阅读说明：本技术 一种宽频宽温高磁导率Mn-Zn铁氧体材料及其制备方法与应用 (Wide-frequency wide-temperature high-permeability Mn-Zn ferrite material and preparation method and application thereof ) 是由 赖治邦 于 2020-12-15 设计创作，主要内容包括：本发明属于铁氧体材料技术领域,特别公开了一种宽频宽温高磁导率Mn-Zn铁氧体材料及其制备方法与应用。所述铁氧体材料,包括主成分和辅助成分；主成分包括51.5-53.5mol％氧化铁、氧化锰24.5-26.8mol％、余量为氧化锌；所述辅助成分相对于主成分的含量为：0～400ppm氧化铋、0～100ppm氧化硅、0～800ppm氧化钼和0～100ppm氧化铌,0～500ppm碳酸钙,所述辅助成分的含量均不为0。主成分和辅助成分配比合理,选择的辅助成分合适,含量适中,该锰-锌铁氧体材料既具有宽频特性又具有高导磁率的特性。(The invention belongs to the technical field of ferrite materials, and particularly discloses a Mn-Zn ferrite material with wide frequency, wide temperature range and high magnetic conductivity, and a preparation method and application thereof. The ferrite material comprises a main component and an auxiliary component; the main components comprise 51.5-53.5 mol% of ferric oxide, 24.5-26.8 mol% of manganese oxide and the balance of zinc oxide; the content of the auxiliary components relative to the main component is as follows: 0-400 ppm of bismuth oxide, 0-100 ppm of silicon oxide, 0-800 ppm of molybdenum oxide, 0-100 ppm of niobium oxide and 0-500 ppm of calcium carbonate, wherein the content of the auxiliary components is not 0. The proportion of the main component and the auxiliary component is reasonable, the selected auxiliary component is proper, the content is moderate, and the manganese-zinc ferrite material has the characteristics of both broadband and high magnetic permeability.)

1. A broadband wide-temperature high-permeability Mn-Zn ferrite material is characterized by comprising a main component and an auxiliary component;

the main components comprise 51.5-53.5 mol% of ferric oxide, 24.5-26.8 mol% of manganese oxide and the balance of zinc oxide; the content of the auxiliary components relative to the main component is as follows: 0-400 ppm of bismuth oxide, 0-100 ppm of silicon oxide, 0-800 ppm of molybdenum oxide, 0-100 ppm of niobium oxide and 0-500 ppm of calcium carbonate, wherein the content of the auxiliary components is not 0.

2. The broadband wide temperature high permeability Mn-Zn ferrite material of claim 1, wherein: the content of the auxiliary component relative to the main component comprises 240-270 ppm of calcium carbonate, 20-30 ppm of silicon oxide, 300-400 ppm of bismuth oxide, 0-800 ppm of molybdenum oxide and 0-200 ppm of niobium oxide, and the content of the auxiliary component is not 0.

3. A method for preparing the broadband wide-temperature high-permeability Mn-Zn ferrite material of claim 1, characterized by comprising the steps of:

(1) mixing the main components according to the proportion according to the formula, and then calcining to obtain calcined powder A;

(2) mixing the obtained powder A with auxiliary components and water, carrying out ball milling to obtain slurry B, and adding PVA to obtain powder;

(3) adding zinc stearate into the powder obtained in the step (2), and compacting and forming in a mode of fixing the density of the green body to obtain a green body;

(4) sintering the obtained green body; according to the sintering process, the method is divided into a temperature rising section, a constant temperature section and a temperature reduction section to obtain a final product.

4. The method of claim 3, wherein: the calcining temperature in the step (1) is 800-900 ℃; the calcining time is 2-10 h.

5. The method according to claim 3 or 4, characterized in that: the weight ratio of the water to the PVA to the slurry B in the step (2) is 2:1: 5-12.

6. The method of claim 3, wherein: and (3) performing wet ball milling to obtain a target particle size of 0.6-1.2 microns.

7. The method of claim 3, wherein: adding the zinc stearate in the step (3) according to the proportion of 0.02-0.05 wt.%.

8. The method of claim 3, wherein: the density of the fixed green embryo in the step (3) is specifically 3.4 +/-0.2 g/cm³。

9. The method of claim 3, wherein: the temperature rising section in the step (4) is heated from room temperature to 1300-1400 ℃, and the temperature rising time is 4-8 h; sintering at the constant temperature section for 6-12 h at 1300-1400 ℃ in the presence of 1-4% of oxygen; cooling the temperature from 1300-1400 ℃ to room temperature in an equilibrium atmosphere at a rate of 3-6 ℃/min.

10. Use of the broadband wide-temperature high-permeability Mn-Zn ferrite material according to claim 1 or 2 in the preparation of electronic components.

Technical Field

The invention belongs to the technical field of ferrite materials, and particularly relates to a Mn-Zn ferrite material with wide frequency, wide temperature range and high magnetic conductivity, and a preparation method and application thereof.

Background

With the rapid development of electronic technology, electronic components are increasingly miniaturized and high-frequency, and besides high magnetic permeability, the high-permeability MnZn ferrite is required to have broad-band and flat μ i-f curve, so that the material can have wider frequency and higher magnetic permeability, and the material has higher EMI filtering frequency. The MnZn ferrite material is prepared by adopting a traditional oxide ceramic process, and the MnZn ferrite material with good broadband characteristic and high magnetic conductivity is developed through the optimization research of a main formula, additives and a proper sintering process.

Disclosure of Invention

In order to overcome the disadvantages and shortcomings of the prior art, the invention provides a Mn-Zn ferrite material with wide frequency, wide temperature range and high magnetic permeability.

The invention also aims to provide a preparation method of the Mn-Zn ferrite material with wide frequency, wide temperature range and high magnetic permeability.

The invention further aims to provide application of the Mn-Zn ferrite material with wide frequency, wide temperature range and high magnetic permeability in preparation of electronic components.

The purpose of the invention is realized by the following scheme:

a broadband wide-temperature high-permeability Mn-Zn ferrite material comprises a main component and an auxiliary component;

the main components comprise 51.5-53.5 mol% of ferric oxide, 24.5-26.8 mol% of manganese oxide and the balance of zinc oxide; the content of the auxiliary components relative to the main component is as follows: 0 to 400ppm bismuth oxide (Bi)₂O₃) 0 to 100ppm of silicon oxide (SiO)₂) 0 to 800ppm of molybdenum oxide (MoO)₃) And 0 to 100ppm of niobium oxide (Nb)₂O₅) 0 to 500ppm of calcium carbonate (CaCO)₃) And the content of the auxiliary components is not 0.

Preferably, the content of the auxiliary component relative to the main component comprises 240-270 ppm of calcium carbonate, 20-30 ppm of silicon oxide, 300-400 ppm of bismuth oxide, 0-800 ppm of molybdenum oxide and 0-200 ppm of niobium oxide, and the content of the auxiliary component is not 0.

A method for preparing the broadband wide-temperature high-permeability Mn-Zn ferrite material comprises the following steps:

(1) mixing the main components according to the proportion according to the formula, and then calcining to obtain calcined powder A;

(2) mixing the obtained powder A with auxiliary components and water, carrying out ball milling to obtain slurry B, and adding PVA to obtain powder;

(3) adding zinc stearate into the powder obtained in the step (2), and compacting and forming in a mode of fixing the density of the green body to obtain a green body;

(4) sintering the obtained green body; according to the sintering process, the method is divided into a temperature rising section, a constant temperature section and a temperature reduction section to obtain a final product.

The calcining temperature in the step (1) is 800-900 ℃, and preferably 850 ℃; the calcination time is 2-10 h, preferably 6 h.

The ball milling in the step (2) is wet ball milling, and the target particle size is 0.6-1.2 mu m; preferably 0.9 μm; the grinding time is adjusted according to the particle size of the powder.

The weight ratio of the water to the PVA and the slurry B in the step (2) is 2:1: 5-12, and preferably 2:1: 8.

Adding the zinc stearate in the step (3) according to the proportion of 0.02-0.05 wt.%.

The density of the fixed green embryo in the step (3) is specifically 3.4 +/-0.2 g/cm³。

The temperature rising section in the step (4) is heated from room temperature to 1300-1400 ℃, and the temperature rising time is 4-8 h; sintering at the constant temperature section for 6-12 h at 1300-1400 ℃ in the presence of 1-4% of oxygen; cooling the temperature from 1300-1400 ℃ to room temperature in an equilibrium atmosphere at a rate of 3-6 ℃/min.

The Mn-Zn ferrite material with wide frequency, wide temperature and high magnetic conductivity is applied to the preparation of electronic elements.

Compared with the prior art, the invention has the following advantages and beneficial effects:

the manganese-zinc ferrite material has the characteristics of both broadband characteristic and high magnetic permeability, because the proportion of the main component and the auxiliary component is reasonable, the selected auxiliary component is proper, and the content is moderate.

Drawings

FIG. 1 shows the initial permeability as a function of temperature for the products obtained in example 3 and comparative example.

FIG. 2 is a graph showing the initial permeability at different frequencies of the products obtained in examples 1 to 3 and comparative example.

Detailed Description

The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto. The room temperature and unspecified temperatures according to the invention are 25-32 ℃.

The reagents used in the examples are commercially available without specific reference.

The preparation method of the Mn-Zn ferrite material with wide frequency, wide temperature and high magnetic permeability in the embodiment is as follows:

(1) mixing the main components, and presintering at 850 deg.C for 6 hr to obtain powder A;

(2) mixing the powder A obtained in the step (1) with the auxiliary components to obtain a ball grinding material B, adding deionized water into the ball grinding material B for ball grinding to obtain slurry B with the average particle size of 0.9 mu m, adding a polyvinyl alcohol solution into the slurry B, and stirring to obtain powder B, wherein the weight ratio of the polyvinyl alcohol solution to the slurry B is 1: 8.

(3) adding 0.02-0.05% of zinc stearate into the powder B obtained in the step (2), and then performing compression molding to obtain a green body, wherein the density of the fixed green body is specifically 3.4 +/-0.2 g/cm³。

(4) Sintering the green body obtained in the step (3) on a specific curve: a temperature rising stage: heating in air at 25-1380 deg.c for 6 hr; and (3) a heat preservation stage: at 1380 ℃, the oxygen content is 2 percent, and the temperature is kept for 8 hours; and (3) cooling: and (3) cooling at 1300-25 ℃ in a balanced atmosphere at the rate of 4.5 ℃/min to obtain the broadband wide-temperature high-permeability Mn-Zn ferrite material.

Example 1

A broadband wide-temperature high-permeability Mn-Zn ferrite material comprises a main component and an auxiliary component; the main raw material component is 51.5 wt% Fe₂O₃Calculated iron oxide, 24.5% by weight as Mn₃O₄Calculated manganese oxide and the balance of zinc oxide; the auxiliary raw material comprises 300ppm of CaCO based on the main component₃Calculated calcium oxide, 50ppm as SiO₂Calculated silica, 350ppm by Bi₂O₃Calculated bismuth oxide, 700ppm in terms of MoO₃Calculated molybdenum oxide, 10ppm as Nb₂O₅Calculated niobium oxide.

Example 2

A broadband wide-temperature high-permeability Mn-Zn ferrite material comprises a main component and an auxiliary component; the main raw material component contains 52.5 wt% of Fe₂O₃Calculated iron oxide, 25.5 wt.% as Mn₃O₄Calculated manganese oxide and the balance of zinc oxide; the auxiliary raw material comprises 400ppm of CaCO based on the main component₃Calculated calcium oxide, 25ppm by SiO₂Calculated silica, 300ppm by Bi₂O₃Calculated bismuth oxide, 600ppm by MoO₃Calculated molybdenum oxide, 5ppm as Nb₂O₅Calculated niobium oxide.

Example 3

A broadband wide-temperature high-permeability Mn-Zn ferrite material comprises a main component and an auxiliary component; the main raw material had a composition of 53.5 wt% Fe₂O₃Calculated iron oxide, 26.8 wt.% as Mn₃O₄Calculated manganese oxide and the balance of zinc oxide; the auxiliary raw material comprises 500ppm of CaCO based on the main component₃Calculated calcium oxide, 10ppm by SiO₂Calculated silica, 300ppm by Bi₂O₃Calculated bismuth oxide, 600ppm by MoO₃Calculated molybdenum oxide, 10ppm as Nb₂O₅Calculated niobium oxide.

The broadband high permeability manganese-zinc ferrite materials obtained from examples 1 to 3 of the present invention and the comparative example were tested to have the technical effects shown in the following table. The comparative example is the general performance of the existing high-conductivity broadband material industry.

TABLE 1

The initial permeability of the material obtained by the invention is more than 13000(25 ℃), and the initial permeability is more than 10000 in the range of 5-125 ℃, as shown in figure 1. In addition, the initial magnetic permeability is more than 13000 mu i within the range of 10 kHz-100 kHz; the initial magnetic permeability of 200kHz is more than 11000 mu i; the cut-off frequency is larger than 850KHz, as shown in figure 2, and the hysteresis constant eta B of the material is smaller than 0.5 multiplied by 10< -6>/mT (-25 ℃, B1 is 1.5mT, B2 is 3 mT).

The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.