CN101620907A - Broad temperature low standby power consumption FPT type soft magnetic ferrite and preparation method thereof - Google Patents

Broad temperature low standby power consumption FPT type soft magnetic ferrite and preparation method thereof Download PDF

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CN101620907A
CN101620907A CN200910033030A CN200910033030A CN101620907A CN 101620907 A CN101620907 A CN 101620907A CN 200910033030 A CN200910033030 A CN 200910033030A CN 200910033030 A CN200910033030 A CN 200910033030A CN 101620907 A CN101620907 A CN 101620907A
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power consumption
fpt
auxiliary element
standby power
oxygen
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CN101620907B (en
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石炎
刘九皋
王修炜
顾骏
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NANJING FINEMAG TECHNOLOGY Co Ltd
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NANJING FINEMAG TECHNOLOGY Co Ltd
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Abstract

The invention discloses a broad temperature low standby power consumption FPT type soft magnetic ferrite and a preparation method thereof. The composition calculated by content of oxides is as follows: 52-55mol% of Fe2O3, 7-10mol% of ZnO and the balance of MnO; a first auxiliary component comprises 0.01wt%-0.1wt% of CaO and 0.005wt%-0.02wt% of SiO2; a second auxiliary component comprises one or more of V2O5, Nb2O5, Ta2O5, ZrO2 and K2O, the content is 0-0.2wt% by calculation, and a third auxiliary component comprises 0.05-1wt% of TiO2 and 0.05-1wt% of Co2O3. Pre-burning under the protection of nitrogen, sintering, the control of cooling atmosphere and the densification process are carried out, thereby leading the power consumption PCV of a magnetic core at 100kHz and 200mT within the temperature of 25 DEG C-120 DEG C to be respectively less than 400kw/m<3> and 350kw/m<3>, and a time stability indicator thereof which is a disaccommodation factor Df is less than 2*10<-6>.

Description

Broad temperature low standby power consumption FPT type soft magnetic ferrite and preparation method thereof
Technical field
The present invention relates to a kind of broad temperature low standby power consumption FPT type soft magnetic ferrite and preparation method thereof, belong to the ferrite magnetic material technical field.
Background technology
Main branch---the soft magnetic ferrite of high-new magnetic material, be a kind of development basic function material very rapidly, be widely used in all departments that IT industry, auto industry, aerospace field, traffic and transportation sector, naval vessel and national defence weapon change system etc. almost spread all over national economy.For making the said equipment system high efficiency, stable, reliability service, the material electromagnetic property must effectively be controlled with variation of temperature, just can meet the standard of zero tolerance.The outdoor facilities of modern communications equipment, as repeater, repeater, microwave relay station, submarine cable, optical cable underwater installation etc. under unattended situation, must guarantee the tolerance harsh and unforgiving environments, decades failsafe.This just requires employed components and parts to have the good characteristic of wide temperature, low-power consumption, long-life, high stability.
For reaching above purpose, each big ferrite company of the world falls over each other to develop, and has successively released various readily marketable products, to satisfy the needs of different purposes.As TDK company, with power consumption P CVBe improvement direction, recent two decades comes, and materials such as PC30-PC40-PC44-PC45,46-PC47 have successively been released in generations of improvement, and the power consumption number of valley point temperature is from initial 600kw/m 3Gradually be reduced to 410kw/m 3, 300kw/m 3, until 250kw/m 3Unfortunately the normal temperature power consumption does not but have much changes, and minimum remains at 600kw/m 3About.Normal temperature is the temperature of all watch-dogs, the long-time holding state of instrument appliance, if its power consumption can not reduce, the energy quantity of waste is surprising.Data shows that only in Germany, annual standby operation power loss just reaches about 20,000,000,000 KWh, and this has been equivalent to the electricity needs in 1 year in Berlin city.The U.S. has also issued corresponding rules, and limiting time lowers stand-by power consumption.At this global heat subject, German EPCOS company (former Siemens ferrite) has released the novel N51 Ferrite Material that can reduce the Switching Power Supply stand-by power consumption in June, 2006, though regrettably this material is pressed onto the normal temperature power consumption less than 407kw/m 3, but high temperature sticks up 700kw/m 3Gone, promptly the high temperature power consumption is still violated the common fault of the PC45 of TDK company, PC46 material.
The invention enables 25 ℃～100 ℃ wide temperature range P CVAll less than 400kw/m 3, subtract the factor D that falls F＜2 * 10 -6, guaranteed magnetic core long-life work and be unlikely to premature failure; This material can reach wide temperature at bell jar stove sintering and be lower than 350kw/m 3Index, make that its manufacturing cost is lower, quality is higher, have favorable social and economic benefits, table 1 is produced level and N51 material property in batches relatively for the present invention.
Table 1
Figure G2009100330301D00021
Chinese patent application (CN1749209A) discloses a kind of high saturation magnetic flux density, low loss manganese-zinc ferrite material and preparation method thereof, and it is lower than 245kw/m by mixing and technology controlling and process when having obtained 100kHz 200mT45 ℃ 3Power consumption and during 25 ℃ of 1194A/m 50mT saturation flux density be higher than the result of 535mT, but avoided the introduction of hot properties, obviously its scope of application is quite limited.
Chinese patent application (CN1810710A) discloses manganese-zinc ferrite of a kind of wide temperature and higher magnetic permcability and preparation method thereof for another example, though reached the wide temperature low-power consumption purpose, but to being used for the time stability that communications field emphasis is considered---than not research of disaccommodation factor, thereby also limited its scope of application.
Summary of the invention
FPT wide temperature low-power consumption ferrite of the present invention is compared with the conventional power ferrite, has the characteristics of power consumption equilibrium in higher magnetic permeability, the wideer serviceability temperature scope, has also improved the time stability index especially and has subtracted the factor D that falls FIndex makes the user to the clear and definite estimation of component failure life-span energy.The normal temperature power consumption has reduced by 30% when especially being in holding state, and when being used for LCD backlight electric power converter and POP power transformer, it is about 25% that its energy conversion efficiency improves, and volume then reduces 1/3; When being used for automotive electronics, vary in size when causing temperature significantly to change when driving the load action, this wide temperature low-power consumption core material can be made contributions to miniaturization, car body lightweight and the energy savings of automobile power source as first-selection.PC40, the PC44 that this material and Japanese TDK company produce, PC47 power ferrite material relatively, initial permeability μ iImproved 30%, the normal temperature power consumption has reduced by 30%; The N51 low standby power loss ferrite new material of not long ago releasing with German EPCOS company relatively, high temperature power consumption (operating state) reduces by 40%, saturation flux density improves 8%.Also improve time stability index ratio simultaneously and subtracted the factor D that falls F＜2 * 10 -6, i.e. the fluctuation of magnetic core inductance value, 20 years afterwards less than 1%.
For guaranteeing the realization of above excellent properties, effective measures have been taked at the technical matters aspects.As everyone knows, the characteristics of MnZn ferrite material are exactly magnetocrystalline anisotropy constant K 1Has extremely strong temperature dependency, its K 1-T characteristic, just K 1Value all has positive and negative variation usually with the variation of temperature curve and passes the form at zero point.Near the initial permeability μ of material zero point iHas maximum and power consumption P CVAll has minimum.This is because μ iWith K 1Relation near inverse ratio is arranged, and anisotropy constant (K 1) and magnetostriction constant (λ S) magnetic core total losses minimum when trending towards zero.The temperature spot of corresponding this extreme value is called the valley point of power consumption.The key problem in technology of wide adiabator is exactly to wish the characteristic of valley point is extended to the total temperature section, just makes K 1-T curve and μ i-T song.
Present desired temperature range is mild as far as possible, avoids bimodal form to occur.This just requires preferred principal component Fe 2O 3, Mn 3O 4, ZnO three's proportioning except that guaranteeing the basic magnetic characteristic of material, must be sought the 4th metal ion species, control magnetocrystalline anisotropy constant K 1Temperature characterisitic, the major part magnetic hysteresis loss of core loss is reduced at wide temperature range, simultaneously by the interpolation of various micro constitutents and the best fit of material sintering temperature, atmosphere and cooling rate, reach the purpose of control ferrite microstructure, crystallite dimension, vacancy concentration and macroscopical density, thereby reduce eddy current loss and aftereffect loss.Its innovative point is: be used for changing μ-T, K 1The 4th metal ion species (Co of-T characteristic 3+Or Ti 4+) negative effect that brings must seek effective trace element and neutralize with it or water down so that eliminate; Desire to reach the electromagnetic performance of comprehensive excellence of wide temperature low-power consumption, also must meticulous adjustment preheating, binder removal, sintering, the atmosphere cooling off each section temperature curve and adapt to it, such as preliminary grinding adds calcium, inferior mill adds cobalt and other anti-oxidant measure etc.Calcium carbonate adds when the rouge and powder sand milling, is decomposed into calcium oxide after pre-burning, and is water-soluble in black powder slurry like this, can fully disperse with the calcium hydroxide form, and stronger with additive silicic acid affinity.And for cobalt oxide, if add in a sand milling, Part of Co in pre-burning and the cooling procedure 2+Can be oxidized to Co 3+Thereby, with the Co of surplus 3O 4(spinel structure) form and CoFe 2O 4Altogether molten, Co wherein 3O 4Only under 1400 ℃ of high temperature or 1200 ℃ of strongly reducing atmospheres, could decompose, can cause the Ferrite Material existence mistake cobalt in various degree after burning till like this, uncontrollable composite material K 1Compensation effect, influence μ-T form, Co in addition 3O 4Common moltenly also can cause magnetic permeability μ iDescend.So must take secondary to add the cobalt measure.
Broad temperature low standby power consumption FPT type soft magnetic ferrite of the present invention and magnetic core, what be different from the common power Ferrite Material is to have increased the time stability index to subtract the factor D that falls FOne, make the user to the clear and definite estimation of component failure life-span energy.Such as, FPT materials processing becomes effective permeability μ eBe 2000 transformer magnetic core, the user winds the line, assembles, is aged to installation, if whole process two months, so after 200 months, being changed to relatively of magnetic core winding electric sensibility reciprocal:
&Delta;L L = &Delta;&mu; &mu; = D . F &CenterDot; &mu; e &CenterDot; lg 200 2 = 2 &times; 10 - 6 &times; 2000 &times; 2 = 8 &times; 10 - 3
After promptly 16 years (200 months), its variable quantity only is 8 * 10 -3, this just requires to take measures in prescription and technology, strict control Fe 2+Ion concentration and O 2-The ion vacancy concentration, the partial pressure of oxygen of further preferred additive and sintering cooling atmosphere.Result of study shows, subtract and drop on that two peak values also can appear in similar μ-T curve between-20～+ 50 ℃, one near-20～+ 20 ℃, another appears near 20～60 ℃, and the height of these two peak values and the temperature value of peak value occurs, be subjected to the influence of composition, doping and firing atmosphere of basic recipe very big.Universal law is: Mn 3O 4Content is fixed, Fe 2O 3The normal temperature D that content is big FValue is big, along with Fe 2O 3The increase of content, near the peak value 40 ℃ increases and moves to the normal temperature direction; In addition, at Fe 2O 3Under the little situation of content, normal temperature D FAlso increase, this be because near the peak value 0 ℃ along with Fe 2O 3Minimizing and move to the normal temperature direction, thereby also cause normal temperature D FIncrease.So at Mn 3O 4Content one regularly must have a best Fe 2O 3Content makes normal temperature D FValue is minimum.If Fe 2O 3Content is fixed, and changes Mn 3O 4Content, its result just in time with change Fe 2O 3The situation of content is opposite.Add impurity SnO 2Can make normal temperature D FValue diminishes, TiO 2, Ta 2O 5, Co 2O 3With SnO 2Act on identically, act on the opposite Li that has 2O, Na 2O, MgO etc.The interpolation of above plurality of impurities can effectively improve the magnetism of material energy, as μ-T, and D F-T, P Cv-T characteristic makes temperature factor α μ, subtract the factor D that falls F, volume power consumption P CvMinimum.
Technical problem to be solved by this invention is that a kind of broad temperature low standby power consumption FPT type soft magnetic ferrite and preparation method thereof is provided.
The technical solution adopted for the present invention to solve the technical problems is as follows:
A kind of broad temperature low standby power consumption FPT type soft magnetic ferrite, its principal phase is the spar structure, it is characterized in that principal component content is calculated as with oxide: Fe 2O 3Be 52～55mol%; ZnO is 7～9mol%; All the other are MnO; Fe wherein 2O 3Preferably ratio is 53～54mol%, and ZnO is 8～9mol%; All the other are MnO.
The first auxiliary element content that adds is calculated as with oxide: CaO is 0.01wt%～0.1wt%; SiO 2Be 0.005wt%～0.02wt%;
Second auxiliary element that adds is one or more in the following oxide: V 2O 5, Nb 2O 5, Ta 2O 5, ZrO 2, K 2O, each impurity content calculates with oxide and is respectively 0～0.2wt% in second auxiliary element of interpolation, and the total amount of described second auxiliary element adds up to and is less than or equal to 0.3wt%;
The 3rd auxiliary element content that adds is calculated as with oxide: TiO 2Be 0.05～1wt%; , Co 2O 3Be 0.05～1wt%.
The preparation method of a kind of broad temperature low standby power consumption FPT type soft magnetic ferrite of the present invention, its technology comprises the steps:
1), raw-material mixing:
With prepare by 52～55mol%Fe 2O 3, 7～9mol%ZnO, principal component that all the other are formed for MnO and by 0.01wt%～0.1wt%CaCO 3, 0.005wt%～0.02wt%SiO 2First auxiliary element of forming is put into ball mill, the deionized water of weight such as adding, ball milling 1～3 hour;
2), pre-burning:
The material oven dry that above-mentioned mix grinding is good, send into pre-firing pre-burning again, the calcined temperature scope is 900～1050 ℃, and temperature retention time is 2～4 hours, and atmosphere is air, pre-firing cooling area feeds nitrogen, cooling atmosphere control oxygen content makes pre-imitation frosted glass powder magnetization degree less than 1% below 5%, prevents that peroxidating and quenching phenomenon from taking place, in order to avoid the magnetic core properties of product are inferior, embrittlement, cracking, cause qualification rate to reduce;
3), impurity adds:
Select for use by 0～0.2wt%V 2O 5, 0～0.2wt%Nb 2O 5, 0～0.2wt%Ta 2O 5, 0～0.2wt%ZrO 2, 0～0.2wt%K 2Second auxiliary element of one or more compositions among the O and by 0.05～1wt%TiO 2, 0.05～1wt%Co 2O 3The 3rd auxiliary element of forming is united interpolation as additive, and wherein the total content of second auxiliary element is less than or equal to 0.3wt%;
4) secondary ball milling:
Pre-imitation frosted glass and additive are put into ball mill, the deionized water of weight such as adding, ball milling 8 hours, the particle mean size that makes slip is less than 1.2 μ m;
5) forming and sintering:
With the slurry oven dry, add the 10wt% ingredients by weight, concentration is 9% polyvinyl alcohol solution, evenly mixes, and uses 45 order sub-sieve granulations, and compression moulding, puts into bell jar stove sintering, the control of sintering process temperature is as follows:
Temperature rise period: programming rate per hour about 150 ℃, to 800 ℃, carries out in the air atmosphere, takes the air blast discharging, the about 100m of flow velocity 3/ h, the accelerating impurity volatilization in case adhesive residue causes pore, guarantees that effectively product magnetic and density improve.
Per hour about 250 ℃, partial pressure of oxygen is 0.005% to programming rate between 800 ℃ to 1200 ℃;
1200 ℃ to 1250 ℃ heating-up times are 1 hour, and pre-incubation is 1 hour again, and partial pressure of oxygen is 0.5～1%;
Heating up between 1250 ℃ to 1370 ℃ is 1 hour, and partial pressure of oxygen is 1～3%;
Holding stage: be incubated 2～6 hours about 1370 ℃, partial pressure of oxygen is 2～8%;
Temperature-fall period: per hour about 150 ℃, partial pressure of oxygen switches to about 0.5～2% cooling rate between 1370 ℃ to 1250 ℃; 1250 ℃ down cooling rate drop to about 150 ℃ and come out of the stove per hour about 250 ℃, whole process is kept equilibrium oxygen partial pres-sure about about 0.2～0.01%.
The technology of the present invention process characteristic is:
1, in the ferritic prescription of FPT wide temperature low-power consumption, adjusted Fe especially 2O 3, Mn 3O 4, ZnO three's ratio with synthetic desirable μ-T curve, is improved B S, B rAnd temperature characterisitic, add the 4th kind of metal oxide Co again 2O 3Or TiO 2, move and pressing μ-T two peaks, also utilize effective additive attenuating loss and water down Co 3+, Ti 4+Intensify effect, and notice that preliminary grinding adds calcium, inferior mill adds the order of cobalt, thereby obtains the wide temperature low-power consumption material of excellent performance;
2, improve nitrogen kiln, pre-firing and controlled atmospher comprehensively, can closs packing, the low-cost FPT wide temperature low-power consumption FERRITE CORE of producing in batches, make 25 ℃～100 ℃ wide temperature range P CVAll less than 400kw/m 3, subtract the factor D that falls F＜2 * 10 -6, guaranteed magnetic core long-life work and be unlikely to premature failure; This material can reach wide temperature at bell jar stove sintering and be lower than 350kw/m 3Index, make that its manufacturing cost is lower, quality is higher, have favorable social and economic benefits;
3, broad temperature low standby power consumption FPT type soft magnetic ferrite of the present invention and magnetic core, the normal temperature power consumption has reduced by 30% when being in holding state, when being used for LCD backlight electric power converter and POP power transformer, it is about 25% that its energy conversion efficiency improves, and volume then reduces 1/3; When being used for automotive electronics, vary in size when causing temperature significantly to change when driving the load action, this wide temperature low-power consumption core material can contribute to miniaturization, car body lightweight and the energy savings of automobile power source as first-selection.
Description of drawings
Fig. 1 is FPT material of the present invention and different materials PCV～T curve comparison diagram.
Fig. 2 is the measured performance figure of FPT material of the present invention.
Embodiment
Embodiment 1
Raw-material selection:
Commercially pure Fe 2O 3, the above V of ZnO, MnO and chemical pure 2O 5, Nb 2O 5, Ta 2O 5, ZrO 2, K 2CO 3, SnO 2, TiO 2, Co 2O 3Deng;
The design of components of the broad temperature low standby power consumption FPT type soft magnetic ferrite of example 1 of the present invention:
The main component content of Ferrite Material is calculated as with oxide: Fe 2O 3For 53.5mol%, ZnO are 7.5mol%, all the other are MnO; First adds auxiliary calculating with oxide comprises: SiO 2Be 100ppm (0.01wt%); CaO is 700ppm (0.07wt%); Second auxiliary element that adds calculates with oxide and comprises: V 2O 5Be 300ppm (0.03wt%), Nb 2O 5Be 150ppm (0.015wt%); The 3rd auxiliary element content that adds is calculated as with oxide: TiO 2Be 1000ppm (0.1wt%); Co 2O 3Be 2000ppm (0.2wt%).
The preparation method of broad temperature low standby power consumption FPT type soft magnetic ferrite of the present invention, its technology comprises the steps:
1), raw-material mixing:
With aforementioned prepare by Fe 2O 3, the principal component formed of ZnO, MnO and by CaCO 3, SiO 2First auxiliary element of forming is put into ball mill, the deionized water of weight such as adding, ball milling 2 hours;
2), pre-burning:
Pre-burning in the stove is sent in the raw material oven dry that above-mentioned mix grinding is good, and the calcined temperature scope is 980 ℃, and temperature retention time is 2 hours, and atmosphere is air, and pre-firing cooling area feeds nitrogen, and cooling atmosphere control oxygen content makes the powder magnetization degree less than 1% below 5%;
3), impurity adds:
With the aforesaid second auxiliary element (V 2O 5Be 300ppm, Nb 2O 5Be 150ppm), the 3rd auxiliary element (TiO 2Be 1000ppm, Co 2O 3Be 2000ppm) unite interpolation for additive;
4) secondary ball milling:
Material is put into ball mill, the deionized water of weight such as adding, ball milling 8 hours, the particle mean size that makes pre-imitation frosted glass is less than 1.2 μ m;
5) forming and sintering:
With the slurry oven dry, the adding ingredients by weight is that the concentration of 10wt% is 9% polyvinyl alcohol solution (PVA), evenly mixes, and uses 45 order sub-sieve granulations, and compression moulding, puts into bell jar stove sintering, and the control of sintering process temperature is as follows:
Temperature rise period: programming rate per hour about 150 ℃, to 800 ℃, carries out in the air atmosphere, takes the air blast discharging, the about 100m of flow velocity 3/ h;
Per hour about 250 ℃, partial pressure of oxygen is 0.005% to programming rate between 800 ℃ to 1200 ℃;
1200 ℃ to 1250 ℃ heating-up times are 1 hour, and pre-incubation is 1 hour again, and partial pressure of oxygen is 0.5～1%;
Heating up between 1250 ℃ to 1370 ℃ is 1 hour, and partial pressure of oxygen is 1～3%;
Holding stage: be incubated 2～6 hours about 1370 ℃, partial pressure of oxygen is 2～8%;
Temperature-fall period: per hour about 150 ℃, partial pressure of oxygen switches to about 0.5-2% cooling rate between 1370 ℃ to 1250 ℃; 1250 ℃ down cooling rate drop to about 150 ℃ and come out of the stove per hour about 250 ℃, whole process is kept about the about 0.2-0.01% of equilibrium oxygen partial pres-sure.
Embodiment 2
Raw-material selection:
Commercially pure Fe 2O 3, the above V of ZnO, MnO and chemical pure 2O 5, Nb 2O 5, Ta 2O 5, ZrO 2, K 2CO 3, SnO 2, TiO 2, Co 2O 3Deng;
The design of components of the broad temperature low standby power consumption FPT type soft magnetic ferrite of example 2 of the present invention:
The main component content of Ferrite Material is calculated as with oxide: Fe 2O 3For 54mol%, ZnO are 8mol%, all the other are MnO; First adds auxiliary calculating with oxide comprises: SiO 2Be 50ppm (0.005wt%); CaO is 500ppm (0.05wt%); Second auxiliary element that adds calculates with oxide and comprises: Ta 2O 5Be 150ppm (0.015wt%), Nb 2O 5Be 200ppm (0.02wt%), ZrO 2Be 300ppm (0.03wt%); The 3rd auxiliary element content that adds is calculated as with oxide: TiO 2Be 500ppm (0.05wt%); Co 2O 3Be 5000ppm (0.5wt%).
The preparation method of the broad temperature low standby power consumption FPT type soft magnetic ferrite of example 2 of the present invention, its technology comprises the steps:
1), raw-material mixing:
With aforementioned prepare by Fe 2O 3, the principal component formed of ZnO, MnO and by CaCO 3, SiO 2First auxiliary element of forming is put into ball mill, the deionized water of weight such as adding, ball milling 2 hours; The calcium that adds, silicon ion form the calcium silicates barrier layer in the place's segregation of Mn-Zn ferrite crystal boundary, can improve the grain boundary resistance rate and significantly reduce eddy current loss for increasing grain boundary resistance with the containment eddy current;
2), pre-burning:
The raw material oven dry that mix grinding in the step 1) is good, put into the stove pre-burning again, calcined temperature is 980 ℃, the pre-burning time is about 2 hours, pre-burning atmosphere is air, and pre-firing cooling area feeds nitrogen, and the control oxygen content is below 5%, make material carry out pre-burning under nitrogen protection, its powder magnetization degree is less than 1%;
3), impurity adds:
With the aforesaid second auxiliary element (Ta 2O 5Be 150ppm, Nb 2O 5Be 200ppm, ZrO 2Be 300ppm, the 3rd auxiliary element (TiO 2Be 500ppm; Co 2O 3Be 5000ppm) unite interpolation as additive;
4) secondary ball milling:
Material is put into ball mill, the deionized water of weight such as adding, ball milling 8 hours, the particle mean size that makes pre-imitation frosted glass is less than 1.2 μ m;
5) forming and sintering:
With the slurry oven dry, the adding ingredients by weight is that the concentration of 10wt% is 9% polyvinyl alcohol solution (PVA), evenly mixes, and uses 45 order sub-sieve granulations, and compression moulding, puts into bell jar stove sintering, and the control of sintering process temperature is as follows:
Temperature rise period: programming rate per hour about 150 ℃, to 800 ℃, carries out in the air atmosphere, takes the air blast discharging, the about 100m of flow velocity 3/ h;
Per hour about 250 ℃, partial pressure of oxygen is 0.005% to programming rate between 800 ℃ to 1200 ℃;
1200 ℃ to 1250 ℃ heating-up times are 1 hour, and pre-incubation is 1 hour again, and partial pressure of oxygen is 0.5～1%;
Heating up between 1250 ℃ to 1370 ℃ is 1 hour, and partial pressure of oxygen is 1～3%;
Holding stage: be incubated 2～6 hours about 1370 ℃, partial pressure of oxygen is 2～8%;
Temperature-fall period: per hour about 150 ℃, partial pressure of oxygen switches to about 0.5-2% cooling rate between 1370 ℃ to 1250 ℃; 1250 ℃ down cooling rate drop to about 150 ℃ and come out of the stove per hour about 250 ℃, whole process is kept about the about 0.2-0.01% of equilibrium oxygen partial pres-sure.
The electromagnetic performance test result of above-mentioned two example sintered samples sees Table 2.
Table 2
Electromagnetic performance Test condition Example 1 Example 2
Initial permeability μ i Frequency: 10kHz ??3350 ??3510
Than disaccommodation factor D F×10 -6 10 minutes-100 minutes, with surveying μ i ??1.6 ??1.8
Curie temperature Tc (℃) With surveying μ i ??235 ??230
Saturation flux density Bs (mT) ??1194A/m，50Hz，100℃ ??420 ??425
Power consumption (Pcv kw/m 3) ??100kHz，200mT，25℃ ??350 ??345
Power consumption (Pcv kw/m 3) ??100kHz，200mT，60℃ ??347 ??326
Power consumption (Pcv kw/m 3) ??100kHz，200mT，100℃ ??330 ??295
Power consumption (Pcv kw/m 3) ??100kHz，200mT，120℃ ??360 ??355
Density (kg/m 3) ??25℃ ??4.9 ??4.9
Can find out from comparison example: with Fe 2O 3Content increases, and saturation flux density Bs rises, and rises but initial permeability μ with the minimizing Curie temperature Tc of ZnO content iDescend; With TiO 2And Co 2O 3Unite the reinforcement of mending the reward effect, wide temperature characteristics improves; Doping system has been guaranteed the balance and the reduction of low-and high-frequency power consumption; The effect that technologies such as atmosphere control and pre-incubation improve density of material is obvious.
Above-mentioned specific embodiment only is that the present invention's spirit is described in further detail, but the present invention is not limited to given example.The technical staff of the technical field of the invention can make various modification or replenishes or adopt similar fashion to substitute described instantiation, but can't depart from spirit of the present invention or surmount the scope of appended claims definition.

Claims (6)

1, a kind of broad temperature low standby power consumption FPT type soft magnetic ferrite, its principal phase is a spinel structure, it is characterized in that principal component content is calculated as with oxide: Fe 2O 3Be 52～55mol%; ZnO is 7～9mol%; All the other are MnO;
The first auxiliary element content that adds is calculated as with oxide: CaO is 0.01wt%～0.1wt%; SiO 2Be 0.005wt%～0.02wt%;
Second auxiliary element that adds is one or more in the following oxide: V 2O 5, Nb 2O 5, Ta 2O 5, ZrO 2, K 2O, addition calculate with oxide and are respectively 0～0.2wt%, and the total amount of described second auxiliary element adds up to and is less than or equal to 0.3wt%;
The 3rd auxiliary element content that adds is calculated as with oxide: TiO 2Be 0.05～1wt%; , Co 2O 3Be 0.05～1wt%.
2, broad temperature low standby power consumption FPT type soft magnetic ferrite according to claim 1 is characterized in that, the principal component preferred content is calculated as with oxide: Fe 2O 3Be 53～54mol%, ZnO is 7～9mol%; All the other are MnO.
3, a kind of preparation method of broad temperature low standby power consumption FPT type soft magnetic ferrite, its technology comprises the steps:
1), raw-material mixing:
With prepare by 52～55mol%Fe 2O 3, 7～9mol%ZnO, principal component that all the other are formed for MnO and by 0.01wt%～0.1wt%CaCO 3, 0.005wt%～0.02wt%SiO 2First auxiliary element of forming is put into ball mill, the deionized water of weight such as adding, ball milling 1～3 hour;
2), pre-burning:
Pre-firing pre-burning is sent in the raw material oven dry that above-mentioned mix grinding is good again, and the calcined temperature scope is 900～1050 ℃, temperature retention time is 2～4 hours, and pre-burning atmosphere is air, and pre-firing cooling area feeds nitrogen, cooling atmosphere control oxygen content makes pre-imitation frosted glass powder magnetization degree less than 1% below 5%;
3), impurity adds:
Select for use by 0～0.2wt%V 2O 5, 0～0.2wt%Nb 2O 5, 0～0.2wt%Ta 2O 5, 0～0.2wt%ZrO 2, 0～0.2wt%K 2Second auxiliary element of one or more compositions among the O and by 0.05～1wt%TiO 2, 0.05～1wt%Co 2O 3The 3rd auxiliary element of forming is united interpolation as additive, and wherein the total content of second auxiliary element is less than or equal to 0.3wt%;
4) secondary ball milling:
Pre-imitation frosted glass powder and additive are put into ball mill, the deionized water of weight such as adding, ball milling 8 hours, the particle mean size that makes slurry is less than 1.2 μ m;
5) forming and sintering:
With the slurry oven dry, the concentration that adds the 10wt% ingredients by weight is 9% poly-vinyl alcohol solution, evenly mixes, and uses 45 order sub-sieve granulations, and compression moulding, puts into bell jar stove sintering, and the control of sintering process temperature is as follows:
Temperature rise period: programming rate per hour about 150 ℃, to 800 ℃, carries out in the air atmosphere, takes the air blast discharging, the about 100m of flow velocity 3/ h;
Per hour about 250 ℃, partial pressure of oxygen is 0.005% to programming rate between 800 ℃ to 1200 ℃;
1200 ℃ to 1250 ℃ heating-up times are 1 hour, and pre-incubation is 1 hour again, and partial pressure of oxygen is 0.5～1%;
Heating up between 1250 ℃ to 1370 ℃ is 1 hour, and partial pressure of oxygen is 1～3%;
Holding stage: be incubated 2～6 hours about 1370 ℃, partial pressure of oxygen is 2～8%;
Temperature-fall period: per hour about 150 ℃, partial pressure of oxygen switches to about 0.5～2% cooling rate between 1370 ℃ to 1250 ℃; 1250 ℃ down cooling rate drop to about 150 ℃ and come out of the stove per hour about 250 ℃, whole process is kept equilibrium oxygen partial pres-sure about about 0.2～0.01%.
4, the broad temperature low standby power consumption FPT type MnZn ferrite material of claim 1～3, except that preferred main formula with mixing, also necessary meticulous adjustment pre-burning and sintering cooling atmosphere, control densification process, product density is improved, thereby further increase saturation flux density Bs, at 1194A/m, 50Hz, saturation flux density Bs is greater than 420mT under 100 ℃ of test conditions.
5, any broad temperature low standby power consumption FPT type MnZn ferrite material of claim 1～3 demagnetized back 10 minutes and 100 minutes test initial permeability μ iVariation, its than disaccommodation factor less than 2.0 * 10 -6
6, any broad temperature low standby power consumption FPT type MnZn ferrite material of claim 1～3 is between 25 ℃～120 ℃ in test condition, 100kHz, and during 200mT, power consumption P CVAll less than 400kw/m 3And 350kw/m 3
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