3.5%, 4%, 4.5%, 5%, etc., but is not limited to the recited values, and other values not recited in the range of values are equally applicable. In the fourth temperature rising section, only nitrogen is introduced into the sintering furnace.
After reaching 1360 ℃, preserving the heat for 4 to 6 hours, and then entering a cooling stage.
Further, the temperature is reduced under the protection of nitrogen, the temperature reduction rate is controlled to be 1-3 ℃/min, and the oxygen concentration in the temperature reduction section is controlled to be 500ppm less.
In this scheme, mix into a small amount of reducing gas in through toward nitrogen gas, can accelerate the oxygen extraction, reduce the oxygen content in the sintering furnace, can also further accelerate sintering rate, not only through reducing the rate of rise in temperature, realize as much as possible oxygen extraction, but through the initiative oxygen that consumes, can accelerate sintering treatment time, reduce the sintering cost, promote sintering rate.
The embodiment of the application also provides a manganese-zinc ferrite material comprising Fe2O3、ZnO、Mn3O4And a doped oxide, wherein the components are in mole fraction, the Fe2O3The content of (A) is 62.0 mol% -66.0 mol%, the content of ZnO is 17.0 mol% -19.0 mol%, and the balance is Mn3O4And a doped oxide, wherein the doped oxide comprises CaO, SiO2、V2O5、SnO2And TiO2。
In the scheme, the characteristic requirement of high saturation magnetic induction intensity of the material is ensured by improving the iron content in the manganese-zinc ferrite material; further doping the material with oxide through CaO and SiO2With TiO2The synergistic effect of the manganese-zinc ferrite is beneficial to the growth of manganese-zinc ferrite grains, the refinement of the grains, the increase of the thickness of a grain boundary and the improvement of the resistivity of the material; by adding SnO2And V2O5And the loss of the material can be effectively reduced.
The following examples are intended to illustrate the invention in more detail. The embodiments of the present invention are not limited to the following specific embodiments. The present invention can be modified and implemented as appropriate within the scope of the main claim.
Example 1
Preparing materials: fe2O3The content of (B) is 62.5 mol%, the content of ZnO is 18.5 mol%, and the balance is Mn3O4And (4) carrying out the batching of the main components. The doped oxide comprises 150-400 ppm of CaO and 80-250 ppm of SiO in percentage by mass2200 to 600ppm of V2O5200-450 ppm SnO2100 to 350ppm of TiO2And (5) carrying out additive compounding.
Feeding and mixing: in the feeding process, half of Fe is fed firstly2O3After charging ZnO and Mn3O4Then another half of Fe is added2O3Uniformly mixing the materials, and wet grinding and sanding to obtain first slurry; and carrying out spray granulation on the first slurry to obtain a spherical first granular material.
And (3) sintering the first particle material in a sectional type atmosphere, controlling the pre-sintering temperature to be 900-980 ℃, preserving heat for 2 hours, and controlling the oxygen content to be 21-25% in a sintering manner in an oxidizing atmosphere at 800-600 ℃ in a cooling section, so that the material can fully absorb oxygen to obtain a second particle material.
And mixing the second particle material with water according to the weight ratio of 3:2, placing the mixture into a sand mill for secondary sand milling, adding the doped oxide, controlling the sand milling particle size D50 to be 1.5 +/-0.1 mu m, and performing sand milling for about 120min to obtain second slurry.
Adding a defoaming agent into the second slurry, starting stirring, then adding a binder polyvinyl alcohol, continuing stirring, carrying out spray granulation, and further carrying out compression molding on granules obtained by granulation to obtain an annular magnetic core green compact with the density of 3.0 +/-0.05 g/cm3。
Sintering by adopting sectional mixed gas and nitrogen, sintering by adopting air at 25-500 ℃, and controlling the heating rate to be 0.5-2 ℃/min; then, sintering by adopting nitrogen at 850-1000 ℃, controlling the oxygen content at 3-5% and the heating rate at 2-4 ℃/min; carrying out sectional type inflation at 1000-1150 ℃, adopting nitrogen and methane gas to mix and sinter (98.5% of nitrogen and 1.5% of methane), and keeping the temperature at 1050 ℃ for 90min, controlling the oxygen content to be 0.3%, heating to 1150 ℃, and controlling the heating rate to be 2-4 ℃/min; controlling the oxygen content to be 0.5 percent, controlling the oxygen content to be about 3 percent after 1200 ℃, continuously heating to 1360 ℃ and keeping the temperature for 4-6 hours, and controlling the heating rate to be 1-4 ℃/min. And (3) filling nitrogen at 1080 ℃ in a cooling section, keeping the temperature for 60min, and controlling the oxygen content to be below 500ppm until the sample is placed in a kiln to obtain a sample S1.
Example 2
Sample S2, prepared according to the preparation method of example 1, differs from example 1 in Fe when compounded2O3The content of (B) is 65 mol%, the content of ZnO is 17.5 mol%, and the balance is Mn3O4And doping oxidationA compound (I) is provided.
Example 3
Sample S3, prepared according to the preparation method of example 1, differs from example 1 in Fe when compounded2O3The content of (B) is 66 mol%, the content of ZnO is 17.0 mol%, and the balance is Mn3O4And a doped oxide.
Example 4
Sample S4, prepared according to the preparation method of example 1, differs from example 1 in Fe when compounded2O3The content of (A) is 63 mol%, the content of ZnO is 18.0 mol%, and the balance is Mn3O4And a doped oxide.
Comparative example 1
Sample D1 was prepared according to the preparation method of example 1, except that in the compounding of example 1, no doped oxide was added, and the compounding included Fe2O3Has a content of 62.5 mol%, a content of ZnO of 18.5 mol%, and the balance of Mn3O4。
Comparative example 2
Sample D2 was prepared according to the preparation method of example 1, except that: the spherical particle material was not pre-sintered.
Comparative example 3
Sample D2 was prepared according to the preparation method of example 1, except that: in the sintering stage, a mixed gas of nitrogen and a reducing gas is not used.
And (3) testing:
magnetic properties of the manganese-zinc-ferrite material samples (S1 to S4) prepared in examples 1 to 4 and the manganese-zinc-ferrite material samples (D1 to D3) prepared in comparative examples 1 to 3 were measured, respectively, and the results are shown in table 1 below:
TABLE 1 magnetic Property parameters of Mn-Zn ferrite Material
Figure BDA0003035551290000121
From the test data in the table above, it can be seen that the manganese-zinc-ferrite material of comparative example 1 has no doped oxide and the power consumption of the material is significantly improved compared to example 1.
The manganese-zinc-ferrite material of comparative example 2 compared to example 1, without pre-sintering the spherical particle material, did not meet the design requirements for material Bs and did not reach a density of 4.9g/cm3。
The manganese-zinc-ferrite material of comparative example 3 compared to example 1, did not use a mixed gas of nitrogen and a reducing gas in the sintering stage, and the final product had a density of 4.75g/cm3And the material Bs and the magnetic permeability do not reach the design requirements.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims (9)

1. A preparation method of an ultrahigh Bs low-loss manganese zinc ferrite material for cloud computing is characterized by comprising the following steps:
mixing Fe2O3、ZnO、Mn3O4Mixing to obtain a precursor material, wherein the precursor material comprises 62.0 mol% -66.0 mol% of Fe2O317.0 mol% -19.0 mol% of ZnO and the balance of Mn3O4(ii) a Mixing the precursor material, water and a binder, and then carrying out wet ball milling to obtain first slurry;
carrying out spray granulation on the first slurry to obtain a first granular material;
pre-sintering the first particle material to obtain a second particle material;
mixing the second particle material, water, a binder and an additive, and performing wet ball milling to obtain a second slurry, wherein the additive comprises the following components in percentage by mass: 0.015 to 0.04 wt% CaO, 0.008 to 0.025 wt% SiO20.02 to 0.06 wt% of V2O50.02-0.045 wt% of SnO2And 0.01 to 0.035wt% of TiO2；
Performing spray granulation on the second slurry to obtain a third granular material, and pressing the third granular material into an annular magnetic core green body;
and carrying out sectional sintering on the green annular magnetic core.
2. The method for preparing according to claim 1, characterized in that the method comprises at least one of the following features a to c:
a. the precursor material, water and the adhesive are mixed according to the mass ratio of 100: (50-80) and (5-10) mixing;
b. the diameter of zirconium balls adopted by the first slurry in wet ball milling is 2-10 mm, and the wet ball milling time is controlled to be 45-60 min;
c. the average particle diameter of the particles in the first slurry was controlled to be 3.5 μm. + -. 0.1. mu.m.
3. The method of claim 1, wherein the second particulate material has a bulk density of 1.2 ± 0.3g/cm3。
4. The method of manufacturing according to claim 1, characterized in that the method comprises at least one of the following features a to b:
a. the pre-sintering temperature is 900-980 ℃, and the heat preservation time is 2-3 h;
b. and in the temperature reduction section of the pre-sintering treatment, the oxygen content is controlled to be 21-25% by adopting an oxidizing atmosphere rapid temperature reduction mode at the temperature of 800-600 ℃.
5. The method of manufacturing according to claim 1 or 2, characterized in that the method comprises at least one of the following features a to c:
a. the second granular material, water and the adhesive are mixed according to the mass ratio of 8: (2-4) mixing (1-3);
b. the diameter of zirconium balls adopted by the second slurry in wet ball milling is 1-5 mm, and the wet ball milling time is controlled to be 60-120 min;
c. the average particle diameter of the particles in the second slurry was controlled to be 1.5 μm. + -. 0.2. mu.m.
6. The method according to claim 1, wherein the loose packed density of the third particulate material is controlled to be 1.45 ± 0.1g/cm3。
7. The method according to claim 1, wherein the step sintering comprises:
air sintering is adopted, the temperature of the first temperature rise section is controlled to be 25-500 ℃, and the temperature rise rate is 0.5-2 ℃/min;
adopting nitrogen for sintering, controlling the temperature of the second temperature rising section to be 850-1000 ℃, controlling the oxygen concentration in the second temperature rising section to be 3-5%, and controlling the temperature rising rate to be 1-4 ℃/min;
mixing and sintering nitrogen and reducing gas, controlling the temperature of a third temperature rise section to be 1000-1150 ℃, preserving the heat at 1050 ℃ for 30-90 min, controlling the oxygen concentration in the third temperature rise section to be 0-0.5%, and controlling the temperature rise rate to be 1-4 ℃/min;
adopting nitrogen for sintering, controlling the temperature of the fourth temperature rising section to be 1150-1360 ℃, controlling the oxygen concentration in the fourth temperature rising section to be 3-5%, and controlling the temperature rising rate to be 1-4 ℃/min;
and (3) cooling under the protection of nitrogen, wherein the cooling rate is controlled to be 1-3 ℃/min, and the concentration of oxygen in the cooling section is controlled to be 500ppm less.
8. The method according to claim 7, wherein the reducing gas includes at least one of methane, ethane, ethylene, carbon monoxide, and hydrogen.
9. The method according to claim 1, wherein the degree of magnetization of the pre-sintered second particulate material is 8% or less.
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