CN115448714A - Manganese-zinc ferrite material, preparation method and application - Google Patents

Manganese-zinc ferrite material, preparation method and application Download PDF

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CN115448714A
CN115448714A CN202211246395.4A CN202211246395A CN115448714A CN 115448714 A CN115448714 A CN 115448714A CN 202211246395 A CN202211246395 A CN 202211246395A CN 115448714 A CN115448714 A CN 115448714A
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manganese
zinc
oxide
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ferrite material
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李斌
张政委
顾燮峰
许杰
张海浪
黄子谦
彭春兰
周晓强
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Shanghai Baosteel Magnetics Co ltd
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Abstract

The invention provides a manganese-zinc ferrite material and a preparation method and application thereof, wherein the material comprises a main component and an auxiliary component, the main component comprises ferric oxide, manganese oxide and zinc oxide, and the auxiliary component comprises calcium carbonate, nano-silica, niobium pentoxide, bismuth oxide and molybdenum trioxide; the preparation method comprises the steps of weighing, mixing calcium carbonate and nano-silica in the main component and the auxiliary component, presintering, ball milling, sanding, granulating, molding, sintering and the like; according to the invention, the Curie temperature and the magnetic conductivity are improved by adding the main components with specific types and contents; the loss factor is effectively reduced by adding the calcium carbonate and the nano calcium dioxide in advance as auxiliary components, so that the material disclosed by the invention is prepared under the condition of normal temperature of 10kHzLower specific loss factor less than or equal to 2 x 10 ‑6 And the specific loss factor is less than or equal to 15 multiplied by 10 under the condition of 100kHz ‑6 The initial magnetic permeability mu i is more than 9900 under the condition of normal temperature of 10-200kHz, and the Curie temperature is more than or equal to 160 ℃.

Description

Manganese-zinc ferrite material, preparation method and application
Technical Field
The invention belongs to the technical field of manganese-zinc soft magnetic ferrite materials, and particularly relates to a manganese-zinc ferrite material with low loss factor, high Curie temperature and high magnetic permeability, a preparation method and application thereof.
Background
With the great popularization of automobiles, the development of the automobile industry is also advanced and accelerated. At present, the cost of electronic equipment in automobiles is increasing, especially the yield of electric automobiles and hybrid automobiles is expanding, and automobile electronics will become one of the most potential electronic industries. The most used magnetic materials for early automobiles are permanent magnetic ferrites and permanent magnetic alloys for various motors, and the demand for soft magnetic ferrite materials for various inductors, transformers, chokes, filters, and the like used in automobiles is increasing.
The high-permeability manganese-zinc ferrite material required by the switching power supply common mode choke coil and the power supply filter magnetic core used on the automobile is required to normally work in a temperature range of-55-150 ℃ (even wider) in order to ensure high reliability and safety of the automobile, and meanwhile, lower loss is required, so that higher requirements are provided for the properties of the high-permeability manganese-zinc ferrite material, such as loss factor, permeability, curie temperature and the like.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a manganese-zinc ferrite material with low loss factor, high Curie temperature and high magnetic conductivity, and a preparation method and application thereof.
In order to achieve the purpose, the solution of the invention is as follows:
the invention provides a manganese-zinc ferrite material, which comprises a main component and an auxiliary component, wherein the main component comprises 52.5-54.0mol% (preferably 53.0-53.5 mol%) of Fe (calculated by taking the total amount of the main component as 100 mol%) 2 O 3 18.5-20.5mol% (preferably 19.5-20.3 mol%) ZnO and the rest MnO.
The auxiliary component comprises 0.01-0.03wt% (preferably 0.015-0.025 wt%) CaCO based on 100wt% of the main component 3 0.001-0.005wt% (preferably 0.002-0.004 wt%) of nano SiO 2 0.01 to 0.05wt% (preferably 0.02 to 0.04 wt%) of Bi 2 O 3 0.01-0.05wt% (preferably 0.02-0.04 wt%) MoO 3 And 0.005-0.015wt% (preferably 0.006-0.01 wt%) Nb 2 O 5 And (4) forming.
Preferably, the manganese-zinc ferrite material has a specific loss factor tan delta/[ mu ] i ≦ 2 × 10 at 10kHz at 25 ℃ -6 At 25 deg.C, specific loss factor tan delta/mu i is less than or equal to 15 x 10 under 100kHz -6 (ii) a The initial magnetic permeability mu i is larger than 9900 under the condition of 10-200kHz at normal temperature, and the Curie temperature is more than or equal to 160 ℃.
The Curie temperature of the manganese-zinc ferrite material is mainly determined by the three components, and is determined according to an empirical formula of the Curie temperature:
Figure BDA0003886814190000021
wherein α =12.8 ℃/%, b =354 ℃; x is Fe 2 O 3 The mol percent content of the ZnO, and Z is the mol percent content of the ZnO) to determine the mixture ratio of the three. From the formula, it is necessary that the curie temperature is high, and the zinc oxide content Z cannot be necessarily high, but the magnetic permeability is reduced when the zinc oxide content is low, so that the high curie temperature and the high initial magnetic permeability are in contradiction. The addition of the auxiliary components has little influence on the Curie temperature, and when the three main components of iron, manganese and zinc are determined, the Curie temperature is basically determined.
By adding Bi 2 O 3 Liquid phase sintering is formed, the solid-liquid reaction area is increased, the reaction rate is improved, the solid-phase reaction is promoted, the porosity is reduced, and the growth of crystal grains is facilitated, so that the purpose of improving the sintering density is achieved, and the magnetic conductivity is facilitated to be improved.
Adding MoO 3 It can also promote grain growth and inhibit the occurrence of excessively large grains, resulting in average grain sizeThe sintered density is increased, thereby improving the initial permeability of the material.
Selecting Fe with large specific surface area 2 O 3 The raw materials also promote the solid-phase reaction, thereby improving the magnetic permeability.
CaCO 3 Nano SiO 2 And Nb 2 O 5 Mainly reduces the loss factor and improves the frequency characteristic of magnetic permeability (namely, the magnetic permeability can be maintained above 9900 at the frequency from 10kHz to 200 kHz).
The second purpose of the invention is to provide a preparation method of the manganese-zinc ferrite material, which comprises the following steps:
(1) Weighing: selecting proper Fe 2 O 3 MnO and ZnO are used as main components of the raw materials, the materials are weighed and mixed according to the percentage of the components, and CaCO in the auxiliary components is weighed 3 And nano SiO 2 ；
(2) Mixing: mixing the main component (Fe) of step (1) 2 O 3 MnO and ZnO), and auxiliary component (CaCO) 3 And nano SiO 2 ) Mixing with deionized water in a grinder, and primarily grinding to obtain powder slurry;
(3) Pre-burning: drying and crushing the powder slurry, and then placing the powder slurry in a muffle furnace at 830-900 ℃ for heat preservation for 1-2h for pre-sintering;
(4) Ball milling: putting the pre-sintered material into a ball mill for ball milling, and primarily milling the pre-sintered material to improve the efficiency of subsequent sand milling;
(5) Sanding: adding bismuth oxide, molybdenum trioxide and niobium pentoxide in auxiliary components into the ball-milled material powder, putting the material powder into a grinder, adding pure water for secondary grinding, mainly correcting the main component and adding other additives (auxiliary components) for grinding at the stage until the D50 particle size of ground slurry is less than 1.1 mu m;
(6) And (3) granulation: drying the ground slurry, and then adding polyvinyl alcohol (PVA) for granulation;
(7) Molding: pressing the granulated material powder into an annular green body;
(8) And (3) sintering: and (3) placing the molded green body into a sintering furnace with atmosphere regulation, sintering under the protection of nitrogen and preserving heat.
Preferably, in step (1), fe 2 O 3 Has a specific surface area of more than 4.0m 2 /g。
Preferably, in the step (2), the ratio of the (main component + auxiliary component) to the deionized water is 1.
The invention adds CaCO in advance 3 And nano SiO 2 The two additives can effectively reduce the loss factor of the material. CaCO added before pre-burning 3 And nano SiO 2 The two additives are more beneficial to the reaction between the two additives and the raw materials in the pre-sintering process, and effectively increase the grain boundary resistance of the manganese-zinc ferrite material, thereby better reducing the loss factor.
In the step (3), the temperature of the pre-sintering stage is 830-900 ℃ and CaCO 3 And nano SiO 2 Can react at the temperature and generate CaSiO with high resistivity 3 Compounds, adding CaCO beforehand 3 And nano SiO 2 The reaction of the manganese-zinc ferrite and the zinc oxide can be facilitated, and the concentration of the reacted compound at the grain boundary of the manganese-zinc ferrite material and the penetration of the reacted compound into the grain are facilitated to a certain depth, so that the resistivity of the manganese-zinc ferrite can be obviously increased, and the loss factor is reduced.
Preferably, in the step (8), the sintering temperature is 1340-1360 ℃, and the heat preservation time is 2-6h.
The invention also provides an application of the manganese-zinc ferrite material in automobile electronic components.
Due to the adoption of the scheme, the invention has the beneficial effects that:
the manganese-zinc ferrite material with the final performance is obtained by adding the main component (the Curie temperature and the magnetic conductivity are improved) and the auxiliary component with specific types and contents for reaction and adding the calcium carbonate and the nano calcium dioxide in advance as the auxiliary component, and compared with the prior art, the manganese-zinc ferrite material has the specific loss factor tan delta/mu i (25 ℃) of less than or equal to 6 multiplied by 10 under the condition of 10kHz -6 Reduced to less than or equal to 2 × 10 -6 Ratio at 100kHzA loss factor tan delta/[ mu ] i (25 ℃) of less than or equal to 30 multiplied by 10 -6 Reduced to less than or equal to 15 multiplied by 10 -6 Therefore, the manganese-zinc ferrite material has the performance of low loss factor, high Curie temperature and high magnetic conductivity.
Detailed Description
The invention provides a manganese-zinc ferrite material and a preparation method thereof.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1: fe as shown in Table 1 2 O 3 Weighing ZnO and MnO in proportion, and simultaneously weighing CaCO 3 Is 0.015wt% and nano SiO 2 0.002wt% of two additives are put into a grinder together and mixed with deionized water with the weight 1 time that of the materials for 30min; drying and crushing the mixed powder, putting the powder into a muffle furnace for presintering at 870 ℃ for 1h, and taking out and cooling; putting the pre-sintered powder into a ball mill, ball-milling for 30min, and taking out; putting the ball-milled powder into a grinding machine, and adding the rest additives (Bi) at the same time 2 O 3 0.03wt% of MoO 3 The addition amount of Nb is 0.03wt% 2 O 5 The addition amount is 0.01 wt%), and pure water is added for wet grinding until the grain diameter of D50 of the slurry is 1.03 mu m; drying the slurry, adding PVA for granulation and forming
Figure BDA0003886814190000032
A sample ring of (1); placing the sample ring in a sintering furnace with atmosphere regulation, setting the sintering temperature to 1350 ℃, and keeping the temperature for 5h; and (5) carrying out electrical property detection on the sintered sample ring. In Table 1, the samples are numbered 1, 2, 3, 4, 5, 6 and the Fe used 2 O 3 The specific surface area is 4.9m 2 Fe used in sample No. 7 2 O 3 The specific surface area is 3.5m 2 /g。
TABLE 1
Figure BDA0003886814190000031
Figure BDA0003886814190000041
Note: the numbered bands are all comparative examples.
In table 1, samples No. 1-3 are examples of the present invention, the main components are all within the range defined by the present invention, and the material properties completely satisfy the index. 4-6 samples are Fe 2 O 3 Or the ZnO content is beyond the limited range of the invention, and the performance can not completely meet the requirement of the index. 7 sample is Fe with specific surface area not within the limits of the present invention 2 O 3 The material properties cannot completely meet the index.
Example 2:
weighing Fe 2 O 3 53.46mol% of ZnO, 20.09mol% of ZnO and the balance of MnO, and CaCO was weighed in the proportions shown in Table 2 3 And nano SiO 2 Putting the two additives into a grinding machine together, adding deionized water with the weight 1.1 times of that of the materials, and mixing for 30min; drying and crushing the mixed powder, putting the powder into a muffle furnace for presintering at 870 ℃ for 1h, and taking out and cooling; putting the pre-sintered powder into a ball mill, ball-milling for 30min, and taking out; putting the ball-milled powder into a grinding machine, and adding the rest additives (Bi) at the same time 2 O 3 0.03wt%, moO 3 The addition amount of Nb is 0.03wt% 2 O 5 The addition amount is 0.01wt percent), and pure water is added for wet milling until the grain diameter of the slurry D50 is 1.01 mu m; drying the slurry, adding PVA for granulation and forming
Figure BDA0003886814190000044
A sample ring of (1); placing the sample ring in a sintering furnace with atmosphere regulation, setting the sintering temperature to 1350 ℃, and keeping the temperature for 5h; and (5) carrying out electrical property detection on the sintered sample ring. Table 3 shows the electromagnetic properties of the samples of example 2.
TABLE 2
Figure BDA0003886814190000042
TABLE 3
Figure BDA0003886814190000043
Figure BDA0003886814190000051
Note: the numbered bands are all comparative examples.
In the examples shown in Table 3, samples No. 8-10 are examples of the present invention, the main additive ratio is within the range defined by the present invention, and the material properties meet the index. The sample is CaCO 11-13 3 Or nano SiO 2 The proportion is beyond the limit range of the invention, and the performance can not completely meet the index requirement. Sample No. 14 differs from sample No. 8 mainly by nano CaCO 3 And nano SiO 2 Different modes of addition, caCO 3 And nano SiO 2 The addition of (2) is not in the mixing step, but in the sanding step after ball milling, the addition of grinding together with other additives, the 14 × sample performance also does not fully meet the index requirements.
Example 3:
weighing Fe 2 O 3 53.46mol% of ZnO, 20.09mol% of ZnO and the balance of MnO, and CaCO as required 3 Is 0.015wt% and nano SiO 2 0.002wt% of two additives are put into a grinder together and mixed with deionized water with the weight 1 time that of the materials for 30min; drying and crushing the mixed powder, placing the powder in a muffle furnace for presintering at 870 ℃ for 1h, and taking out the powder for cooling; putting the pre-sintered powder into a ball mill, ball-milling for 30min, and taking out; the ball-milled powder was placed in a mill while the remaining additives (Bi) were added as per Table 4 2 O 3 、MoO 3 、Nb 2 O 5 ) Adding pure water to wet-grind until the grain diameter of the slurry D50 is 1.07 mu m; after the slurry is dried,adding PVA for granulation and forming
Figure BDA0003886814190000054
A sample ring of (3); placing the sample ring in a sintering furnace with atmosphere regulation, setting the sintering temperature to 1350 ℃, and keeping the temperature for 5h; the sintered sample rings were subjected to electrical property test, and table 5 shows the electromagnetic properties of the samples of example 3.
TABLE 4
Figure BDA0003886814190000052
Note: the numbered bands are comparative examples.
TABLE 5
Figure BDA0003886814190000053
Figure BDA0003886814190000061
Note: the numbered bands are comparative examples.
In Table 5, samples No. 15-17 are examples of the present invention, the main additive ratios are all within the range defined by the present invention, and the material properties meet the specifications. 18X-20X sample is Bi 2 O 3 、MoO 3 Or Nb 2 O 5 The proportion is beyond the limit range of the invention, and the performance can not completely meet the requirement of the index.
The comparison of the performance test results shows that the manganese-zinc ferrite material prepared by the formula and the preparation method has the specific loss factor tan delta/mu i (25 ℃) less than or equal to 2 multiplied by 10 under the condition of 10kHz -6 The specific loss factor tan delta/mu i (25 ℃) is less than or equal to 15 multiplied by 10 under the condition of 100kHz -6 And has good frequency characteristics, initial magnetic permeability mu i is larger than 9900 under the condition of 10-200kHz at normal temperature, and Curie temperature is more than or equal to 160 ℃.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments and the generic principles defined herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments. Those skilled in the art should appreciate that many modifications and variations are possible in light of the above teaching without departing from the scope of the invention.

Claims (7)

1. A manganese-zinc ferrite material is characterized in that: the manganese-zinc ferrite material comprises a main component and an auxiliary component, wherein the main component comprises 52.5-54.0mol% of ferric oxide, 18.5-20.5mol% of zinc oxide and the balance of manganese oxide, wherein the total amount of the main component is 100 mol%;
the auxiliary component comprises 0.01-0.03wt% of calcium carbonate, 0.001-0.005wt% of nano silicon dioxide, 0.01-0.05wt% of bismuth oxide, 0.01-0.05wt% of molybdenum trioxide and 0.005-0.015wt% of niobium pentoxide, wherein the auxiliary component accounts for 100wt% of the main component.
2. The manganese-zinc-ferrite material of claim 1, wherein: the manganese-zinc ferrite material has a specific loss factor tan delta/mu i of not more than 2 x 10 at 25 ℃ and 10kHz -6 At 25 deg.C, specific loss factor tan delta/mu i is less than or equal to 15 x 10 under 100kHz -6 (ii) a The initial magnetic permeability mu i is larger than 9900 under the condition of 10-200kHz at normal temperature, and the Curie temperature is more than or equal to 160 ℃.
3. The method for preparing a manganese-zinc-ferrite material according to claim 1, wherein: which comprises the following steps:
(1) Weighing: selecting ferric oxide, manganese oxide and zinc oxide as main components of raw materials, weighing and proportioning, and simultaneously weighing calcium carbonate and nano-silica in auxiliary components;
(2) Mixing: mixing the main component, the auxiliary component and the deionized water obtained in the step (1), and primarily grinding to obtain powder slurry;
(3) Pre-burning: drying and crushing the powder slurry, and then placing the powder slurry in a muffle furnace at 830-900 ℃ for heat preservation for 1-2h for pre-sintering;
(4) Ball milling: ball milling the pre-sintered material;
(5) Sanding: adding bismuth oxide, molybdenum trioxide and niobium pentoxide in auxiliary components into the ball-milled material powder, and adding pure water for secondary grinding until the D50 particle size of the ground slurry is less than 1.1 mu m;
(6) And (3) granulation: drying the ground slurry and then granulating;
(7) Molding: pressing the granulated material powder into an annular green body;
(8) And (3) sintering: and sintering the formed green body under the protection of nitrogen and preserving heat.
4. The method of claim 3, wherein: in the step (1), the specific surface area of the ferric oxide is more than 4.0m 2 /g。
5. The method of claim 3, wherein: in the step (2), the ratio of the main component to the auxiliary component to the deionized water is 1.
6. The method of claim 3, wherein: in the step (8), the sintering temperature is 1340-1360 ℃, and the heat preservation time is 2-6h.
7. The use of the manganese-zinc-ferrite material of claim 1 in automotive electronic components.
CN202211246395.4A 2022-10-12 2022-10-12 Manganese-zinc ferrite material, preparation method and application Pending CN115448714A (en)

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Application publication date: 20221209