CN112125655A - Preparation method of high-temperature high-frequency low-loss ferrite material - Google Patents
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Abstract
The invention relates to the technical field of ferrite materials, and discloses a preparation method of a ferrite material with high temperature, high frequency and low loss, which comprises the following preparation steps: 1) mixing and grinding 52-58 mol% of ferric oxide, 9-13 mol% of zinc oxide, 0.5-5 mol% of nickel oxide and 31-38 mol% of manganese carbonate to form grinding powder; 2) presintering the ground powder at 950-1050 ℃ to form fired powder; 3) adding tin dioxide, titanium dioxide and vanadium pentoxide into the fired powder according to the mass ratio, and grinding the primary powder with the particle size reaching submicron level again; 4) adding an organic adhesive into the primary powder, and forming into a granular blank; 5) placing the granular blank in a sintering furnace for high-temperature sintering for several hours to form a high-temperature high-frequency low-loss ferrite material; the purpose of reducing power loss under the high-temperature and high-frequency conditions is achieved.
Description
Technical Field
The invention relates to the technical field of ferrite materials, in particular to a preparation method of a ferrite material with high temperature, high frequency and low loss.
Background
The ferrite material is composed of a MnNiZn ferrite material containing a predetermined amount of a main component of iron oxide, manganese oxide, zinc oxide, and nickel oxide, and further containing a predetermined amount of bismuth oxide, magnesium oxide, and cobalt oxide, and therefore, the ferrite material can provide a high-strength MnNiZn ferrite material having extremely good temperature characteristics (a small rate of change in permeability with respect to a change in temperature), a high quality factor Q, and a high strength.
At present, the preparation process of ferrite materials needs to sequentially carry out the following steps of formula, primary ball milling, presintering, doping, secondary ball milling, granulation molding, sintering and the like. The purpose of the processes is to increase the grain boundary resistivity of the ferrite material, reduce the eddy current loss under high frequency and achieve the purpose of reducing the loss under the high frequency condition.
In the prior art, the preparation methods of the ferrite materials disclosed above are difficult to achieve the purpose of low power loss under high temperature and high frequency conditions.
Disclosure of Invention
The invention aims to provide a preparation method of a ferrite material with high temperature, high frequency and low loss, and aims to solve the problem that the preparation method of the ferrite material in the prior art is difficult to achieve low power loss under the condition of high temperature and high frequency.
The invention discloses a preparation method of a ferrite material with high temperature, high frequency and low loss, which comprises the following preparation steps:
1) uniformly mixing and grinding 52-58 mol% of ferric oxide, 9-13 mol% of zinc oxide, 0.5-5 mol% of nickel oxide and 31-38 mol% of manganese carbonate to form grinding powder;
2) pre-burning the ground powder obtained in the step 1) at the temperature of 950-1050 ℃ to form fired powder;
3) adding the following additives into the fired powder obtained in the step 2) according to the mass ratio: tin dioxide, titanium dioxide and vanadium pentoxide, and grinding again to enable the particle size of the ground powder to reach submicron primary powder;
4) adding an organic binder into the primary powder obtained in the step 3), and granulating and molding the primary powder into a granular blank;
5) and placing the granular blank obtained in the step 4) in a sintering furnace for high-temperature sintering for a plurality of hours to form the high-temperature high-frequency low-loss ferrite material.
Further, in the step 1), the grinding powder is prepared by adopting a ball milling mode.
Further, in the step 5), during sintering of the granular green material, the inside of the sintering furnace is in a weakly oxidized state.
Further, in the step 5), the oxygen partial pressure inside the sintering furnace is in a weak oxidation state of 1.5% to 5% in the process of sintering the granular green material.
Further, in the step 5), during sintering the granular blank, the sintering temperature inside the sintering furnace is 1320 ℃.
Further, in the step 5), the sintering time of the granular blank in the sintering furnace is 2-4 h.
Further, in the step 2), the pre-sintering time of the grinding powder is 1.5 to 2.5 hours.
Further, in the step 4), the mass ratio of the organic binder added into the primary powder is 7 wt% -8 wt%.
Further, in the step 3), the fired powder added with the additive is subjected to ball milling.
Further, in the step 3), the mass ratio of the additive added to the fired powder material is 0.02-0.3 wt% of tin dioxide, 0.02-0.3 wt% of titanium dioxide, and 0.02-0.3 wt% of vanadium pentoxide.
Compared with the prior art, the preparation method of the high-temperature high-frequency low-loss ferrite material provided by the invention has the advantages that a proper formula is adopted to grind the material into grinding powder, the additive is added into the pre-sintered sintering powder and ground into primary powder, the organic binder is added into the primary powder to form granular blank, the granular blank is sintered, the grain boundary resistivity of the material is increased, the eddy current loss under the high-frequency condition is reduced, and the temperature point of the two peaks of the characteristic curve is adjusted, so that the purpose of reducing the power loss under the high-temperature high-frequency condition is achieved. The power loss is the lowest at a higher working temperature of more than 120-180 ℃, and each technical index is good. The power loss is low in the frequency range of 100-1000K Hz.
Drawings
FIG. 1 is a P-T test curve of the high-temperature, high-frequency and low-loss ferrite material provided by the present invention;
FIG. 2 is a Q-F test curve of the high-temperature, high-frequency and low-loss ferrite material provided by the present invention (curve a) and the conventional ferrite material (curves b and c).
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The following describes the implementation of the present invention in detail with reference to specific embodiments.
The same or similar reference numerals in the drawings of the present embodiment correspond to the same or similar components; in the description of the present invention, it should be understood that if there is an orientation or positional relationship indicated by the terms "upper", "lower", "left", "right", etc. based on the orientation or positional relationship shown in the drawings, it is only for convenience of describing the present invention and simplifying the description, but it is not intended to indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and therefore, the terms describing the positional relationship in the drawings are only used for illustrative purposes and are not to be construed as limiting the present patent, and the specific meaning of the terms may be understood by those skilled in the art according to specific circumstances.
Referring to fig. 1-2, a preferred embodiment of the present invention is shown.
The preparation method of the ferrite material with high temperature, high frequency and low loss comprises the following preparation steps:
1) uniformly mixing and grinding 52-58 mol% of ferric oxide, 9-13 mol% of zinc oxide, 0.5-5 mol% of nickel oxide and 31-38 mol% of manganese carbonate to form grinding powder;
2) pre-burning the ground powder obtained in the step 1) at the temperature of 950-1050 ℃ to form fired powder;
3) adding the following additives into the fired powder obtained in the step 2) according to the mass ratio: tin dioxide, titanium dioxide and vanadium pentoxide, and grinding again to enable the particle size of the ground powder to reach submicron primary powder;
4) adding an organic binder into the primary powder obtained in the step 3), and granulating and molding the primary powder into a granular blank;
5) and placing the granular blank obtained in the step 4) in a sintering furnace for high-temperature sintering for a plurality of hours to form the high-temperature high-frequency low-loss ferrite material.
According to the preparation method of the high-temperature high-frequency low-loss ferrite material, a proper formula is adopted to grind the ferrite material into grinding powder, an additive is added into the sintering powder formed by pre-sintering and ground to form primary powder, an organic binder is added into the primary powder to form granular blank, the granular blank is sintered, the grain boundary resistivity of the material is increased, the eddy current loss under the high-frequency condition is reduced, and the temperature point of the two peaks of the characteristic curve is adjusted, so that the purpose of reducing the power loss under the high-temperature high-frequency condition is achieved.
By fine-tuning the formula and sintering process, series ferrite materials can be prepared, and the ferrite materials with proper performance characteristics are selected according to different use conditions
The power loss is the lowest at a higher working temperature of more than 120-180 ℃, and each technical index is good. The power loss is low in the frequency range of 100-1000K Hz.
In the step 1), grinding powder is prepared by adopting a ball milling mode.
In step 5), during sintering of the granular green material, the inside of the sintering furnace is in a weakly oxidized state.
In step 5), the oxygen partial pressure inside the sintering furnace is in a weak oxidation state of 1.5% to 5% during sintering of the granular green material.
In step 5), the sintering temperature inside the sintering furnace was 1320 ℃ during sintering of the granulated green material.
In the step 5), the sintering time of the granular blank in the sintering furnace is 2-4 h.
In the step 2), the pre-sintering time of the grinding powder is 1.5-2.5 h.
In the step 4), the mass ratio of the organic binder added into the primary powder is 7-8 wt%.
In the step 3), the fired powder added with the additive is subjected to ball milling.
In the step 3), the mass ratio of the additive added into the fired powder is 0.02-0.3 wt% of tin dioxide, 0.02-0.3 wt% of titanium dioxide and 0.02-0.3 wt% of vanadium pentoxide.
The following provides a preferred embodiment.
The preparation method of the ferrite material with high temperature, high frequency and low loss comprises the following preparation steps:
step 1), adopting 54.2 mol% ferric oxide, 11.5 mol% zinc oxide, 1.5 mol% nickel oxide and 32.8 mol% manganese carbonate as a formula, and ball-milling and mixing uniformly to form grinding powder;
step 2), pre-burning the formed grinding powder prepared in the step 1) for 2 hours at the temperature of 980 ℃ to form fired powder;
step 3), adding the following additives into the fired powder obtained in the step 2) according to the mass ratio: 0.05 weight percent of stannic oxide, 0.05 weight percent of titanium dioxide and 0.05 weight percent of vanadium pentoxide, and performing ball milling again to ensure that the particle size of the ball-milled powder reaches submicron primary powder;
step 4), granulating and forming, namely adding 7 wt% of organic binder into the primary powder obtained in the step 3, uniformly mixing and granulating the mixture to form the powder according to the required shape and size;
and 5) sintering, namely placing the granular blank obtained in the step 4 into a sintering furnace, and sintering for 3 hours at 1320 ℃ in a weak oxidizing atmosphere with the oxygen partial pressure of 2%.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. The preparation method of the ferrite material with high temperature, high frequency and low loss is characterized by comprising the following preparation steps:
1) uniformly mixing and grinding 52-58 mol% of ferric oxide, 9-13 mol% of zinc oxide, 0.5-5 mol% of nickel oxide and 31-38 mol% of manganese carbonate to form grinding powder;
2) pre-burning the ground powder obtained in the step 1) at the temperature of 950-1050 ℃ to form fired powder;
3) adding the following additives into the fired powder obtained in the step 2) according to the mass ratio: tin dioxide, titanium dioxide and vanadium pentoxide, and grinding again to enable the particle size of the ground powder to reach submicron primary powder;
4) adding an organic binder into the primary powder obtained in the step 3), and granulating and molding the primary powder into a granular blank;
5) and placing the granular blank obtained in the step 4) in a sintering furnace for high-temperature sintering for a plurality of hours to form the high-temperature high-frequency low-loss ferrite material.
2. The method for preparing a high-temperature high-frequency low-loss ferrite material according to claim 1, wherein in the step 1), the grinding powder is prepared by a ball milling method.
3. A method for preparing a high temperature, high frequency and low loss ferrite material as claimed in claim 1 or 2, wherein in said step 5), during sintering of the granular blank, the inside of said sintering furnace is in a weak oxidation state.
4. A method for preparing a high-temperature high-frequency low-loss ferrite material as claimed in claim 1 or 2, wherein in said step 5), during the process of sintering the granular blank, the oxygen partial pressure inside said sintering furnace is in a weak oxidation state of 1.5-5%.
5. A method for preparing a high-temperature high-frequency low-loss ferrite material as claimed in claim 1 or 2, wherein in the step 5), the sintering temperature inside the sintering furnace is 1320 ℃ during the process of sintering the granular blank.
6. The preparation method of the high-temperature high-frequency low-loss ferrite material as claimed in claim 1 or 2, wherein in the step 5), the sintering time of the granular blank in the sintering furnace is 2-4 h.
7. The method for preparing a high-temperature high-frequency low-loss ferrite material according to claim 1 or 2, wherein in the step 2), the pre-sintering time of the grinding powder is 1.5 h-2.5 h.
8. The method for preparing a high-temperature high-frequency low-loss ferrite material according to claim 1 or 2, wherein in the step 4), the mass ratio of the organic binder added to the primary powder is 7-8 wt%.
9. The method for preparing a high-temperature high-frequency low-loss ferrite material as claimed in claim 1 or 2, wherein in said step 3), the fired powder added with additives is ball-milled.
10. The method for preparing a high-temperature high-frequency low-loss ferrite material according to claim 1 or 2, wherein in the step 3), the mass ratio of the additives added to the fired powder is 0.02-0.3 wt% of tin dioxide, 0.02-0.3 wt% of titanium dioxide, and 0.02-0.3 wt% of vanadium pentoxide.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113345673A (en) * | 2021-04-28 | 2021-09-03 | 北京计算科学研究中心 | High-frequency ultra-thin type switching power supply |
| CN115196958A (en) * | 2022-06-02 | 2022-10-18 | 江苏信维感应材料科技有限公司 | High-frequency wide-temperature MnZn ferrite and preparation method thereof |
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| JPH113813A (en) * | 1997-06-12 | 1999-01-06 | Kawasaki Steel Corp | Ferrite material |
| JP2000286119A (en) * | 1999-03-30 | 2000-10-13 | Kawasaki Steel Corp | Ferrite |
| CN101486567A (en) * | 2008-01-14 | 2009-07-22 | 王永安 | Preparation of high-frequency high temperature low loss MnNiZn ferrite material |
| CN107352992A (en) * | 2017-07-04 | 2017-11-17 | 浙江大学 | A kind of powder size control method of wideband wide-temperature and low-consumption manganese-zinc ferrite |
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2020
- 2020-08-13 CN CN202010814988.0A patent/CN112125655A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5846448A (en) * | 1994-04-27 | 1998-12-08 | Tdk Corporation | Ferrite and ferrite core for power supply |
| JPH113813A (en) * | 1997-06-12 | 1999-01-06 | Kawasaki Steel Corp | Ferrite material |
| JP2000286119A (en) * | 1999-03-30 | 2000-10-13 | Kawasaki Steel Corp | Ferrite |
| CN101486567A (en) * | 2008-01-14 | 2009-07-22 | 王永安 | Preparation of high-frequency high temperature low loss MnNiZn ferrite material |
| CN107352992A (en) * | 2017-07-04 | 2017-11-17 | 浙江大学 | A kind of powder size control method of wideband wide-temperature and low-consumption manganese-zinc ferrite |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113345673A (en) * | 2021-04-28 | 2021-09-03 | 北京计算科学研究中心 | High-frequency ultra-thin type switching power supply |
| CN115196958A (en) * | 2022-06-02 | 2022-10-18 | 江苏信维感应材料科技有限公司 | High-frequency wide-temperature MnZn ferrite and preparation method thereof |
| CN115196958B (en) * | 2022-06-02 | 2023-08-15 | 江苏信维感应材料科技有限公司 | High-bandwidth and high-temperature MnZn ferrite and preparation method thereof |
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