CN104557007A - Manganese zinc ferrite with wide operating temperature range and low loss power and preparation method of manganese zinc ferrite - Google Patents

Manganese zinc ferrite with wide operating temperature range and low loss power and preparation method of manganese zinc ferrite Download PDF

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CN104557007A
CN104557007A CN201410834031.7A CN201410834031A CN104557007A CN 104557007 A CN104557007 A CN 104557007A CN 201410834031 A CN201410834031 A CN 201410834031A CN 104557007 A CN104557007 A CN 104557007A
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temperature
300khz
principal constituent
content
power
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邢冰冰
张强原
潘晓东
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TDG Holding Co Ltd
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Abstract

The invention relates to manganese zinc ferrite with a wide operating temperature range and low loss power and a preparation method of the manganese zinc ferrite. The materials of the manganese zinc ferrite comprise the following main components: 52.5mol%-53.5mol% of Fe2O3, 8.0mol%-10.0mol% of ZnO, and the balance of Mn3O4; the total content of accessory components of CaCO3, Nb2O5, Bi2O3 and Co2O3 is 0.05wt%-0.75wt% of the total quantity of the main components. The manganese zinc ferrite adopts a dry method to prepare powder, the dry method successively comprises the steps of mixing, presintering, smashing, pelleting, pressing and sintering, wherein the sintering temperature is 1260 DEG C-1280 DEG C. According to the manganese zinc ferrite disclosed by the invention, the initial permeability mui is 2000-4000(10kHz, 0.25mT, 22 DEG C-28 DEG C), the power loss Pcv is smaller than 300kW/m3(300kHz, 100mT, (0-140 DEG C)+/-3 DEG C) and is smaller than 300kW/m3(300kHz, 100mT, +/-3 DEG C), the relative loss factor tan delta/mui is smaller than 5*10<-6>(300kHz), and the design requirements for an energy-saving environment friendly power source to a low-loss high-frequency transformer can be well satisfied.

Description

A kind of wide-temperature and low-consumption power Mn-Zn ferrite and preparation method thereof
Technical field
The invention belongs to power Mn-Zn soft magnetic ferrite technical field, be specifically related to the MnZn ferrite material preparation method of a kind of wide operating temperature range, low-power consumption.
Technical background
Current information industry is fast-developing, one of mainstay industry having become world economy, therefore become the important component part of global novel material industry as the soft magnetic ferrite of information industry important foundation functional materials, and the demand of soft magnetic ferrite will continue to increase.
The demand of 3G, 4G cell phone and fixing television telephone set increases rapidly in the market, 4C(computer, communication, photoelectricity, content service) market development is rapid, mobile switch is progressively developed to miniaturization and unattended, programme-controlled exchange is fast-developing, cloud service, pocket computer enormous amount, make day by day to increase the demand of high frequency, miniaturization, high-performance, low-loss magneticsubstance.
Green illumination refers to the efficiency by improving electric lighting and system, the atmospheric polluting material reducing generating discharge and greenhouse gases.The starting point of Green Lighting Project is not only economic benefit, the more important thing is minimizing generated energy, thus reduction nonrenewable resources fires the consumption of coal.Replace incandescent light for compact fluorescent lamp, can save the electric consumption of more than 70%, the energy consumption that efficient electric light source can make cooling light fixture give out heat simultaneously obviously reduces.At present, in global range, European Union, Russia, Japan, Australia, Canada, Korea S and the U.S. have put into effect the relevant policies about superseded incandescent light all, and object is to widely popularize electricity-saving lamp.With regard to China, the usage ratio of incandescent light and electricity-saving lamp is about 8: 1, and China has about 3,000,000,000 incandescent light at present.2012, the popularity rate of China's electricity-saving lamp was about 15%, and the electricity-saving lamp popularity rate of the U.S. also only has about 20%.Therefore, electricity-saving lamp market outlook are very wide.And Green Lighting Project needs a large amount of MnZn ferrite materials for the manufacture of less energy-consumption luminescent lamp, every electricity-saving lamp is to the consumption of soft magnetic ferrite at about 0.2-0.5 kilogram, and demand is huge.
Along with people to energy-conserving and environment-protective require more and more higher, the external power supplies such as power supply adaptor, switch power supply, charger as efficient, energy-conservation powered products also in this requirements of plan.European Union is independently advancing the voluntary of external power source (power supply adaptor, switch power supply, charger) and mandatory plan, to improve the efficiency requirement of external power source further.And USDOE (DoE) has also issued the bulletin of advising Rulemaking first in 2013, namely DoE VI, mainly for power supply adaptor, switch power supply and charger product.New Energy Efficiency Standard is proposed higher requirement to average efficiency and stand-by power consumption, traditional manganese zinc ferrites for power supplies can not meet the requirement of people to power-efficient, the novel material lower in the urgent need to loss, stability better, Applicable temperature scope is wider.
Summary of the invention
For the new demand of energy-conserving and environment-protective power supply product, the object of this invention is to provide that a kind of operating temperature range is wider, power loss is lower, the better manganese zinc ferrites for power supplies of temperature stability, this material has following excellent over-all properties: higher initial permeability, wider operating temperature range, lower power loss, be conducive to the raising of power-efficient, meet the demand of power supply product to high power density, high stability, energy-conserving and environment-protective future development.
The cardinal principle of technical solution problem of the present invention is: adopt Fe 2o 3the rich iron formula that/ZnO mol ratio is greater than 5%, adds CaCO in minor component 3with Nb 2o 5, Bi 2o 3combined dopants optimizes crystal grain vesicular structure, reduces the high band relative loss factor factor; Co is added in minor component 2o 3reduce spillage of material temperature factor; Adopt special pre-burning atmosphere technology controlling and process pre-burning powder electromagnetism physical property, reduce the specific loss factor of material.
The technical solution used in the present invention is:
First aspect, a kind of wide-temperature and low-consumption power Mn-Zn ferrite, in 0 DEG C ~ 140 DEG C temperature ranges, in 10kHz ~ 300kHz range of frequency, has excellent power loss P cvfor in power supply adaptor, switch power supply, charger, LED drive power, effectively can reduce equipment loss, improve power supply average efficiency and no-load efficiency, meet the demand be applied under severe environmental conditions, it comprises principal constituent and minor component, and principal constituent is: ferric oxide, trimanganese tetroxide and zinc oxide; Described principal constituent is as follows in the content of respective standard substance:
Fe 2O 3：52.5mol%~53.5mol%，
ZnO：8.0mol%~10.0mol%，
All the other are Mn 3o 4;
Described minor component comprises calcium carbonate, Niobium Pentxoxide, bismuth oxide and cobalt oxide, relatively described principal constituent total amount, and described minor component is with its standard substance CaCO separately 3, Nb 2o 5, Bi 2o 3and Co 2o 3the total content of meter is 0.05wt% ~ 0.75wt%.
Preferred as one, relatively described principal constituent total amount, described minor component calcium carbonate, Niobium Pentxoxide, bismuth oxide and cobalt oxide are with its standard substance CaCO separately 3, Nb 2o 5, Bi 2o 3and Co 2o 3the content of meter is respectively: CaCO 3: 0.03 wt% ~ 0.1 wt%, Nb 2o 5: 0.005 wt% ~ 0.05 wt%, Bi 2o 3: 0.01 wt% ~ 0.1 wt%, Co 2o 3: 0.15 wt% ~ 0.5 wt%.
Described wide-temperature and low-consumption power Mn-Zn ferrite, it has low power loss under 10kHz ~ 500kHz, 10mT ~ 100mT range of condition, and the 300kHz power loss factor is less than 5 × 10 -6.
Second aspect, a kind of preparation method of the wide-temperature and low-consumption power Mn-Zn ferrite as described in first aspect, comprises mixing, pre-burning, pulverizing, granulation, compacting and sintering step successively, wherein:
(1) mix: by principal constituent proportion ingredient, carry out dry mixed together; Described principal constituent in the content of respective standard substance is: Fe 2o 3: 523.5mol% ~ 53.5mol%, ZnO:8.0mol% ~ 10.0mol%, all the other are Mn 3o 4;
(2) pre-burning: carry out pre-burning by adding in rotary kiln after principal constituent slip spraying dry, calcined temperature controls at 850 DEG C ~ 1000 DEG C, and burn-in time is 30 ~ 90 minutes, pre-burning atmosphere oxygen partial pressure P o2be 20% ~ 35%;
(3) pulverize: carry out wet pulverization add minor component in the principal constituent Preburning material that upper step pre-burning obtains after, grinding time is 60 ~ 120 minutes, after pulverizing, slip size controlling is at 0.8 ~ 1.2 μm; Described minor component is with its standard substance CaCO separately 3, Nb 2o 5, Bi 2o 3and Co 2o 3the total content of meter is 0.075wt% ~ 0.18wt%;
(4) granulation: the slip of upper step add be equivalent to slip weight 1.5% PVA solution, adopt mist projection granulating, obtain particulate material; The content of described PVA solution is 7.5%-20%;
(5) suppress: the particulate material of upper step adopted powder former compacting to obtain blank, the pressed density of blank controls at 3.0 ± 0.2g/cm 3;
(6) sinter: the blank that upper step obtains is sintered in clock hood type furnace, temperature rise rate controls at 1.25 ~ 3 DEG C/min, carry out densification at 900 DEG C to firing temperature to control, control oxygen level lower than 1%, sintering temperature controls at 1260 DEG C ~ 1280 DEG C, holding-zone Control for Oxygen Content is 5.0% ~ 7.5%, and be incubated 3 ~ 5 hours, rate of temperature fall controls at 1.25 ~ 2 DEG C/min.
Preferred as one, pulverising step (3) in, described minor component calcium carbonate, Niobium Pentxoxide, bismuth oxide and cobalt oxide are with its standard substance CaCO separately 3, Nb 2o 5, Bi 2o 3and Co 2o 3the content of meter is respectively: CaCO 3: 0.03 wt% ~ 0.1 wt%, Nb 2o 5: 0.005 wt% ~ 0.05 wt%, Bi 2o 3: 0.01 wt% ~ 0.1 wt%, Co 2o 3: 0.15 wt% ~ 0.5 wt%.
In manufacture method of the present invention, sintering temperature is at 1260 DEG C ~ 1280 DEG C, and the sintering temperature of the material 1280 DEG C ~ 1300 DEG C of relatively conventional initial magnetic permeability 2000 ~ 4000, reduces 20 DEG C.In the present invention, the production technique of energy-conserving and environment-protective power supply wide temperature low-power consumption MnZn ferrite material has lower sintering temperature, effectively can reduce the production energy consumption of product.
The present invention is mixed by the minor component of rational principal constituent proportioning and optimization, be equipped with suitable processing condition, under the condition of sintering temperature and low, obtained tiny homogeneous, the cavernous Mn-Zn ferrite of microcosmic crystal grain, this ferrite has the initial magnetic permeability of 2000 ~ 4000, wide operating temperature range and low power loss and low power loss temperature factor.Specifically, the initial permeability μ of Mn-Zn ferrite that obtains of the present invention ifor: 2000 ~ 4000(10kHz, 0.25mT, 25 DEG C ± 3 DEG C), its power loss P cvbe less than 300kW/m 3(300kHz, 100mT, (0 ~ 140 DEG C) ± 3 DEG C), specific loss factor t an δ/μ ibe less than 5 × 10 -6(300kHz).Energy-conserving and environment-protective power supply wide-temperature and low-consumption power Mn-Zn ferrite of the present invention, in wider operating temperature range, over-all properties is superior, and the performances such as its initial permeability, power loss and saturation magnetization can be good at the service requirements meeting switch power high-frequency transformer.Within the scope of particularly 0 DEG C ~ 140 DEG C, there is low power loss, can be good at the power loss reducing high-frequency transformer, improve average efficiency and the no-load efficiency of power supply.
The present invention has following characteristics compared with prior art: the power supply wide temperature low-power consumption Mn-Zn ferrite adopting dry method p owder production method to prepare has low power loss, wide operating temperature range, low loss temperature factor, stable production technique and excellent performance, can be good at meeting the design requirements of energy-conserving and environment-protective power supply to low-loss high-frequency transformer.
Accompanying drawing explanation
Fig. 1 toroidal core exemplar.
Fig. 2 densification sintering atmosphere figure.
Embodiment
Below by way of specific embodiment, the invention will be further described, but the present invention is not limited to these embodiments.
embodiment 1:
Take the Fe of 52.7mol% 2o 3, 37.8 mol% Mn 3o 4with the ZnO of 9.5 mol%.After above-mentioned principal constituent mixing, add in sand mill and mix, mixing time 30 minutes, sends into rotary kiln after spraying dry, pre-burning at 900 DEG C ± 10 DEG C temperature.In Preburning material, add minor component input sand mill subsequently pulverize, grinding time 120 minutes, after pulverizing, slip size controlling is at 0.8 ~ 1.2 μm; Relatively described principal constituent total amount, described minor component is respectively in the content (wt%) of its standard substance separately: CaCO 3: 0.03, Nb 2o 5: 0.005, Bi 2o 3: 0.02, Co 2o 3: 0.40.Described mixing sand milling and pulverizing in sand grinding process needs to add the 45 wt % that pure water is equivalent to principal constituent total amount, and dispersion agent and defoamer some (being as the criterion to obtain setting particle size range).Last add in sand milling slip be equivalent to slip weight 1.5% PVA solution (PVA content 8%) obtain Mn-Zn ferrite particles by spray tower mist projection granulating.
Getting this particle adopts pressure forming to be toroidal core as shown in Figure 1.Pressed density controls at 3.0 ± 0.2g/cm 3sinter in clock hood type furnace, as shown in Fig. 2 curve, temperature rise rate controls at 1.25 ~ 3 DEG C/min, carries out densification and controls, control oxygen level volume ratio lower than 1% at 900 DEG C to sintering temperature, sintering temperature controls at 1260 DEG C ~ 1280 DEG C, holding-zone oxygen level volume ratio controls 5.0% ~ 7.5%, and be incubated 3 ~ 5 hours, rate of temperature fall controls at 1.25 ~ 2 DEG C/min.Obtained described Mn-Zn ferrite toroidal core product size is mm × 10, T25mm × 15 mm.Through magnetic core prepared by said process, test normal temperature initial permeability μ respectively with instruments such as HP4284A LCR tester, high/low temperature thermostat containers i, the power loss P that 300kHz/100 mT condition is lower 0 DEG C, 140 DEG C cv, the specific loss factor t an δ/μ under 300kHz condition i.
Prepared magnetic core is evaluated.Normal temperature initial permeability μ ibe under 2000 ~ 4000,300kHz/100 mT condition, 0 DEG C of power loss P cv< 300kW/m 3, 140 DEG C of power loss P cv< 300kW/m 3, 300kHz specific loss factor t an δ/μ i< 5 × 10 -6 .when above condition all meets the requirements, be evaluated as " √ ": good, if having one undesirable, be evaluated as "×": bad.
Table 1 toroidal core material property I of the present invention
As shown in table 1, the initial permeability μ of embodiment 1 i: 2176, meet initial permeability μ i2000 ~ 4000, requirement, and there is excellent power loss P cv, under meeting 300kHz, 100 mT conditions, 0 DEG C of power loss P cv< 300kW/m 3(actual 224kW/m 3), 140 DEG C of power loss P cv< 300kW/m 3(actual 239 kW/m 3), 300kHz specific loss factor t an δ/μ i< 5 × 10 -6(actual 3.2 × 10 -6), evaluating characteristics is good (" √ ") all.
embodiment 2 ~ 6:
As shown in table 1, except the Fe as principal constituent 2o 3form outside the composition of 52.5mol% ~ 53.5mol% scope and ZnO changes within the scope of 8.0mol% ~ 10.0mol%, all the other are trimanganese tetroxide.All the other techniques are carried out all similarly to Example 1, and after above-mentioned principal constituent mixing, add in sand mill and mix, mixing time 30 minutes, sends into rotary kiln after spraying dry, pre-burning at 900 DEG C ± 10 DEG C temperature.In Preburning material, add minor component input sand mill subsequently pulverize, grinding time 120 minutes, after pulverizing, slip size controlling is at 0.8 ~ 1.2 μm; Relatively described principal constituent total amount, described minor component is respectively in the content (wt%) of its standard substance separately: CaCO 3: 0.03, Nb 2o 5: 0.005, Bi 2o 3: 0.02, Co 2o 3: 0.40.Described mixing sand milling and pulverizing in sand grinding process needs to add the 45wt% that pure water is equivalent to principal constituent total amount, and dispersion agent and defoamer some (being as the criterion to obtain setting particle size range).Last add in sand milling slip be equivalent to slip weight 1.5% PVA solution (PVA content 8%) obtain Mn-Zn ferrite particles by spray tower mist projection granulating.
Getting this particle adopts pressure forming to be toroidal core as shown in Figure 1, and pressed density controls at 3.0 ± 0.2g/cm 3sinter in clock hood type furnace, as shown in Fig. 2 curve, temperature rise rate controls at 1.25 ~ 3 DEG C/min, carries out densification and controls, control oxygen level volume ratio lower than 1% at 900 DEG C to sintering temperature, sintering temperature controls at 1260 DEG C ~ 1280 DEG C, holding-zone oxygen level volume ratio controls 5.0% ~ 7.5%, and be incubated 3 ~ 5 hours, rate of temperature fall controls at 1.25 ~ 2 DEG C/min.Obtained described Mn-Zn ferrite toroidal core product size is mm × 10, T25mm × 15 mm.Through magnetic core prepared by said process, test normal temperature initial permeability μ respectively with instruments such as HP4284A LCR tester, high/low temperature thermostat containers i, the power loss P that 300kHz/100 mT condition is lower 0 DEG C, 140 DEG C cv, the specific loss factor t an δ/μ under 300kHz condition i.
Prepared magnetic core is evaluated.Normal temperature initial permeability μ ibe under 2000 ~ 4000,300kHz/100 mT condition, 0 DEG C of power loss P cv< 300kW/m 3, 140 DEG C of power loss P cv< 300kW/m 3, 300kHz specific loss factor t an δ/μ i< 5 × 10 -6 .when above condition all meets the requirements, be evaluated as " √ ": good, if having one undesirable, be evaluated as "×": bad.
As shown in table 1, the initial permeability μ of embodiment 2 ~ 6 i: 2106 ~ 3512, meet initial permeability μ i2000 ~ 4000, requirement, and there is excellent power loss P cv, under meeting 300kHz, 100mT condition, 0 DEG C of power loss P cv< 300kW/m 3(actual 224 ~ 275 kW/m 3), 140 DEG C of power loss P cv< 300kW/m 3(actual 207 ~ 299 kW/m 3), 300kHz specific loss factor t an δ/μ i< 5 × 10 -6(actual 2.6 ~ 4.5 × 10 -6), evaluating characteristics is good (" √ ") all.
comparative example 1 ~ 8:
As shown in table 1, except the Fe as principal constituent 2o 3form outside the composition of 52mol% ~ 54mol% scope and ZnO changes within the scope of 7.0mol% ~ 10.5mol%, all the other are trimanganese tetroxide.All the other techniques are all same with embodiment 1 ~ 6 carries out, and after above-mentioned principal constituent mixing, add in sand mill and mix, mixing time 30 minutes, sends into rotary kiln after spraying dry, pre-burning at 900 DEG C ± 10 DEG C temperature.In Preburning material, add minor component input sand mill subsequently pulverize, grinding time 120 minutes, after pulverizing, slip size controlling is at 0.8 ~ 1.2 μm; Relatively described principal constituent total amount, described minor component is respectively in the content (wt%) of its standard substance separately: CaCO 3: 0.03, Nb 2o 5: 0.005, Bi 2o 3: 0.02, Co 2o 3: 0.40.Described mixing sand milling and pulverizing in sand grinding process needs to add the 45wt% that pure water is equivalent to principal constituent total amount, and dispersion agent and defoamer some (being as the criterion to obtain setting particle size range).Last add in sand milling slip be equivalent to slip weight 1.5% PVA solution (PVA content 8%) obtain Mn-Zn ferrite particles by spray tower mist projection granulating.
Getting this particle adopts pressure forming to be toroidal core as shown in Figure 1, and pressed density controls at 3.0 ± 0.2g/cm 3sinter in clock hood type furnace, as shown in Fig. 2 curve, temperature rise rate controls at 1.25 ~ 3 DEG C/min, carries out densification and controls, control oxygen level volume ratio lower than 1% at 900 DEG C to firing temperature, sintering temperature controls at 1260 DEG C ~ 1280 DEG C, holding-zone oxygen level volume ratio controls 5.0% ~ 7.5%, and be incubated 3 ~ 5 hours, rate of temperature fall controls at 1.25 ~ 2 DEG C/min.Obtained described Mn-Zn ferrite toroidal core product size is mm × 10, T25mm × 15 mm.Through magnetic core prepared by said process, test normal temperature initial permeability μ respectively with instruments such as HP4284A LCR tester, high/low temperature thermostat containers i, the power loss P that 300kHz/100 mT condition is lower 0 DEG C, 140 DEG C cv, the specific loss factor t an δ/μ under 300kHz condition i.
Prepared magnetic core is evaluated.Normal temperature initial permeability μ ibe under 2000 ~ 4000,300kHz/100 mT condition, 0 DEG C of power loss P cv< 300kW/m 3, 140 DEG C of power loss P cv< 300kW/m 3, 300kHz specific loss factor t an δ/μ i< 5 × 10 -6 .when above condition all meets the requirements, be evaluated as " √ ": good, if having one undesirable, be evaluated as "×": bad.
Comparative example 1 is that iron oxide content is more than 52.5mol% ~ 53.5mol% upper limit (in column additional " ※ ").
Comparative example 2 is that iron oxide content is more than 52.5mol% ~ 53.5mol% lower limit (in column additional " * ").
Comparative example 3 is that zinc oxide content is more than 8.0mol% ~ 10.0mol% upper limit (in column additional " ※ ").
Comparative example 4 is that zinc oxide content is more than 8.0mol% ~ 10.0mol% lower limit (in column additional " * ").
Comparative example 5 is iron oxide contents more than 52.5mol% ~ 53.5mol% upper limit (in column additional " ※ "), and zinc oxide content is more than 8.0mol% ~ 10.0mol% upper limit (in column additional " ※ ").
Comparative example 6 is iron oxide contents more than 52.5mol% ~ 53.5mol% upper limit (in column additional " ※ "), and zinc oxide content is more than 8.0mol% ~ 10.0mol% lower limit (in column additional " * ").
Comparative example 7 is iron oxide contents more than 52.5mol% ~ 52.5mol% lower limit (in column additional " * "), and zinc oxide content is more than 8.0mol% ~ 10.0mol% upper limit (in column additional " ※ ").
Comparative example 8 is iron oxide contents more than 52.5mol% ~ 53.5mol% lower limit (in column additional " * "), and zinc oxide content is more than 8.0mol% ~ 10.0mol% lower limit (in column additional " * ").
Its result shown in table 1, to exceeding initial permeability μ iadditional " ※ " of 2000 ~ 4000 upper limits, additional " * " of lower limit, the power loss P that 300kHz, 100mT condition is lower 0 DEG C, 140 DEG C cvexceed additional " ※ " of the upper limit, 300kHz specific loss factor t an δ/μ iexceed additional " ※ " of the upper limit.The evaluation of comparative example 1 ~ 8 all bad ("×").
evaluate 1:
Contrast above embodiment and comparative example can be found out, containing with Fe 2o 352.5mol% ~ 53.5mol% ferric oxide of meter, in 8.0mol% ~ 10.0mol% zinc oxide of ZnO, all the other are trimanganese tetroxides, relatively described principal constituent total amount, and described minor component is respectively in the content (wt%) of its standard substance separately: CaCO 3: 0.03, Nb 2o 5: 0.005, Bi 2o 3: 0.02, Co 2o 3: 0.40, can confirm to meet initial permeability μ ibe under 2000 ~ 4000,300kHz/100 mT condition, 0 DEG C of power loss P cv< 300kW/m 3, 140 DEG C of power loss P cv< 300kW/m 3, 300kHz specific loss factor t an δ/μ i< 5 × 10 -6requirement.
embodiment 7 ~ 8:
As shown in table 2, as the Fe of principal constituent 2o 3, ZnO, Mn 3o 4content is all identical with embodiment 1, changes the content of the minor component cobalt oxide as additive, to its normal temperature initial permeability μ i, the power loss P that 300kHz, 100mT condition is lower 0 DEG C, 140 DEG C cvcharacteristic, the specific loss factor t an δ/μ under 300kHz condition istudy.
Embodiment 7 is lower limits that cobalt oxide content is in 0.15 wt% ~ 0.5wt% scope.
Embodiment 8 is upper limits that cobalt oxide content is in 0.15 wt% ~ 0.5wt% scope.
Except the composition pressed listed by table 2, all adopt and obtain Mn-Zn ferrite goods exemplar with embodiment 1 same process, test normal temperature initial permeability μ respectively with instruments such as HP4284A LCR tester, high/low temperature thermostat containers i, the power loss P that 300kHz/100mT condition is lower 0 DEG C, 140 DEG C cv, the specific loss factor t an δ/μ under 300kHz condition i.
Prepared magnetic core is evaluated.Normal temperature initial permeability μ ibe under 2000 ~ 4000,300kHz/100 mT condition, 0 DEG C of power loss P cv< 300kW/m 3, 140 DEG C of power loss P cv< 300kW/m 3, 300kHz specific loss factor t an δ/μ i< 5 × 10 -6 .when above condition all meets the requirements, be evaluated as " √ ": good, if having one undesirable, be evaluated as "×": bad.
As shown in table 2, the initial permeability μ of embodiment 7 ~ 8 i: 2571 ~ 3856, meet initial permeability μ i2000 ~ 4000, requirement, and there is excellent power loss P cv, under meeting 300kHz, 100mT condition, 0 DEG C of power loss P cv< 300kW/m 3(actual 225 ~ 257 kW/m 3), 140 DEG C of power loss P cv< 300kW/m 3(actual 218 ~ 287 kW/m 3), 300kHz specific loss factor t an δ/μ i< 5 × 10 -6(actual 2.0 ~ 3.5 × 10 -6), evaluating characteristics is good (" √ ") all.
comparative example 9 ~ 10:
In comparative example 9 ~ 10, change the content of the minor component cobalt oxide as additive, to its normal temperature initial permeability μ i, the power loss P that 300kHz, 100mT condition is lower 0 DEG C, 140 DEG C cvcharacteristic, the specific loss factor t an δ/μ under 300kHz condition istudy.
As shown in table 2, as the Fe of principal constituent in comparative example 9 ~ 10 2o 3, ZnO, Mn 3o 4content is identical with embodiment 1.
Comparative example 9 is cobalt oxide content lower limits (in column additional " * ") more than 0.15 wt% ~ 0.5wt% scope.
Comparative example 10 is cobalt oxide content upper limits (in column additional " ※ ") more than 0.15 wt% ~ 0.5wt% scope.
Except the composition pressed listed by table 2, all adopt and obtain Mn-Zn ferrite goods exemplar with embodiment 1 same process.Normal temperature initial permeability μ is tested respectively with instruments such as HP4284A LCR tester, high/low temperature thermostat containers i, the power loss P that 300kHz/100mT condition is lower 0 DEG C, 140 DEG C cv, the specific loss factor t an δ/μ under 300kHz condition i.
Prepared magnetic core is evaluated.Normal temperature initial permeability μ ibe under 2000 ~ 4000,300kHz/100 mT condition, 0 DEG C of power loss P cv< 300kW/m 3, 140 DEG C of power loss P cv< 300kW/m 3, 300kHz specific loss factor t an δ/μ i< 5 × 10 -6 .when above condition all meets the requirements, be evaluated as " √ ": good, if having one undesirable, be evaluated as "×": bad.
Table 2 toroidal core material property II of the present invention
Its result shown in table 2, to exceeding initial permeability μ iadditional " ※ " of 2000 ~ 4000 upper limits, additional " * " of lower limit, the power loss P that 300kHz, 100mT condition is lower 0 DEG C, 140 DEG C cvexceed additional " ※ " of the upper limit, 300kHz specific loss factor t an δ/μ iexceed additional " ※ " of the upper limit.The evaluation of comparative example 9 ~ 10 all bad ("×").
evaluate 2:
Contrast above embodiment and comparative example can be found out, containing with Fe 2o 352.5mol% ~ 53.5mol% ferric oxide of meter, in 8.0mol% ~ 10.0mol% zinc oxide of ZnO, all the other are trimanganese tetroxides, relatively described principal constituent total amount, and described minor component is respectively (wt%) in the content of its standard substance separately: CaCO 3: 0.03, Nb 2o 5: 0.005, Bi 2o 3: 0.02, Co 2o 3: 0.15 ~ 0.5, can confirm to meet initial permeability μ ibe under 2000 ~ 4000,300kHz/100 mT condition, 0 DEG C of power loss P cv< 300kW/m 3, 140 DEG C of power loss P cv< 300kW/m 3, 300kHz specific loss factor t an δ/μ i< 5 × 10 -6requirement.
comparative example 11 ~ 16:
In comparative example 11 ~ 16, change arbitrarily as minor component calcium carbonate, the Niobium Pentxoxide of additive, the content of bismuth oxide, to its normal temperature initial permeability μ i, the power loss P that 300kHz, 100mT condition is lower 0 DEG C, 140 DEG C cvcharacteristic, the specific loss factor t an δ/μ under 300kHz condition istudy.
As shown in table 3, as the Fe of principal constituent in comparative example 11 ~ 16 2o 3, ZnO, Mn 3o 4content is identical with embodiment 1.
Comparative example 11 is calcium carbonate content lower limits (in column additional " * ") more than 0.03wt% ~ 0.1wt% scope.
Comparative example 12 is calcium carbonate content upper limits (in column additional " ※ ") more than 0.03wt% ~ 0.1wt% scope.
Comparative example 13 is Niobium Pentxoxide content lower limits (in column additional " * ") more than 0.005wt% ~ 0.05wt% scope.
Comparative example 14 is Niobium Pentxoxide content upper limits (in column additional " ※ ") more than 0.005wt% ~ 0.05wt% scope.
Comparative example 15 is bismuth oxide content lower limits (in column additional " * ") more than 0.01wt% ~ 0.03wt% scope.
Comparative example 16 is bismuth oxide content upper limits (in column additional " ※ ") more than 0.01wt% ~ 0.03wt% scope.
Except the composition pressed listed by table 3, all adopt and obtain Mn-Zn ferrite goods exemplar with embodiment 1 same process.Normal temperature initial permeability μ is tested respectively with instruments such as HP4284A LCR tester, high/low temperature thermostat containers i, the power loss P that 300kHz/100mT condition is lower 0 DEG C, 140 DEG C cv, the specific loss factor t an δ/μ under 300kHz condition i.
Prepared magnetic core is evaluated.Normal temperature initial permeability μ ibe under 2000 ~ 4000,300kHz/100 mT condition, 0 DEG C of power loss P cv< 300kW/m 3, 140 DEG C of power loss P cv< 300kW/m 3, 300kHz specific loss factor t an δ/μ i< 5 × 10 -6 .when above condition all meets the requirements, be evaluated as " √ ": good, if having one undesirable, be evaluated as "×": bad.
Table 3 toroidal core material property III of the present invention
Its result shown in table 3, to exceeding initial permeability μ iadditional " ※ " of 2000 ~ 4000 upper limits, additional " * " of lower limit, the power loss P that 300kHz, 100mT condition is lower 0 DEG C, 140 DEG C cvexceed additional " ※ " of the upper limit, 300kHz specific loss factor t an δ/μ iexceed additional " ※ " of the upper limit.The evaluation of comparative example 11 ~ 16 all bad ("×").
evaluate 3:
Contrast above embodiment and comparative example can be found out, containing with Fe 2o 352.5mol% ~ 53.5mol% ferric oxide of meter, in 8.0mol% ~ 10.0mol% zinc oxide of ZnO, all the other are trimanganese tetroxides, relatively described principal constituent total amount, and described minor component is respectively (wt%) in the content of its standard substance separately: CaCO 3: 0.03 ~ 0.1, Nb 2o 5: 0.005 ~ 0.05, Bi 2o 3: 0.01 ~ 0.03, Co 2o 3: 0.04, can confirm to meet initial permeability μ ibe under 2000 ~ 4000,300kHz/100 mT condition, 0 DEG C of power loss P cv< 300kW/m 3, 140 DEG C of power loss P cv< 300kW/m 3, 300kHz specific loss factor t an δ/μ i< 5 × 10 -6requirement.
As mentioned above, adopt the wide operating temperature range low-loss manganese zine ferrite that in the present invention prepared by formula, power production method and sintering method, there is the good characteristics such as high initial magnetoconductivity, low-power consumption, wide operating temperature range, the low specific loss factor, the transformer made of this design of material can adapt to harsh environments, loss is low, can meet European Union, U.S.'s new standard to the demand for development of power supply.

Claims (5)

1. a wide-temperature and low-consumption power Mn-Zn ferrite, in 0 DEG C ~ 140 DEG C temperature ranges, in 10kHz ~ 300kHz range of frequency, has excellent power loss P cvfor in power supply adaptor, switch power supply, charger, LED drive power, effectively can reduce equipment loss, improve power supply average efficiency and no-load efficiency, meet the demand be applied under severe environmental conditions, it comprises principal constituent and minor component, and principal constituent is: ferric oxide, trimanganese tetroxide and zinc oxide; It is characterized in that, described principal constituent is as follows in the content of respective standard substance:
Fe 2O 3：52.5mol%~53.5mol%，
ZnO：8.0mol%~10.0mol%，
All the other are Mn 3o 4;
Described minor component comprises calcium carbonate, Niobium Pentxoxide, bismuth oxide and cobalt oxide, relatively described principal constituent total amount, and described minor component is with its standard substance CaCO separately 3, Nb 2o 5, Bi 2o 3and Co 2o 3the total content of meter is 0.05wt% ~ 0.75wt%.
2. wide-temperature and low-consumption power Mn-Zn ferrite as claimed in claim 1, is characterized in that: relatively described principal constituent total amount, and described minor component calcium carbonate, Niobium Pentxoxide, bismuth oxide and cobalt oxide are with its standard substance CaCO separately 3, Nb 2o 5, Bi 2o 3and Co 2o 3the content of meter is respectively: CaCO 3: 0.03 wt% ~ 0.1 wt%, Nb 2o 5: 0.005 wt% ~ 0.05 wt%, Bi 2o 3: 0.01 wt% ~ 0.1 wt%, Co 2o 3: 0.15 wt% ~ 0.5 wt%.
3. wide-temperature and low-consumption power Mn-Zn ferrite as claimed in claim 1 or 2, it is characterized in that having low power loss under 10kHz ~ 500kHz, 10mT ~ 100mT range of condition, the 300kHz power loss factor is less than 5 × 10 -6.
4. a preparation method for wide-temperature and low-consumption power Mn-Zn ferrite as claimed in claim 1, is characterized in that, comprise mixing, pre-burning, pulverizing, granulation, compacting and sintering step successively, wherein:
(1) mix: by principal constituent proportion ingredient, carry out dry mixed together; Described principal constituent in the content of respective standard substance is: Fe 2o 3: 523.5mol% ~ 53.5mol%, ZnO:8.0mol% ~ 10.0mol%, all the other are Mn 3o 4;
(2) pre-burning: carry out pre-burning by adding in rotary kiln after principal constituent slip spraying dry, calcined temperature controls at 850 DEG C ~ 1000 DEG C, and burn-in time is 30 ~ 90 minutes, pre-burning atmosphere oxygen partial pressure P o2be 20 ~ 35%;
(3) pulverize: carry out wet pulverization add minor component in the principal constituent Preburning material that upper step pre-burning obtains after, grinding time is 60 ~ 120 minutes, after pulverizing, slip size controlling is at 0.8 ~ 1.2 μm; Described minor component is with its standard substance CaCO separately 3, Nb 2o 5, Bi 2o 3and Co 2o 3the total content of meter is 0.075wt% ~ 0.18wt%;
(4) granulation: the slip of upper step add be equivalent to slip weight 1.5% PVA solution, adopt mist projection granulating, obtain particulate material; The content of described PVA solution is 7.5%-20%;
(5) suppress: the particulate material of upper step adopted powder former compacting to obtain blank, the pressed density of blank controls at 3.0 ± 0.2g/cm 3;
(6) sinter: the blank that upper step obtains is sintered in clock hood type furnace, temperature rise rate controls at 1.25 ~ 3 DEG C/min, carry out densification at 900 DEG C to firing temperature to control, control oxygen level lower than 1%, sintering temperature controls at 1260 DEG C ~ 1280 DEG C, holding-zone Control for Oxygen Content is 5.0% ~ 7.5%, and be incubated 3 ~ 5 hours, rate of temperature fall controls at 1.25 ~ 2 DEG C/min.
5. the preparation method of wide-temperature and low-consumption power Mn-Zn ferrite as claimed in claim 4, is characterized in that, pulverising step (3) in, described minor component calcium carbonate, Niobium Pentxoxide, bismuth oxide and cobalt oxide are with its standard substance CaCO separately 3, Nb 2o 5, Bi 2o 3and Co 2o 3the content of meter is respectively: CaCO 3: 0.03 wt% ~ 0.1 wt%, Nb 2o 5: 0.005 wt% ~ 0.05 wt%, Bi 2o 3: 0.01 wt% ~ 0.1 wt%, Co 2o 3: 0.15 wt% ~ 0.5 wt%.
CN201410834031.7A 2014-12-30 2014-12-30 Manganese zinc ferrite with wide operating temperature range and low loss power and preparation method of manganese zinc ferrite Pending CN104557007A (en)

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