CN103058643B - Mn-Zn soft magnetic ferrite material with high, temperature, high superposition and low power consumption, and preparation method of Mn-Zn soft magnetic ferrite material - Google Patents
Mn-Zn soft magnetic ferrite material with high, temperature, high superposition and low power consumption, and preparation method of Mn-Zn soft magnetic ferrite material Download PDFInfo
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Abstract
The invention discloses a Mn-Zn soft magnetic ferrite material with high, temperature, high superposition and low power consumption. Main elements of the Mn-Zn soft magnetic ferrite material comprise 69.5-73% of Fe2O3, 5-10% of ZnO and the balance of Mn3O4; and additives comprise 0.01-0.08% of CaO, 0.015-0.09% of Nb2O5, 0.02-0.1% of V2O5, 0.03-0.2% of TiO2, 0.06-0.7% of Co2O3, 0.003-0.13% of ZrO2, 0.01-0.1% of K2CO3 and 0.04-0.5% of NiO. The invention also discloses a preparation method of the Mn-Zn soft magnetic ferrite material. According to the method, sintering is performed in a nitrogen protection atmosphere, and a densification process is adopted in sintering. A finished product made of the material by the method disclosed by the invention has the characteristics that the initial magnetic conductivity is high, the superposition property is good, the power consumption under a high-frequency testing condition is low, and the Curie temperature is higher than 260 DEG C.
Description
Technical field
The present invention relates to ferrite field of electronic materials, particularly relate to a kind of wide temperature height superposition low power consumption Mn-Zn soft magnetic ferrite and preparation method.
Background technology
Along with constantly developing rapidly of electronics work and rest industry, maximum as current production rate, most widely used soft magnetic ferrite, has been widely used in various electronic devices and components.MnZn ferrite material technical feature competitively improves in Ge great ferrite company of the world, to adapt to no Application Areas, the users such as convertible frequency air-conditioner, Non-polarized lamp lighting electronic, power electronics, IT industry, communication, domestic electronic overcritical under, a kind ofly require that material has higher Bs, better DC superposition characteristic, lower power loss, wider frequency of utilization and wider thermal adaptation scope, therefore, the research of MnZn ferrite material has entered into wide temperature, high DC stacked, high Bs, lower power loss field.Analyze the material that market Shang Ge material manufacturing firm releases, be not difficult to find out that a kind of wide temperature, low-loss material are all being sought by each material producer, to replace numerous high-frequency and low-consumption Ferrite Materials.
Widely using and performance raising of environmental protection electromagnetic induction electrodeless lamp, facilitates continually developing and operation of this material, widely uses under low frequency 200 ~ 300kHz low and medium frequency state.But use Non-polarized lamp efficiency to reach best under how existence takes into account built-in and external two kinds of structures and require to have enough magnetic permeabilities at-40 DEG C, require that heating is little, loss is low simultaneously simultaneously; On the other hand electronic product always has current component at work, affecting normal use, therefore also needing material to have enough Bs, DC superposition characteristic for preventing electronic product not because there being the existence of electric current.
As most popular supply transformer, office automation, domestic electronic, communication etc. require to have wide temperature, low-loss, high magnetic permeability, high DC stacked be indispensable assembly, Non-polarized lamp and vehicle electronics require in the change of wide temperature, high-frequency range internal loss and magnetic permeability little, have high stability and high reliability.Use under having the occasion of big current or DC bias field in vehicle electronics switching medium power supply, this requirement all needs material to have the difference of enough large saturation magnetic flux density Bs and remanent magnetism Br, thus impact has good superimposed characteristics.
As the low-loss manganese-zinc power ferrite material of the disclosed a kind of high saturated Bs of Chinese patent application (CN101183582A), it is by optimization of C/C composites and doping, particularly adds under 2 ~ 4mol%Ni0 obtains BS(100 degree and is greater than 460T) high frequency power consumption 500kHz, 50mT, be less than 150kW/m under 100 degree
3, but do not mention broad temperature, broadband and Curie temperature height, thus it is of limited application.
Disclose a kind of high saturation magnetic flux density, low loss manganese-zinc ferrite material and preparation method thereof in Chinese patent application (CN1749209A) in addition, it by doping and technology controlling and process, obtain 100kHz, 200mT, 45 DEG C time lower than 245kw/m
3power consumption and 1194A/m, 50mT, 25 DEG C time saturation magnetic flux density higher than the result of 535mT, but do not mention wide gentle wideband, Curie temperature equally, thus its use range is quite limited.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of wide temperature height superposition low power consumption Mn-Zn soft magnetic ferrite and preparation method, made finished product has high initial permeability and suitable 25 degree ~ 140 degree power consumptions, power consumption plateau in 25 DEG C ~ 140 DEG C temperature ranges, remanent magnetism is little, and superimposed characteristics is good, under high frequency 500kHz, 50mT, 100 degree of test conditions, power consumption loss is less than 300kw/m simultaneously
3, at 1MHz, 30mT, the loss of 100 DEG C of test condition power consumptions is less than 500kw/m
3, Curie temperature reaches more than 260 DEG C.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: provide a kind of wide temperature height superposition low power consumption Mn-Zn soft magnetic ferrite, its principal constituent by mass percentage, calculates with oxide compound: Fe
20
3be 69.5 ~ 73%, Zn0 be 5 ~ 10%; All the other are Mn
30
4; Fe
20
3, Mn
30
4be 100% with Zn0 sum;
Additive is counted based on the total mass of principal constituent, by mass percentage, calculates and comprises: Ca0:0.01 ~ 0.08%, Nb with oxide compound
20
5: 0.015 ~ 0.09%, V
20
5: 0.02 ~ 0.1%, Ti0
2: 0.03 ~ 0.2%, C0
20
3: 0.06 ~ 0.7%, Zr0
2: 0.003 ~ 0.13%, K
2c0
3: 0.01 ~ 0.1%, Ni0:0.04 ~ 0.5%.
In a preferred embodiment of the present invention, described principal constituent by mass percentage, calculates with oxide compound: Fe
20
3: 71.5%, Mn
30
4: 23.5%, Zn0:5%, described additive by mass percentage, calculates with oxide compound: Ca0:0.05%, Nb
20
5: 0.05%, V
20
5: 0.02%, Ti0
2: 0.08%, C0
20
3: 0.18%, Zr0
2: 0.015%, K
2c0
3: 0.05%, Ni0:0.08%.
Another object of the present invention is to provide a kind of preparation method of wide temperature height superposition low power consumption Mn-Zn soft magnetic ferrite, comprises the following steps:
1), Fe
20
3be 69.5 ~ 73%, Zn0 be 5 ~ 10%, surplus is Mn304, mixes with star ball mill, makes principal constituent powder;
2), the principal constituent powder of step 1) gained is carried out pre-burning at 800 ~ 1000 DEG C; Soaking time is 2 ~ 4.5 hours;
3), by step 2) powder of gained adds following additive in mass ratio:
Ca0:0.02 ~ 0.06%, Nb
20
5: 0.02 ~ 0.06%, V
20
5: 0.03 ~ 0.1%, Ti0
2: 0.04 ~ 0.15%, C0
20
3: 0.08 ~ 0.2%, Zr0
2: 0.005 ~ 0.10%, K
2c0
3: 0.01 ~ 0.04%, Ni0:0.05 ~ 0.2%, and carry out second time star ball milling, make secondary star ball milling powder;
4), the secondary star ball milling powder of step 3) gained is dried after granulation, shaping, make sample blank;
5), by the sample blank of step 4) gained sinter in nitrogen protective sintering kiln, make magnetic core.
In a preferred embodiment of the present invention, described step 4): the secondary star ball milling powder of step 3) gained is added in mass ratio the PVA organic binder bond of 8 ~ 12%, and mix, after granulation, powder pressing is become sample blank by testing laboratory's 10 tons of press.
In a preferred embodiment of the present invention; described step 5) is: be placed in nitrogen protective sintering kiln by the sample blank of step 4) obtained by molding and sinter; be about 1% carry out densification intensification section 1150 ~ 1250 DEG C by oxygen level; 1320 ~ 1350 DEG C of insulations 4 ~ 6 hours; be 4 ~ 7% in holding-zone oxygen partial pressure, temperature descending section is balanced atmosphere sintering.
In a preferred embodiment of the present invention, the average particle size range of the described principal constituent powder made in described step 1) reaches 0.7 ~ 1.1 micron; The median size of the described secondary star ball milling powder made in described step 3) reaches 0.7 ~ 1.0 micron.
In a preferred embodiment of the present invention, in described step 4), the density of the described sample blank that compacting is formed is 3.0 ± 0.05g/cm
3, sintering the described magnetic core density made in described step 5) is 4.85 ± 0.05g/cm
3.
In a preferred embodiment of the present invention, described principal constituent by mass percentage, calculates with oxide compound: Fe
20
3: 71.5%, Mn
30
4: 23.5%, Zn0:5%, described additive by mass percentage, calculates with oxide compound: Ca0:0.05%, Nb
20
5: 0.05%, V
20
5: 0.02%, Ti02:0.08%, C0
20
3: 0.18%, Zr0
2: 0.015%, K
2c0
3: 0.05%, Ni0:0.08%.
The invention has the beneficial effects as follows:
The present invention's wide temperature height superposition low power consumption Mn-Zn soft magnetic ferrite adds calcium oxide, titanium oxide and cobalt/cobalt oxide, barium oxide, nickel oxide by above-mentioned formula and compound, make described ferrite have the initial permeability of 3500 ± 25%, and valley point power loss reach 270kw/m in 25 ~ 140 DEG C of temperature provinces
3, Tc is greater than 260 DEG C, and under 500KHZ, 50mT, 100 degree of test conditions, power consumption loss is less than 300kw/m
3, at 1MHz, 30mT, the loss of 100 DEG C of test condition power consumptions is less than 500kw/m
3.
The preparation method of the present invention's wide temperature height superposition low power consumption Mn-Zn soft magnetic ferrite, by the principal constituent of optimization and the composite mixed and suitable reduction median size of optimization, increase the activity of material, formed uniform, consistence is good, without the microtexture of another phase, sintering process temperature, atmosphere curve simultaneously by optimizing, form the ferrite that void content is low, density is large.
In sum, wide temperature prepared by the present invention, high frequency, high-curie temperature low-loss iron oxygen ferrite, can be used for Non-polarized lamp electromagnetism coupling apparatus, in the electronic materials such as vehicle electronics, its special performance is:
The Curie temperature overwhelming majority of the wide adiabator of numerous high-frequency and low-consumptions is greater than 230 DEG C for Tc, and can reach about 270 DEG C individually, some high temperature power consumptions are too high, partly at very low temperature as magnetic permeability when-35 DEG C is too low, Non-polarized lamp cannot start.The wide temperature of the present invention, high frequency, high-curie temperature well solve the appearance of this problem.
On the other hand, the present invention is by too large for low-consumption Mn-Zn ferrite material High-frequency and low-frequency power consumption difference, and the problem that cannot take into account well solves and uses these analogous products 500kHz, 1MHz two frequencies can meet the requirement of user.
Utilize material of the present invention and the product made by preparation method not only for domestic electronic, communicate, the field such as photoelectricity, automotive electronics, more for the Non-polarized lamp frontiers such as electromagnetism coupling apparatus magnetic core market and vehicle electronics, forceful electric power, convertible frequency air-conditioner.
Embodiment
Below preferred embodiment of the present invention is described in detail, can be easier to make advantages and features of the invention be readily appreciated by one skilled in the art, thus more explicit defining is made to protection scope of the present invention.
Embodiment one:
Take the Fe of 53mol
20
3, the Mn0 of 38.5mol all the other be Zn0, wherein Mn0 raw material form is trimanganese tetroxide, use source-2, middle steel sky type, its Mn% is greater than 71%, iron oxide red adopts domestic Baosteel iron oxide red, purity is greater than 99.2%, zinc oxide is capital, Shanghai, its purity is greater than 99.7%, after above-mentioned raw materials is mixed, drop in sand mill in the lump and stir, controlling median size is 0.7 ~ 1.0 micron, after heater case oven dry, at 900 ± 30 DEG C of temperature, electricity consumption heating revolving kiln carries out pre-burning, secondary sand milling is carried out after pre-burning, in sand grinding process, add pure water, dispersion agent, defoamer, and add additive, relatively described principal constituent total amount, in described additive, the mass percentage content of each material respectively: Ca0:0.05%, Nb
20
5: 0.015%, V
20
5: 0.06%, Ti0
2: 0.06%, C0
20
3: 0.2%, Zr0
2: 0.03%, K
2c0
3: 0.4%, Ni0:0.3% controls median size is 0.7 ~ 1.0 micron, finally carries out secondary spraying and obtains Mn-Zn ferrite particles powder.
Get this particulate material shaping compacting T25*15*12(mm) toroidal core and EC4244 magnetic core, compact density is 3.0 ± 0.05g/cm
3, 1320 ~ 1380 DEG C of nitrogen protection insulations 4 ~ 6 hours, cooling area cooled under carrying out balanced atmosphere by Blake equation.
Through the magnetic core prepared by said process, grind the instruments such as BHS-40 DC characteristic tester, thermostat container and resistivity tester through U.S. AW2335 power consumption instrument, TH2828S, TH1773, Japan's reason and record correlation properties at magnetic core as table 1 and table 2.
Embodiment two
Take the Fe20 of 53.8mol
3, the Mn0 of 39.5mol all the other be Zn0, wherein Mn0 raw material form is trimanganese tetroxide, use source-2, middle steel sky type, its Mn% is greater than 71%, iron oxide red adopts domestic Baosteel iron oxide red, purity is greater than 99.2%, zinc oxide is capital, Shanghai, its purity is greater than 99.7%, after above-mentioned raw materials is mixed, drop in sand mill in the lump and stir, controlling median size is 0.7 ~ 1.0 micron, after heater case oven dry, at 880 ± 30 DEG C of temperature, electricity consumption heating revolving kiln carries out pre-burning, secondary sand milling is carried out after pre-burning, in sand grinding process, add pure water, dispersion agent, defoamer, and add additive, relatively described principal constituent total amount, in described additive, the mass percentage content of each material respectively: Ca0:0.02%, Nb
20
5: 0.05%, V
20
5: 0.02%, Ti0
2: 0.02%, C0
20
3: 0.3%, Zr0
2: 0.05%, K
2c0
3: 0.2%, Ni0:0.7% controls median size is 0.7 ~ 1.0 micron, finally carries out secondary spraying and obtains Mn-Zn ferrite particles powder.
Get this particulate material shaping compacting T25*15*12(mm) toroidal core and EC4244 magnetic core, compact density is 3.0 ± 0.05g/cm
3, 1320 ~ 1380 DEG C of nitrogen protection insulations 4 ~ 6 hours, cooling area cooled under carrying out balanced atmosphere by Blake equation.
Through the magnetic core prepared by said process, grind the instruments such as BHS-40 DC characteristic tester, thermostat container and resistivity tester through U.S. AW2335 power consumption instrument, TH2828S, TH1773, Japan's reason and record correlation properties at magnetic core as table 1 and table 2.
Table 1 toroidal core material property of the present invention
Table 2 the present invention is for the superimposed characteristics of EC4244
From table 1 and table 2, ferrite in manganese zinc series of the present invention, by adjusting principal constituent and minor component, is specially Ti0
2and C0
20
3the reinforcement of hybrid compensation effect, wide temperature characteristics is obvious; Doping system such as Ni0 adds the raising using Tc, and control climate and densification process use this material to have higher initial permeability simultaneously, and the power dissipation ratio in 25 ~ 140 DEG C of temperature provinces is more smooth, and 100 DEG C of power consumptions are less than 280 mw/cm
3, high frequency power consumption is lower, DC stacked excellent, and Curie temperature is greater than 260 DEG C.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (5)
1. a wide temperature height superposition low power consumption Mn-Zn soft magnetic ferrite, it is characterized in that, its principal constituent by mass percentage, calculates with oxide compound: Fe
20
3be 69.5 ~ 73%, Zn0 be 5 ~ 10%; All the other are Mn
30
4; Fe
20
3, Mn
30
4be 100% with Zn0 sum;
Additive is counted based on the total mass of principal constituent, by mass percentage, calculates and comprises: Ca0:0.01 ~ 0.08%, Nb with oxide compound
20
5: 0.015 ~ 0.09%, V
20
5: 0.02 ~ 0.1%, Ti0
2: 0.03 ~ 0.2%, C0
20
3: 0.06 ~ 0.7%, Zr0
2: 0.003 ~ 0.13%, K
2c0
3: 0.01 ~ 0.1%, Ni0:0.04 ~ 0.5%.
2. wide temperature height superposition low power consumption Mn-Zn soft magnetic ferrite according to claim 1, it is characterized in that, described principal constituent by mass percentage, calculates with oxide compound: Fe
20
3: 71.5%, Mn
30
4: 23.5%, Zn0:5%, described additive by mass percentage, calculates with oxide compound: Ca0:0.05%, Nb
20
5: 0.05%, V
20
5: 0.02%, Ti0
2: 0.08%, C0
20
3: 0.18%, Zr0
2: 0.015%, K
2c0
3: 0.05%, Ni0:0.08%.
3. a preparation method for wide temperature height superposition low power consumption Mn-Zn soft magnetic ferrite, is characterized in that, comprise the following steps:
1), Fe
20
3be 69.5 ~ 73%, Zn0 be 5 ~ 10%, surplus is Mn
30
4, mix with star ball mill, make principal constituent powder; The average particle size range of the described principal constituent powder made in described step 1) reaches 0.7 ~ 1.1 micron;
2), the principal constituent powder of step 1) gained is carried out pre-burning at 800 ~ 1000 DEG C; Soaking time is 2 ~ 4.5 hours;
3), by step 2) powder of gained adds following additive in mass ratio:
Ca0:0.02 ~ 0.06%, Nb
20
5: 0.02 ~ 0.06%, V
20
5: 0.03 ~ 0.1%, Ti0
2: 0.04 ~ 0.15%, C0
20
3: 0.08 ~ 0.2%, Zr0
2: 0.005 ~ 0.10%, K
2c0
3: 0.01 ~ 0.04%, Ni0:0.05 ~ 0.2%, and carry out second time star ball milling, make secondary star ball milling powder; The median size of the described secondary star ball milling powder made in described step 3) reaches 0.7 ~ 1.0 micron;
4), the secondary star ball milling powder of step 3) gained is dried after granulation, shaping, make sample blank;
5), the sample blank of step 4) obtained by molding is placed in nitrogen protective sintering kiln sinters; be 1% carry out densification intensification section 1150 ~ 1250 DEG C by oxygen level; 1320 ~ 1350 DEG C of insulations 4 ~ 6 hours, be 4 ~ 7% in holding-zone oxygen partial pressure, temperature descending section is balanced atmosphere sintering.
4. the preparation method of wide temperature height superposition low power consumption Mn-Zn soft magnetic ferrite according to claim 3, it is characterized in that, described step 4): the secondary star ball milling powder of step 3) gained is added in mass ratio the PVA organic binder bond of 8 ~ 12%, and mix, after granulation, powder pressing is become sample blank by testing laboratory's 10 tons of press.
5. the preparation method of wide temperature height superposition low power consumption Mn-Zn soft magnetic ferrite according to claim 3, it is characterized in that, in described step 4), the density of the described sample blank that compacting is formed is 3.0 ± 0.05g/cm
3, sintering the magnetic core density made in described step 5) is 4.85 ± 0.05g/cm
3.
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| CN103524124A (en) * | 2013-09-13 | 2014-01-22 | 苏州天源磁业有限公司 | Sintering method of high-magnetic-permeability MnZn ferrite material |
| CN103760399A (en) * | 2013-12-31 | 2014-04-30 | 上海宝钢磁业有限公司 | Method for manufacturing Hall current sensor by using ferrite and Hall current sensor |
| CN103951411A (en) * | 2014-04-15 | 2014-07-30 | 南通冠优达磁业有限公司 | Wide-temperature-range low-power-consumption high-Curie-temperature manganese/zinc ferrite material and preparation method thereof |
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| CN105330284A (en) * | 2015-11-27 | 2016-02-17 | 全椒君鸿软磁材料有限公司 | Method for preparing wide-temperature high-conductivity soft magnetic ferrite core material |
| CN105565391A (en) * | 2015-12-22 | 2016-05-11 | 南通华兴磁性材料有限公司 | Preparation process of wide-temperature low-power-consumption manganese zinc ferrite powder |
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| CN106007696A (en) * | 2016-05-13 | 2016-10-12 | 泰州茂翔电子器材有限公司 | Wide-temperature-range high-Bs ferrite material and preparing technology thereof |
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| CN108275994B (en) * | 2018-01-18 | 2020-11-03 | 常熟市三佳磁业有限公司 | Manganese-zinc ferrite with wide temperature range, low power consumption and high direct current superposition characteristic and preparation method thereof |
| CN109354489B (en) * | 2018-11-12 | 2021-02-26 | 横店集团东磁股份有限公司 | High-frequency low-loss ferrite material and preparation method thereof |
| CN111233451A (en) * | 2018-11-28 | 2020-06-05 | 泰州茂翔电子器材有限公司 | High Bs, high frequency and low loss magnetic material |
| CN111039666A (en) * | 2019-12-26 | 2020-04-21 | 天通控股股份有限公司 | Manganese zinc ferrite material with ultrahigh saturation magnetic flux density and preparation method thereof |
| CN115784731A (en) * | 2022-11-22 | 2023-03-14 | 上海华源磁业股份有限公司 | Preparation method of high-impedance soft magnetic ferrite magnetic core |
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