CN103951411A - Wide-temperature-range low-power-consumption high-Curie-temperature manganese/zinc ferrite material and preparation method thereof - Google Patents
Wide-temperature-range low-power-consumption high-Curie-temperature manganese/zinc ferrite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a wide-temperature-range superposed low-power-consumption high-Curie-temperature manganese/zinc ferrite material and a preparation method thereof, belonging to the technical field of soft magnetic ferrite materials. The manganese/zinc ferrite material comprises main components and additives, wherein the main components comprises the following materials in percentage by mass measured by oxide: 69.0-72.5% of Fe2O3, 6-10% of ZnO and the balance of Mn3O4, Fe2O3, with the sum of the Mn3O4 and ZnO being 100%; the additives comprises the following materials by weight percent measured by oxide: 0.02-0.07% of CaO, 0.02-0.08% of Nb2O5, 0.02-0.08% of V2O5, 0.05-0.25% of TiO2, 0.08-0.6% of CO2O3, 0.003-0.10% of ZrO2, 0.04-0.4% of NiO, 0.02-0.10% of MgO, and the like. The manganese/zinc ferrite material disclosed by the invention is mainly used in the fields of home electronics, communications, optoelectronics, automotive electronics and like, and is especially applicable for new fields of electrodeless lamp electromagnetic coupler core markets as well as automotive electronics, strong current, inverter air conditioners, etc. The manganese/zinc ferrite material has the beneficial effects of low power consumption, wide temperature range, high Curie temperature and the like.
Description
Technical field
The invention belongs to ferrite technical field of electronic materials, be specifically related to the high stack of a kind of wide temperature reduce power consumption high-curie temperature MnZn ferrite material and preparation method thereof.
Background technology
Along with constantly developing rapidly of electronics and information 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 world Ge great ferrite company, to adapt to no Application Areas, at convertible frequency air-conditioner, Non-polarized lamp lighting electronic, power electronics, IT industry, communication, under the users' such as domestic electronic requirement, a kind of material that requires has higher BS, better DC superposition characteristic, lower power loss, wider frequency of utilization and wider thermal adaptation scope, higher Curie temperature, therefore, the research of MnZn ferrite material has entered into wide temperature, high DC stacked, high BS, lower power loss field, high-curie temperature field more.Analyze the material that market Shang Ge material manufacturing firm releases, be not difficult to find out that each material producer all seeking a kind of wide temperature, low-loss material, high-curie temperature to replace numerous high-frequency and low-consumption Ferrite Materials.
Being widely used and performance raising of environmental protection electromagnetic induction electrodeless lamp, has promoted continually developing and going into operation of this material, under low frequency 200～300KHZ low and medium frequency state, is widely used.But exist how to take into account under built-in and external two kinds of structures, use Non-polarized lamp efficiency to reach best, require at-40 ℃, to have enough magnetic permeabilities simultaneously, require heating little simultaneously, loss is low; Electronic product always has electric current composition at work on the other hand, for preventing that electronic product is because there being the existence of electric current to affect normal use, therefore also needs material to have enough BS, DC superposition characteristic; Simultaneously under specific environment as envrionment temperature reach 280 ℃ or when higher electron device can also normally work.
As the requirements such as most popular supply transformer, office automation, domestic electronic, communication have wide temperature, low-loss, high magnetic permeability, high DC stacked be indispensable assembly, Non-polarized lamp and vehicle electronics require to change at wide temperature, high-frequency range internal loss and magnetic permeability little, have high stability and high reliability.Vehicle electronics switch power supply is all used conventionally under the occasion of large electric current or DC bias field, and this requirement all needs material to have the difference of enough large saturation magnetic flux density BS and remanent magnetism BR, and superimposed characteristics is good.
The low-loss manganese-zinc power ferrite material of a kind of high saturated BS as disclosed in Chinese patent application (CN101183582A), it particularly adds 2～4mol%Ni0 to obtain being greater than 460T under BS(100 degree by optimization of C/C composites and doping) high frequency power consumption 500KHZ, 50mT, 100 degree under be less than 150KW/m
3, but do not mention broad temperature, broadband and Curie temperature height, thereby it is of limited application.
In Chinese patent application (CN1749209A), disclose a kind of high saturation magnetic flux density, low loss manganese-zinc ferrite material and preparation method thereof in addition, it is by doping and technology controlling and process, obtained 100KHZ, 200mT, 45 ℃ time lower than 245kw/m
3power consumption and 1194A/m, 50mT, saturation magnetic flux density, higher than the result of 535mT, but is not mentioned wide gentle wideband, Curie temperature equally 25 ℃ time, thereby its use range is quite limited.
Summary of the invention
The object that the present invention will reach is that a kind of high initial permeability and suitable 25～140 ℃ of power consumptions that has will be provided, in 25～140 ℃ of temperature ranges, power consumption curve is smooth, remanent magnetism is little, superimposed characteristics is good, under high frequency 500KHZ, 50mT, 100 ℃ of test conditions, power consumption loss is less than 250kw/m3 simultaneously, at 1MHZ, 30mT, the loss of 100 ℃ of test condition power consumptions is less than 400kw/m3, and Curie temperature reaches the soft magnetic ferrite of the 270 ℃ of above high stack of high frequency range temperature low-loss high-curie temperatures.
The technical solution adopted in the present invention is:
Wide temperature low-power consumption high-curie temperature MnZn ferrite material and a preparation method, this ferrite comprises principal constituent and minor component, and described principal constituent comprises ferric oxide, zinc oxide and manganese oxide, and its principal constituent by mass percentage, is calculated with oxide compound: Fe
20
3be that 69.0～72.5%, Zn0 is 6～10%; All the other are Mn
30
4; Fe
20
3, Mn
30
4with Zn0 sum be 100%.
Described minor component comprises calcium oxide, titanium oxide and cobalt/cobalt oxide, barium oxide, Zirconium oxide, niobium oxide, magnesium institute oxide compound etc., relatively described principal constituent total amount, it is 0.5～0.7% that described calcium oxide, titanium oxide and cobalt/cobalt oxide, barium oxide, Zirconium oxide, niobium oxide, magnesium oxide be take its standard substance titanium oxide, barium oxide, cobalt/cobalt oxide, Zirconium oxide, magnesium oxide weight percent content; Described in relatively described principal constituent total amount, minor component is respectively Ca0:0.02～0.07%, Nb with standard weights degree separately
20
5: 0.02～0.08%, V
20
5: 0.02～0.0.08%, Ti0
2: 0.05～0.25%, C0
20
3: 0.08～0.6%, Zr0
2: 0.003～0.10%, Ni0:0.04～0.4%, Mg0:0.02～0.10%
Described minor component comprises wherein at least two kinds of calcium oxide, titanium oxide and cobalt/cobalt oxide, barium oxides, relatively described principal constituent total amount, and these minor components are with its standard C a0, V
20
5, Ti0
2, C0
20
3, Mg0 meter total weight percent content be 0.25～0.5%.
Relatively described principal constituent total amount, in described minor component, calcium oxide, titanium oxide and cobalt/cobalt oxide, barium oxide, nickel oxide are separately with its standard substance Ca0, V
20
5, Ti0
2, C0
20
3, Ni0, Mg0 meter weight percent content be respectively: Ca0:0.02～0.07%, V
20
5: 0.02～0.08%, Ti0
2: 0.05～0.25%, C0
20
3: 0.08～0.6%, Ni0:0.04～0.4%, Mgo:0.02～0.06%.
The present invention is by above-mentioned formula and compound interpolation calcium oxide, titanium oxide and cobalt/cobalt oxide, barium oxide, nickel oxide, magnesium oxide makes described ferrite have 3500 ± 25% initial permeability, and valley point power loss reaches 270kw/m3 in 25～140 ℃ of temperature provinces, TC is greater than 270 ℃, under 500KHZ, 50mT, 100 ℃ of test conditions, power consumption loss is less than 280kw/m3, at 1MHZ, 30mT, the loss of 100 ℃ of test condition power consumptions is less than 480kw/m3.
The preparation method of described material, mainly comprises following content:
1, by three kinds of principal constituent Fe
20
3, Mn
30
4, Zn0 raw material mix after through star sand milling once, make median size and be the principal constituent powder of 0.8～1.15 micron.
2, by described principal constituent powder drying, pre-burning, then add pure water, cementing agent and minor component, then carry out star sand milling for the second time, in secondary star sand grinding process, adding tackiness agent and defoamer to make median size is the principal constituent powder of 0.7～0.9 micron.
3,, by mixed powder drying, compression moulding, 1330～1380 ℃ of insulations 4～6 hours, cooling area is cooling under balanced atmosphere must described FERRITE CORE.
In described step 2 and 3, what described oven dry adopted is electronic box baking method; In described step 3, the green density after described compression moulding is 3.0 ± 0.05g/cm3, and the magnetic core density after described sintering is 4.85 ± 0.05g/cm3; Cobalt/cobalt oxide in described minor component adds with tricobalt tetroxide form.
The present invention is by the principal constituent of optimization and the composite mixed and suitable reduction median size of optimization, increase the activity of material, form uniformly, high conformity, without the microtexture of another phase, by sintering process temperature, the atmosphere curve optimized, form the ferrite that void content is low, density is large simultaneously.
Wide temperature prepared by the present invention, high frequency, high stack, 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 of numerous wide adiabators of high-frequency and low-consumption is most is greater than 220 ℃ for TC, can reach individually 270 ℃ of left and right, some high temperature power consumptions are too high, part very low temperature during as-35 ℃ magnetic permeability too low, Non-polarized lamp cannot start.The appearance that the wide temperature of the present invention, high frequency, high-curie temperature, reduce power consumption have well solved this problem.
On the other hand, the present invention differs low-consumption Mn-Zn ferrite material High-frequency and low-frequency power consumption from too large, the problem that cannot take into account well solve use these analogous products can 500KHZ, two frequencies of 1MHZ can meet user's requirement.
Utilize the magnetic core that the present invention makes to there is following beneficial effect:
3500 ± 25% initial permeability, and valley point power loss reaches 270kw/m3 in 25～140 ℃ of temperature provinces, TC is greater than 270 ℃, under 500KHZ, 50mT, 100 ℃ of test conditions, power consumption loss is less than 280kw/m3, at 1MHZ, 30mT, the loss of 100 ℃ of test condition power consumptions is less than 480kw/m3.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment mono-, by weight percentage, takes 69.5% Fe
20
3, all the other are Mn0 for 6.5% Zn0, wherein Mn0 raw material form is trimanganese tetroxide, source-2, steel sky type in use, its Mn% is greater than 71%, iron oxide red adopts Korea S EG company raw material, purity is greater than 99.3%, zinc oxide is capital, Shanghai, its purity is greater than 99.7%, after above-mentioned raw materials is mixed, drop in sand mill and stir in the lump, controlling median size is 0.7～0.9 micron, after heater case oven dry, at 800 ℃ of temperature, electricity consumption heating revolving kiln carries out pre-burning, 3 hours pre-burning time, after pre-burning, carry out secondary sand milling, 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: Ca0:0.025%, Nb
20
5: 0.02%, V
20
5: 0.02%, Ti0
2: 0.05%, C0
20
3: 0.09%, Zr0
2: 0.003%, Ni0:0.04%, MgO:0.02% control median size is 0.7～0.9 micron, finally carries out secondary spraying and obtains Mn-Zn ferrite particles powder.
Get this particulate material moulding compacting T25 mm * 15 mm * 8 mm toroidal cores and EC4445 magnetic cores; compact density is 3.0 ± 0.05g/cm3; 1100 ℃ of intensification sections, by oxygen level, be that densification is carried out in 1% left and right; 1330 ℃ of nitrogen protection insulations 4 hours, cooling area was undertaken under balanced atmosphere cooling by Blake equation.
Through the prepared magnetic core of said process, through U.S. AW2335A power consumption instrument, TH2828S, TH1775, Japan's reason, grind the instruments such as BHS-40 DC characteristic tester, thermostat container and resistivity tester and record correlation properties at magnetic core as table 1 and table 2.
Embodiment bis-, by weight percentage, take 72% Fe
20
3, all the other are Mn0 for 9.5% Zn0, wherein Mn0 raw material form is trimanganese tetroxide, source-2, steel sky type in use, its Mn% is greater than 71%, iron oxide red adopts Korea S EG iron oxide red, purity is greater than 99.3%, zinc oxide is capital, Shanghai, its purity is greater than 99.7%, after above-mentioned raw materials is mixed, drop in sand mill and stir in the lump, controlling median size is 0.7～0.9 micron, after heater case oven dry, at 1000 ℃ of temperature, electricity consumption heating revolving kiln carries out pre-burning, 4.5 hours pre-burning time, after pre-burning, carry out secondary sand milling, in sand grinding process, add pure water, dispersion agent, defoamer, and add additive, relatively described principal constituent total amount, in described additive, the weight percent content of each material respectively: Ca0:0.07%, Nb
20
5: 0.078%, V
20
5: 0.08%, Ti0
2: 0.25%, C0
20
3: 0.6%, Zr0:0.1%, Ni0:0.4%, MgO:0.1% control median size are 0.7～0.9 micron, finally carry out secondary spraying and obtain Mn-Zn ferrite particles powder.
Get this particulate material moulding compacting T25mm*15mm*8mm toroidal core and EC4445 magnetic core; compact density is 3.0 ± 0.05g/cm3; 1250 ℃ of intensification sections, by oxygen level, be that densification is carried out in 1% left and right; 1355 ℃ of nitrogen protection insulations 6 hours, cooling area was undertaken under balanced atmosphere cooling by Blake equation.
Embodiment tri-, by weight percentage, take 70% Fe
20
3, all the other are Mn0 for 9% Zn0, wherein Mn0 raw material form is trimanganese tetroxide, source-2, steel sky type in use, its Mn% is greater than 71%, iron oxide red adopts Korea S EG iron oxide red, purity is greater than 99.3%, zinc oxide is capital, Shanghai, its purity is greater than 99.7%, after above-mentioned raw materials is mixed, drop in sand mill and stir in the lump, controlling median size is 0.7～0.9 micron, after heater case oven dry, at 1000 ℃ of temperature, electricity consumption heating revolving kiln carries out pre-burning, 4.5 hours pre-burning time, after pre-burning, carry out secondary sand milling, in sand grinding process, add pure water, dispersion agent, defoamer, and add additive, relatively described principal constituent total amount, in described additive, the weight percent content of each material respectively: Ca0:0.03%, Nb
20
5: 0.05%, V
20
5: 0.02%, Ti0
2: 0.07%, C0
20
3: 0.2%, Zr0:0.07%, Ni0:0.35%, MgO:0.05% control median size are 0.7～0.9 micron, finally carry out secondary spraying and obtain Mn-Zn ferrite particles powder.
Get this particulate material moulding compacting T25mm*15mm*8mm toroidal core and EC4445 magnetic core; compact density is 3.0 ± 0.05g/cm3; 1150 ℃ of intensification sections, by oxygen level, be that densification is carried out in 1% left and right; 1340 ℃ of nitrogen protection insulations 5 hours, cooling area was undertaken under balanced atmosphere cooling by Blake equation.
Through the prepared magnetic core of said process, by U.S. AW2335A power consumption instrument, with favour TH2828S, grind the instruments such as BHS-40 DC characteristic tester, thermostat container and resistivity tester with favour TH1775, Japan reason and record correlation properties at magnetic core as table 1 and table 2.
Table 1 toroidal core material property of the present invention
The superimposed characteristics that EC4445 is example is take in table 2 the present invention
From table 1 and table 2, ferrite in manganese zinc series material of the present invention, by principal constituent and minor component are adjusted, is specially Ti0
2and C0
30
4the reinforcement of hybrid compensation effect, wide temperature characteristics is obvious; Doping system adds the raising of using TC as Ni0, add MgO that the physical strength of product is improved, atmosphere control simultaneously and densification process are used this material to have higher initial permeability, and the power dissipation ratio in 25～140 ℃ of temperature provinces is more smooth, and 100 ℃ of power consumptions are less than 270 mw/cm
3, high frequency power consumption is lower, DC stacked good, and Curie temperature is greater than 270 ℃.
Claims (3)
1. wide temperature low-power consumption high-curie temperature MnZn ferrite material, is characterized in that, its principal constituent is pressed the mass percent of material, calculates: Fe with oxide compound
20
3be that 69.5～72%, Zn0 is 6.5～9.5%; All the other are Mn
30
4; Fe
20
3, Mn
30
4with Zn0 sum be 100%;
Additive by mass percentage, calculates with oxide compound: Ca0:0.025～0.07%, Nb
20
5: 0.02～0.078%, V
20
5: 0.02～0.08%, Ti0
2: 0.05～0.25%, C0
20
3: 0.09～0.6%, Zr0
2: 0.003～0.10%, Ni0:0.04～0.4%, Mg0:0.02～0.10%.
2. the preparation method of wide temperature low-power consumption high-curie temperature MnZn ferrite material, comprises the following steps:
1) Fe, by mass percentage,
20
3be that 69.0～72.5%, Zn0 is 6.5～9.5%, surplus is Mn
30
4, with star ball mill, mix;
2), the powder of described step 1) gained is carried out at 800～1000 ℃ to pre-burning; Soaking time is 3～4.5 hours;
3), by described step 2) powder of gained adds following additive in mass ratio:
Ca0:0.02～0.07%, Nb
20
5: 0.02～0.08%, V
20
5: 0.02～0.0.08%, Ti0
2: 0.05～0.25%, C0
20
3: 0.08～0.6%, Zr0
2: 0.003～0.10%, Ni0:0.04～0.4%, Mg0:0.02～0.10%, and carry out star ball milling for the second time, make the flat uniform grading of powder after ball milling reach 0.85 left and right micron;
4), the secondary star ball milling material of described step 3) gained is dried after granulation, moulding, make standard green compact sample;
5), the bad sample of life of described step 4) gained is carried out to sintering in nitrogen protective sintering kiln.
3. the preparation method of wide temperature low-power consumption high-curie temperature MnZn ferrite material as claimed in claim 2, it is characterized in that, described step 4): the powder of described step 3) gained is added in mass ratio to 8～10% PVA organic binder bond, and mix, after granulation, on 16 tons of press of testing laboratory, powder pressing is become to sample blank, described step 5) is: the blank of described step 4) obtained by molding is placed on and in nitrogen protective sintering kiln, carries out sintering, 1100～1250 ℃ of intensification sections, by oxygen level, be that densification is carried out in 1% left and right, 1330～1355 ℃ of insulations 4～6 hours, in holding-zone oxygen partial pressure, be 4～6%, temperature descending section is balanced atmosphere sintering.
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Application publication date: 20140730 |