CN102924070B - Wide-temperature, high-frequency and low-power-consumption manganese zinc iron oxidation material and method for manufacturing same - Google Patents
Wide-temperature, high-frequency and low-power-consumption manganese zinc iron oxidation material and method for manufacturing same Download PDFInfo
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Abstract
The invention discloses a wide-temperature, high-frequency and low-power-consumption manganese zinc iron oxidation material and a method for manufacturing the same. The material comprises, by molar percentage, 50.5% to 55.0% of Fe2O3, 7.0% to 11.5% of ZnO, 30.5% to 38.5% of Mn3O4 and additive compositions of Si02, Ca0, Nb205, Zr02, TiO2, NiO and Ta2O5. The method for manufacturing the material comprises steps of: fixing a molar percentage content of the Fe2O3 and fixing contents of the ZnO and the Mn3O4; performing ball-milling for 45 minutes; pre-sintering materials after ball-milling in a rotary kiln; and performing sanding for 2 hours so that powder grain sizes are in a range from 1.0 mu m to 1.2 mu m, adding additives and the like. According to the wide-temperature, high-frequency and low-power-consumption manganese zinc iron oxidation material and the method for manufacturing the same, excellent high-frequency performances are provided for the material, demands of users for temperature characteristics are considered simultaneously, and magnetic cores of a large amount of imported magnetic cores of PC50 and 3F4 and the like in prior home appliance and communication industries can be replaced.
Description
Technical field
The present invention relates to MnZn ferrite material and preparation method thereof, be specially wide temperature high-frequency and low-consumption Mn-Zn ferrite material and preparation method thereof.
Background technology
Along with the development of colour TV, computer and various types of communication equipment is regenerated, various inducers, wave filter, magnetic core of transformer material all require to widen higher frequency of utilization and have lower power loss, therefore each major company of the world competitively develops, nearly 20 years, from the PC30 of tens of kilo hertzs, the material of PC40 level, more the PC44 material of reduce power consumption and the PC50 level material of higher frequency (more than reaching 500kHz) have been released in development.These premium quality product are widely used in high definition digital colour TV, high resolution computer indicating meter, pulse code modulation digital communication (PCM) and WDM and DWDM optical fiber communication equipment.The high frequency of magnetic core element, low power consumption, ensured the high-performance of complete machine device, highly reliable, chip type, mounting, filming.But unsatisfactory, the batch level of current domestic Ge great producer soft magnetic core is still hovered in PC40 left and right, and the residue market of some international major companies also only can be filled in foreign exchange earning aspect.
Soft magnetic ferrite is widely used, a kind of magneticsubstance that consumption is large.220,000 tons of world wide productions in 1997, wherein 50,000 tons of China's output, estimate that world wide production in 2000 will reach 300,000 tons, within 2005, reach 450,000 tons.China will reach 60,000 tons to estimate this year, within 2005, will exceed 150,000 tons, account for 1/3 of full whole world soft magnetic ferrite total amount, account for No. 1 in the world.But it is low that China remains at comparison of technology, some special technological equipments are more backward, cause the problems such as product specification is high not, need further to be solved.For adapting to the growth requirement of the wide temperature high-frequency and low-consumption of domestic and international market high-performance magnetic core, inspired by this, a kind of wide spectrum high-frequency and low-consumption material is just actively sought by each material manufacturing firm, and magnetic permeability and frequency of utilization all should have larger coverage rate, thereby replaces the numerous high-frequency and low-consumption material of item.
Summary of the invention
The present invention is just for above technical problem, provides can increase core stack resistance and reduce high-frequency loss, reduces magnetic hysteresis loss, optimizes wide temperature high-frequency and low-consumption Mn-Zn ferrite material of μ i-T curve and preparation method thereof.
Concrete technical scheme of the present invention is as follows:
Wide temperature high-frequency and low-consumption Mn-Zn ferrite material, in molar percentage, the proportioning of following composition is:
Fe
2O
3：50.5%-55.0%；?ZnO：7.0%-11.5%；?Mn
3O
4：30.5%-38.5%；
Additive component: Si0
260-140ppm, Ca0 350-700ppm,
Nb
20
5?120—550ppm,?Zr0
2?150—450ppm、TiO
2?150-350ppm、NiO?180—1500ppm,?Ta
2O
5:?20—180ppm。
The preparation method of wide temperature high-frequency and low-consumption Mn-Zn ferrite material, steps of the method are:
1) batching: first fix Fe
2o
3mole percent level, and then fixing ZnO and Mn
3o
4mole percent level;
2), ball milling: the dry type 45min that does time by force;
3), pre-burning: the material after ball milling is carried out to pre-burning at rotary kiln, and controlling temperature is 950 DEG C, and the time is 3 hours;
4) sand milling: after 2.0 hours, make the granularity of powder be controlled at median size 1.0-1.2 μ m through sand mill sand milling the material after pre-burning, then add in proportion additive ZrO
2, Ta
2o
5, NiO, CaCO
3, Nb
2o
5,siO
2,and TiO
2;
5), spraying granule: adopt spraying machine to spray, particle is 60-180 order, distribution area >=85%;
6) sintering: adopt controlled atmosphere bell jar sintering oven to carry out sintering, sintering temperature control is 1320 DEG C, is incubated 4 hours, and temperature-fall period is by equilibrium oxygen partial pres-sure.The temperature that the binder removal section of the controlled atmosphere bell jar sintering oven adopting at sintering step adopts is 0-600 DEG C, in binder removal process, slowly heats up, and 2 DEG C/min of speed <, the volumn concentration of oxygen is 20.9%; 3-5 DEG C/the min that heats up after binder removal, the volumn concentration 20.9% of oxygen; Be 1320 DEG C in the temperature of holding-zone, the time is 4 hours, and the volumn concentration of oxygen is 1%-5%; At temperature descending section, be cooled to 1000 DEG C with the speed of 3 DEG C/min; The cooling later stage, the temperature after cooling was 1000 DEG C of < with 5 DEG C/min cooling, and the volumn concentration of oxygen is down to < 0.01%.
Wide temperature high-frequency and low-consumption Mn-Zn ferrite material, Fe
2o
3: 53.3mol%; ZnO:10.2mol%; Mn
3o
4: 36.5mol%; Additive component is ZrO2:Ta
2o
5: NiO:CaCO
3, Nb
2o5:SiO
2,tiO
2.
Mn-Zn ferrite Curie temperature is mainly by Fe in formula
2o
3 +determine with the mol ratio content of ZnO.Experimental formula Of=a(X-2Z/3)-b, in formula, X and Z are respectively Fe
2o
3 +with the mol ratio of ZnO, a=12.8 DEG C, b=354 DEG C, ensures that the power consumption branch of material is near 100 DEG C in addition.
Under high frequency, reduce material power loss approach: improve resistivity, control ferritic crystal grain in optimum regime scope, because crystal grain is too small, Pe can diminish, but Ph increases.The effective way of controlling grain size and resistivity is reasonable blast blending and improves sintering process.
Total formula and doping principle are to make crystal anisotropy constant K 1 and magnetostriction constant lambda s level off to zero.
Mix HfO
2, Nb
2o
5, Ta
2o
5deng oxide compound, be controlled at below 1000PPm, obtain tiny and uniform microtexture, form high resistant grain boundary layer, increase core stack resistance and reduce high-frequency loss.Mix TiO
2, CO
2o
3control the temperature profile of material, reduce magnetic hysteresis loss, optimize μ i-T curve.
Raw-material employing in wide temperature high-frequency and low-consumption Mn-Zn ferrite material: be fixing starting material source, ensure constant product quality, reduce costs, we adopt high-quality iron oxide red, Changsha manganese, the Shanghai zinc of domestic Baosteel, require the purity of main material high, detrimental impurity is few, activity and good fluidity, size-grade distribution is suitable, and specific surface area coupling better.Add appropriate additive, can promote solid state reaction, resistance crystalline substance, flux and increase physical strength, improve the performance of sintered compact.In particle preparation process, adopt dry type conventional ceramic technique, cost is low, technique is simple.Adopt clock hood type furnace and balanced atmosphere method, strictly control the cooling atmosphere curve of sintering and warming and cooling rate.
Feature of the present invention is wide temperature, wideband, reduce power consumption.General ferrite is with the raising of service efficiency, due to the impact of eddy current and natural resonance, power consumption increases, therefore must find one or more additives, mix ferrite crystal boundary, increase its high-frequency resistance, find one or several additives to reduce its resonance energy attenuation simultaneously, also necessary accurate adjustment sintering atmosphere curve, strictly controls solid state reaction process.
Soft magnetic ferrite loss and frequency are generally linear rising relation.Magnetic hysteresis Phv > eddy current Pev when lower than 200KHZ, otherwise higher than 200KHZ.Zenger points out that 200KHZ is a weight break point, under this frequency: Phv=Pev.In the time of f > 200KHZ, eddy-current loss rises to major effect, therefore must manage to improve resistivity.Residual loss is generally the constant that does not rely on f, but is complicated function relation with frequency in radio-frequency field, and its mechanism is that domain wall resonance produces, and crystal grain thinning reduces domain wall and the difficulty that makes it to resonate, and can effectively reduce residual loss.Certainly the higher eddy-current loss being directly proportional to its square of frequency is also larger, just must manage to increase grain boundary resistance with containment eddy-current loss.
Conventionally add SiO
2, Ca, Ta
2o
5, SnO
2and Ca
2o
3, TiO
2deng containing better effects, calcium ion, in the year segregation of Mn-Zn ferrite crystal boundary, forms Calucium Silicate powder blocking layer with silicon, can improve grain boundary resistance rate, significantly reduces eddy-current loss.Add TiO
2also can form calcium titanium type resistive formation, Ti at grain boundaries
4+rise, Fe
3+ion reduces, and Fe
2+content increases, high price Ti
4+because nail is at Fe
2+position, can become a static resistance, has improved the reactive behavior of particle.Control Fe
2+content can also regulate two peak temperatures, adds Co
2+ion is got involved, and ferritic wide temperature characteristics just can obtain.
The preparation method of wide temperature high-frequency and low-consumption Mn-Zn ferrite material, the detailed step of the method is preferably:
1) batching: first fix Fe
2o
3mole percent level be 53.5 %, ensure that material has higher Curie temperature, i.e. 240 DEG C of >, determine scope and the variable quantity of other two kinds of main compositions, carry out mixture experiment design test, searching μ i and P-T curve tendency approach the scheme of target value.And then the mole percent level of fixing ZnO and Mn3O4; When Zn gets 10.2 mol%, Mn
3o
4while getting 36.5 mol%, can obtain lower power consumption.
2), ball milling: the time is 45min, and making compound mean particle size is 1.2 μ m left and right;
3), pre-burning: the material after ball milling is carried out to pre-burning at rotary kiln, object is for partial oxidation thing and carbide are decomposed, make to hold volatile impurity (as the acid group such as Cl, S) evaporation, obtain uniform miscellany and carry out preliminary solid state reaction, be transformed into a spar structure, reduce sintering shrinkage and the distortion of final product, controlling temperature is 950 DEG C, the too low pre-burning object that do not reach of temperature, the too high material powder hardness that not only can cause is excessive, be unfavorable for sand milling and mist projection granulating, also can affect contraction and the magnetic property of sintered products, the time is 3 hours;
4) sand milling: for by levigate the Preburning material after pre-burning, vibration, after 2.0 hours, make the granularity of powder be controlled at median size 1.0-1.2 μ m through sand mill sand milling the material after pre-burning, then add in proportion additive ZrO
2, Ta
2o
5, NiO, CaCO
3, Nb
2o
5,siO
2,and TiO
2, improve the performance of material by adding impurity, mainly help burning, mineralising, resistance brilliant and improve electromagnetic performance effect.In experimentation, first analyze the effect of various additives in ferrite forms, adopt Orthogonal Method to determine various portfolio ratios;
Add nanometer SiO
2-conventional CaCO
3on material property impact,
In actual procedure, Si-Ca is combined as conventional impurity, due to Ca
2+make uniform crystal particles to crystal boundary in segregation, crystal boundary obviously and Si
4+the high-resistance grain boundary layer of common formation, therefore specific loss reduces, and found through experiments and adds nanometer SiO
2with regular grade CaCO
3sample is least in power-consuming, and performance is best.
Add Ta
2o
5-Nb
2o
5-CaCO
3on material property impact,
Ta
5+make Ca
2+concentration at crystal boundary raises, and Nb ion has prevented the volatilization of Zn ion, and Ta and Nb on crystal boundary have diluted Fe
2+concentration, has suppressed its conductive capability, and resistivity is improved, and meanwhile, it is neat regular that suitable doping also can make crystal grain be evenly distributed, and void content reduces relatively, has improved density, has improved temperature profile, and μ i is also improved accordingly.
Add Co
2o
3-TiO
2-Bi
2o
3on material property impact,
The difference of Co-Ti additive is added to grain source simultaneously and carried out contrast experiment, to commercial TiO
2, Co
2o
3carry out pre-burning and ball-milling processing, additive and ferritic particle size matching are improved, add Bi2O3 to form plural components simultaneously, Bi2O3 is a kind of low melting point, in Mn-Zn ferrite sintering, play the effect of liquid phase medium, promote ion diffusion and process, this plays a key effect to improving uniform crystal particles.
5), spraying granule: adopt spraying machine to spray, particle is 60-180 order, distribution area >=85%;
6), sintering: adopt controlled atmosphere bell jar sintering oven to carry out sintering, sintering temperature control is 1320 DEG C, be incubated 4 hours, temperature-fall period is by equilibrium oxygen partial pres-sure, the sintering process of Mn-Zn ferrite is most important, in this stage, ferrite has formed correct chemical constitution, has obtained good microtexture, and lastness can be determined.The most important processing parameter of sintering process is exactly atmosphere control and sintering curre, oxygen partial pressure PO
2determine Fe
2+/ Fe
3+ratio.In balance cooling curve, the relation of PO2 and temperature is determined by the test of BLanK equation.Sintering temperature heating rate and soaking time are the important guarantees that obtains good microtexture.
Controlled atmosphere bell jar sintering oven, comprises clock hood type furnace, controller and vacuum pump, above clock hood type furnace, is connected with controller by pipeline, and controller is connected with vacuum pump.Clock hood type furnace comprises furnace shell and burner hearth, furnace shell inner side arranges burner hearth thermal insulation layer, top at burner hearth arranges venting port, vacuum pump is connected with the venting port on burner hearth by pipeline with controller, and controller can be controlled vacuum pump the gas in burner hearth is controlled, and makes the oxygen content in burner hearth even, can ensure the quality of product, adopt vacuum pump first to make high-temperature furnace body there is negative pressure, and then be filled with nitrogen, accelerate flow of nitrogen gas.Can solve some the nitrogen Dead Core Problems in body of heater.
Positively effect of the present invention is embodied in:
This material has very excellent high frequency performance, can take into account again the demand of user to temperature profile, the magnetic core such as PC50 and 3F4 of alternative current household electrical appliances and a large amount of imports of the communications industry, the simultaneously material such as alternative part PC40, PC44,6H40 also in lower frequency ranges.In the preparation method of this material, owing to having adopted controlled atmosphere bell jar sintering oven, make the oxygen content in burner hearth even, save and use nitrogen, ensure the quality of product.
Brief description of the drawings:
Fig. 1 is the structural representation of controlled atmosphere bell jar sintering oven in the present invention.
Wherein 1---controlled atmosphere bell jar sintering oven clock hood type furnace, 2---controller, 3---vacuum pump, 4---heat exchanger, 5---Controlling System, 6---oxygen analyzer.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, the present invention is described in further detail, but this should be interpreted as to the scope of the above-mentioned theme of the present invention only limits to following embodiment.
Embodiment 1:
Controlled atmosphere bell jar sintering oven is connected with heat exchanger by pipeline, and Controlling System is connected with clock hood type furnace and heat exchanger respectively.Adopt heat exchanger well to control the temperature in burner hearth.Controlling System can detect the temperature in burner hearth, and controls content, the air content etc. of heat exchanger and pure nitrogen gas.Clock hood type furnace is connected with heat exchanger by pipeline, in the middle of pipeline, variable valve is set, and can better carry out the transmission of heat by variable valve.Pure nitrogen gas device is connected with clock hood type furnace by pipeline, and gas inlet is connected with clock hood type furnace by pipeline,
In the time that Controlling System detects that oxygen content is higher, by vacuum pump extracting vacuum, make aobvious negative pressure state in body of heater, be filled with nitrogen, reduce the volume content of oxygen in clock hood type furnace, ensure whole body of heater gas uniform, can reduce like this nitrogen use level.The burner hearth middle part of clock hood type furnace is connected with oxygen analyzer by pipeline, and oxygen analyzer is connected with Controlling System.Controlling System in clock hood type furnace device can be controlled the function of temperature, atmosphere in real time, is a batch sintering oven.Temperature and atmosphere control are controlled in real time, the advantage such as good product quality, finished product consistence of producing.Production handiness is high: owing to being by batch discontinuous sintering, each batch all can be according to the difference of shape of product, size, material etc., and adopts different temperature curves, atmosphere curve and pressure curve.Process curve is set in advance in Controlling System, selects when the time comes by computer, adjusts also very convenient.Be beneficial to very much according to order difference and arrange production flexibly.
Controlled atmosphere bell jar sintering oven has changed the conventional mode that uses the positive pressure-controlled oxygen level of inflated with nitrogen utilization in sintering temperature-fall period.Extract the vacuum in clock hood type furnace by vacuum pump, making the air pressure in body of heater is negative pressure state, is filled with nitrogen by pipeline from purity nitrogen device in clock hood type furnace, reaches the volume content of the oxygen in accurate control clock hood type furnace, ensure the atmosphere homogeneous in whole clock hood type furnace body of heater, reduce the usage quantity of nitrogen.
Fixing Fe
2o
3molar percentage be 53.3%, ensure that material has higher Curie temperature (240 DEG C of >), MnZn ferrite Curie temperature mainly by formula in Fe
2o
3determine with the mol ratio content of ZnO.Experimental formula Of=a(X-2Z/3) X and Z are respectively Fe in-b(formula
2o
3mol ratio with ZnO), a=12.8 DEG C, b=354 DEG C, ensures that the power consumption branch of material is near 100 DEG C in addition, through the orthogonal test basic components of assaying: 53.3 mol%:36.5 mol%:10.2 mol%.
Fixing Fe
2o
3molar percentage be 53.3 mol%, change ZnO and Mn
3o
4molar percentage proportioning (500Kc, 50mT, 100 DEG C) design parameter as seen from table:
Can find out that it is 10.2%, Mn that ZnO gets molar content
3o
4getting molar content is 36.5 o'clock, Fe
2o
3be that 53.3 fixing doping can obtain high temperature low-power consumption.
The data that obtain sample ring Ф 25 are as follows:
Performance test is with SY8232 measurement of power consumption, and HP4284 electric bridge is surveyed inductance
Embodiment 2:
First choose the Fe that Baosteel is produced
2o
353.3 mol%, and then the ZnO10.2mol% of fixing capital production, the Mn in Hunan
3o
436.5mol%; Adopt dry type mixed by force, the time is 45min, then carries out pre-burning in rotary kiln, and controlling temperature is 950 DEG C, and the time is 3 hours; After 2.0 hours, make the granularity of powder be controlled at median size 1.0-1.2 μ m through sand milling; Then add pure water 35wt%, di(2-ethylhexyl)phosphate octanol 0.2wt%, ZrO
20.025wt%, TiO
20.015wt%, 0.025wt%, Nb
2o
50.055wt%.Then spraying granule is pressed into 25*15*10 ring.Adopt controlled atmosphere bell jar sintering oven, sintering temperature is 1320 DEG C, is incubated 4 hours, the temperature that the binder removal section of the controlled atmosphere bell jar sintering oven adopting at sintering step adopts is 500 DEG C, in binder removal process, slowly heat up, speed is 2 DEG C/min, and the volumn concentration of oxygen is 20.9%; 4 DEG C/the min that heats up after binder removal, the volumn concentration 20.9% of oxygen; Be 1320 DEG C in the temperature of holding-zone, the time is 4 hours, and the volumn concentration of oxygen is 4%; At temperature descending section, be cooled to 1000 DEG C with the speed of 3 DEG C/min; The cooling later stage, the temperature after cooling was 800 DEG C with 5 DEG C/min cooling, and the volumn concentration of oxygen is down to 0.005%.
The test of product performance in the present embodiment is with SY8232 measurement of power consumption, and HP4284 electric bridge is surveyed inductance as following table:
Embodiment 3:
First choose the Fe that Baosteel is produced
2o
3molar content be 55.0 %, and then fixing capital produce ZnO, its molar content is 10.2%, the Mn in Hunan
3o
4,its molar content is 36.5%; Adopt dry type mixed by force, the time is 45min, then carries out pre-burning at rotary kiln, and controlling temperature is 950 DEG C, and the time is 3 hours; After 2.0 hours, make the granularity of powder be controlled at median size 1.0 μ m through sand milling; Then add pure water 38wt%, di(2-ethylhexyl)phosphate octanol 0.2wt%, ZrO
20.025wt%, TiO
2200ppm, HfO
20.0148wt%, Nb
2o
50.055wt%.Then spraying granule is pressed into 25*15*10 ring.Adopt controlled atmosphere bell jar sintering oven, sintering temperature is 1320 DEG C, is incubated 4 hours, the temperature that the binder removal section of the controlled atmosphere bell jar sintering oven adopting at sintering step adopts is 500 DEG C, in binder removal process, slowly heat up, speed is 2 DEG C/min, and the volumn concentration of oxygen is 20.9%; 4 DEG C/the min that heats up after binder removal, the volumn concentration 20.9% of oxygen; Be 1320 DEG C in the temperature of holding-zone, the time is 4 hours, and the volumn concentration of oxygen is 4%; At temperature descending section, be cooled to 1000 DEG C with the speed of 3 DEG C/min; The cooling later stage, the temperature after cooling was 800 DEG C with 5 DEG C/min cooling, and the volumn concentration of oxygen is down to 0.005%.
Performance test is with SY8232 measurement of power consumption, and HP4284 surveys inductance as following table:
Embodiment 4:
First choose the Fe that Baosteel is produced
2o
3, its molar content is 53.3 %, and then the ZnO of fixing capital production, its molar content is 10.2%, the Mn in Hunan
3o
4,its molar content is 36.5%; Adopt dry type mixed by force, the time is 45min, then carries out pre-burning at rotary kiln, and controlling temperature is 950 DEG C, and the time is 3 hours; After 2.0 hours, make the granularity of powder be controlled at median size 1.1 μ m through sand milling; Then add pure water 38wt%, di(2-ethylhexyl)phosphate octanol 0.2wt%, ZrO
20.025wt%, TiO
2200ppm, Nb
2o
50.055wt%.Then spraying granule is pressed into 25*15*10 ring.Adopt controlled atmosphere bell jar sintering oven, sintering temperature is 1320 DEG C, is incubated 4 hours, the temperature that the binder removal section of the controlled atmosphere bell jar sintering oven adopting at sintering step adopts is 500 DEG C, in binder removal process, slowly heat up, speed is 2 DEG C/min, and the volumn concentration of oxygen is 20.9%; 4 DEG C/the min that heats up after binder removal, the volumn concentration 20.9% of oxygen; Be 1320 DEG C in the temperature of holding-zone, the time is 4 hours, and the volumn concentration of oxygen is 4%; At temperature descending section, be cooled to 1000 DEG C with the speed of 3 DEG C/min; The cooling later stage, the temperature after cooling was 800 DEG C with 5 DEG C/min cooling, and the volumn concentration of oxygen is down to 0.005%.
Performance test is with SY8232 measurement of power consumption, and HP4284 surveys inductance
Embodiment 5:
First choose the Fe that Baosteel is produced
2o
3, molar content is 53.3 mol%, and then the ZnO1 of fixing capital production, molar content is 0.2mol%, the Mn in Hunan
3o
4,molar content is 36.5mol%; Adopt dry type mixed by force, the time is 45min, then rotary kiln carries out pre-burning, and controlling temperature is 960 DEG C, and the time is 3 hours; After 2.0 hours, make the granularity of powder be controlled at median size 1.2 μ m through sand milling; Then add pure water 38wt%, di(2-ethylhexyl)phosphate octanol 0.2wt%, cacO
3480ppm, SiO
230ppm, Nb
2o
50.055wt%, TiO
2200ppm, then spraying granule is pressed into 25*15*10 ring.Adopt controlled atmosphere bell jar sintering oven, sintering temperature is 1320 DEG C, is incubated 4 hours, the temperature that the binder removal section of the controlled atmosphere bell jar sintering oven adopting at sintering step adopts is 500 DEG C, in binder removal process, slowly heat up, speed is 2 DEG C/min, and the volumn concentration of oxygen is 20.9%; 4 DEG C/the min that heats up after binder removal, the volumn concentration 20.9% of oxygen; Be 1320 DEG C in the temperature of holding-zone, the time is 4 hours, and the volumn concentration of oxygen is 4%; At temperature descending section, be cooled to 1000 DEG C with the speed of 3 DEG C/min; The cooling later stage, the temperature after cooling was 800 DEG C with 5 DEG C/min cooling, and the volumn concentration of oxygen is down to 0.005%.
Performance test is with SY8232 measurement of power consumption, and HP4284 surveys inductance
Can draw from embodiment 1-embodiment 5, the wide temperature high-frequency and low-consumption Mn-Zn ferrite material that adopts this technique to prepare, it has very excellent high frequency performance, can take into account again the demand of user to temperature profile.
The material obtaining in embodiment 1 to embodiment 5 is carried out to fundamental property and is analyzed as follows table:
Claims (4)
1. wide temperature high-frequency and low-consumption Mn-Zn ferrite material, is characterized in that, in molar percentage, the proportioning of following composition is:
Fe
2o
3: 50.5%-55.0%; ZnO:7.0%-11.5%; Mn
3o
4: 30.5%-38.5%, the molar percentage sum of each composition is 100%;
Additive component: SiO
260-140ppm, CaO 350-700ppm,
Nb
2O
5?120—550ppm,?ZrO
2?150—450ppm、TiO
2?150-350ppm、NiO?180—1500ppm,?Ta
2O
5:?20—180ppm；
This material in accordance with the following methods step carries out:
1) batching: first fix Fe
2o
3mole percent level, and then fixing ZnO and Mn
3o
4mole percent level;
2), ball milling: adopt dry type mixed by force, the time is 45min;
3), pre-burning: the material after ball milling is carried out to pre-burning at rotary kiln, and controlling temperature is 950 DEG C, and the time is 3 hours;
4), sand milling: after 2.0 hours, make the granularity of powder be controlled at median size 1.0-1.2 μ m through sand mill sand milling the material after pre-burning, then add additive ZrO
2, Ta
2o
5, NiO, CaCO
3, Nb
2o
5, SiO
2,and TiO
2;
5), spraying granule: adopt spraying machine to spray, particle is 60-180 order, distribution area >=85%;
6), sintering: adopt controlled atmosphere bell jar sintering oven to carry out sintering, sintering temperature control is 1320 DEG C, is incubated 4 hours, and temperature-fall period is by equilibrium oxygen partial pres-sure; The temperature that the binder removal section of controlled atmosphere bell jar sintering oven adopts is 0-600 DEG C, in binder removal process, slowly heats up.
2. wide temperature high-frequency and low-consumption Mn-Zn ferrite material according to claim 1, is characterized in that, in molar percentage, the proportioning of following composition is:
Fe
2O
3：53.3mol%；?ZnO：10.2mol%；?Mn
3O
4：36.5mol%；
Additive component is ZrO
2: Ta
2o
5: NiO:CaO:Nb
2o
5: SiO
2: TiO
2.
3. wide temperature high-frequency and low-consumption Mn-Zn ferrite material according to claim 1, it is characterized in that: the sintering step described in step 6), it is at 2 DEG C/min of the speed < of the binder removal section of controlled atmosphere bell jar sintering oven, and the volumn concentration of oxygen is 20.9%; The speed heating up after binder removal is 3-5 DEG C/min, the volumn concentration 20.9% of oxygen; Be 1320 DEG C in the temperature of holding-zone, the time is 4 hours, and the volumn concentration of oxygen is 1%-5%; At temperature descending section, be cooled to 1000 DEG C with the speed of 3 DEG C/min; The cooling later stage, the temperature after cooling was 1000 DEG C of < with 5 DEG C/min cooling, and the volumn concentration of oxygen is down to < 0.01%.
4. wide temperature high-frequency and low-consumption Mn-Zn ferrite material according to claim 1, it is characterized in that: the controlled atmosphere bell jar sintering oven clock hood type furnace adopting in the sintering step described in step 6), this controlled atmosphere bell jar sintering oven clock hood type furnace comprises controller and vacuum pump, above this clock hood type furnace, be connected with controller by pipeline, controller is connected with vacuum pump.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210434682.8A CN102924070B (en) | 2012-11-05 | 2012-11-05 | Wide-temperature, high-frequency and low-power-consumption manganese zinc iron oxidation material and method for manufacturing same |
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| CN103396111B (en) * | 2013-08-12 | 2016-01-13 | 江苏省晶石磁性材料与器件工程技术研究有限公司 | A kind of high frequency wide-temperature and low-consumption Mn-Zn ferrite and manufacturing process thereof |
| CN105628866A (en) * | 2014-12-01 | 2016-06-01 | 鞍钢股份有限公司 | Device and method for detecting sintering homogeneity degree |
| CN105601288A (en) * | 2015-12-08 | 2016-05-25 | 山东恒瑞磁电科技有限公司 | Ferrite powder sintering process |
| CN106336211A (en) * | 2016-08-25 | 2017-01-18 | 天长市中德电子有限公司 | Wide-temperature, high Bs and high-direct current superposition soft magnetic ferrite material and production method thereof |
| CN106747393A (en) * | 2016-11-15 | 2017-05-31 | 宝钢磁业（江苏）有限公司 | A kind of high-frequency and low-consumption Mn-Zn ferrite sintering process |
| CN107473727B (en) * | 2017-09-21 | 2020-12-08 | 郴州市久隆旺高科电子有限公司 | Wide-frequency wide-temperature high-power-density low-loss manganese-zinc soft magnetic ferrite material and preparation method thereof |
| CN109384463B (en) * | 2018-12-30 | 2021-04-02 | 常熟浩博电子科技有限公司 | High-frequency high-energy-efficiency conversion MnZn ferrite and preparation method thereof |
| CN111377726B (en) * | 2019-01-30 | 2021-12-21 | 浙江春晖磁电科技有限公司 | Manufacturing process for producing broadband high-magnetic-permeability ring |
| CN110803920A (en) * | 2019-09-11 | 2020-02-18 | 横店集团东磁股份有限公司 | Preparation method of high-frequency low-power-consumption NiZn soft magnetic ferrite material |
| CN111138180A (en) * | 2019-12-25 | 2020-05-12 | 江门安磁电子有限公司 | Broadband high-impedance manganese-zinc ferrite material and preparation method thereof |
| CN111056830B (en) * | 2019-12-30 | 2021-11-30 | 苏州冠达磁业有限公司 | Wide-temperature high-frequency high-impedance high-permeability manganese-zinc ferrite and preparation method thereof |
| CN111908909A (en) * | 2020-08-13 | 2020-11-10 | 江西耀润磁电科技有限公司 | Ultrahigh frequency inductor ferrite core and preparation method thereof |
| CN115448714A (en) * | 2022-10-12 | 2022-12-09 | 上海宝钢磁业有限公司 | Manganese-zinc ferrite material, preparation method and application |
| CN116283262B (en) * | 2023-01-28 | 2024-09-13 | 山东春光磁电科技有限公司 | High-temperature-resistant high-permeability high-impedance MnZn ferrite material and preparation method and application thereof |
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| JP3968188B2 (en) * | 1999-03-30 | 2007-08-29 | Ｊｆｅケミカル株式会社 | Ferrite |
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