CN103496963A - Ni-free MnZn ferrite magnetic core with double characteristics and manufacture method - Google Patents
Ni-free MnZn ferrite magnetic core with double characteristics and manufacture method Download PDFInfo
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Abstract
The invention provides a Ni-free MnZn ferrite magnetic core with double characteristics and a manufacture method thereof, wherein the double characteristics mean high temperature and high Bs, and wide temperature and low loss. The ferrite magnetic core comprises main components and auxiliary components. The main components comprise: 53 mol%-54 mol% of Fe2O3, 39 mol%-42 mol% of MnO and 4 mol%-7 mol% of ZnO; and the auxiliary components comprise: Co2O3 or CoO or Co3O4 as a first auxiliary component, SiO2 and CaCO3 as a second auxiliary, and a third auxiliary component which is one or more selected from MoO3, TiO2, SnO2, Nb2O5, V2O5, Sm2O3 and ZrO2. The provided MnZn ferrite magnetic core with double characteristics has unit volume loss Pcv (100kHz, 200mT) less than 350 kW/m<3> at the temperature of 25 DEG C to 120 DEG C, lowest loss of 300 kW/m<3> at the temperature of about 90 DEG C, and saturation magnetic flux density up to 450 mT at the temperature of 100 DEG C.
Description
Technical field
The present invention relates to a kind of MnZn soft magnetic ferrite and manufacture method, particularly a kind of MnZn soft-magnetic ferrite core and manufacture method of having the high Bs of high temperature and wide-temperature and low-consumption dual nature concurrently that does not contain Ni.
Background technology
Soft magnetic ferrite is a kind of magneticsubstance that kind is maximum, most widely used, consumption is maximum, is the important foundation functional materials of electronics and information industry.Prevailing in soft magnetic ferrite production and use is the MnZn ferrite, and the ferritic output of MnZn accounts for 70% of soft magnetic ferrite ultimate production, is field of greatest concern and the most active in current soft magnetic materials.In recent years, the development of MnZn Ferrite Material improves by the depth of single performance the horizontal expansion that turns to many index simultaneously to improve.Such as power ferrite material, except the loss of further reduction material, also require more reducing the wastage in wide temperature range, or more reduce the wastage under broadband, or higher saturation magnetic flux density etc.
Existing multinomial technology can laterally be expanded the ferritic performance of MnZn, but is only the horizontal expansion of a few performance mostly.
In method as disclosed as CN1287985A, by adding the cobalt oxide of minor component, make magnetic ferrites materials in the minimum value of the power loss of the temperature province Inner of 20～100 ℃ at 400kW/m
3below, and in the difference of the maximum value of the power loss of the temperature province of 20～100 ℃ and minimum value at 150kW/m
3below.Realized the horizontal expansion of low-loss at wide temperature range, but and the unrealized performance that has high Bs concurrently.
And for example in the disclosed technical scheme of CN1404076A, NiO by a large amount of interpolations up to 3～6mol%, make magnetic core more than the saturation magnetic flux density of 100 ℃ is up to 450mT, but the low loss characteristic sacrifice is too many, the loss under 100kHz, 200mT, 100 ℃ of conditions is up to 550～900kW/m
3.
In the disclosed technical scheme of CN1649039A, by preparing the shaping powder of specific specific surface area, reached and reduced the purpose of power loss, but also only realized low-loss and high Bs for another example, its normal temperature loss is up to 600kW/m
3above, and the performance of unrealized wide-temperature and low-consumption.
The inventor's openly patent of invention CN102682946A is current unique technical scheme of having taken into account the high Bs of high temperature and wide-temperature and low-consumption dual nature, but wherein need to add the oxide compound of the second ancillary component Ni, Ni belongs to precious metal, and prices are rather stiff, and the production cost of Ferrite Material is high.
Summary of the invention
The object of the present invention is to provide a kind of novel MnZn ferrite core material that has the high Bs of high temperature and wide-temperature and low-consumption dual nature concurrently.
Another object of the present invention is to provide the manufacture method of above-mentioned materials.
The technical solution used in the present invention is:
A kind of MnZn ferrite core, be comprised of major ingredient and auxiliary material, the consisting of with Fe of major ingredient
2o
3the meter 53mol%-54mol% ferric oxide, in the manganese oxide of MnO 39mol%-42mol%, in the zinc oxide of ZnO 4mol%-7mol%, three's sum is counted 100 mol%; Auxiliary material comprises the first auxiliary material, the second auxiliary material and the 3rd auxiliary material, wherein, the oxide compound that the first auxiliary material is Co, at ferrite magnetic, content in the heart is 1000～4500ppm for it; The second auxiliary material is the SiO that addition is 30～300 ppm
2with the addition CaCO that is 50～900 ppm
3; The 3rd auxiliary material is selected from MoO
3, TiO
2, SnO
2, Nb
2o
5, V
2o
5, Sm
2o
3, ZrO
2, its addition is 0～1500 ppm.
Preferably, the first auxiliary material is the Co that addition is 1500～4500 ppm
2o
3, the CoO of 1000～4000 ppm or the Co of 1000～4500 ppm
3o
4.
The manufacture method of above-mentioned MnZn ferrite core, comprise the steps:
1) according to the composition of MnZn ferrite core, take major ingredient, or major ingredient and the first auxiliary material, add water and stir, be ground, spraying drying obtains powder, the gained powder is warming up to 800 ℃～1000 ℃ with the heat-up rate of 200～300 ℃/h, is incubated 1～3 hour, the cooling Preburning material of coming out of the stove to obtain;
2) auxiliary material, water, dispersion agent, the defoamer that by Preburning material, not yet add and do not add fully mix, regrind to powder particle size is D50=0.8～1.2 μ m, D90<2.5 μ m, add organic binder bond, mix, spraying drying obtains 60 orders～200 purpose particulate material;
3) aqueous solution of particulate material and organic binder bond is carried out to batch mixing, the water ratio of controlling particulate material is 0.2～0.4%, is pressed into green compact;
4) green sintering, cooling are come out of the stove, grinding, obtain the MnZn ferrite core.
Preferably, the sintered heat insulating temperature of green compact is 1300 ℃～1360 ℃, and the sintered heat insulating time of green compact is 5～10h.
Preferably, adopt the secondary reduction sintering process during green sintering, sintering and temperature-fall period keep equilibrium oxygen partial pres-sure, and further, the calculation formula of equilibrium oxygen partial pres-sure is lg (P (O
2))=a-b/T, wherein, a value 4～15, b value 10000～19000, the kelvin rating that T is holding temperature, 0≤P (O
2)≤21%.
The invention has the beneficial effects as follows:
MnZn ferrite core material of the present invention, overcome conventional MnZn power ferrite material and can't take into account the deficiency of multiple characteristic, have the high Bs of high temperature and wide-temperature and low-consumption dual nature concurrently, this magnetic core is from unit volume loss Pcv(100kHz, the 200mT of 25 ℃～120 ℃) all be less than 350kW/m
3, near 90 ℃, lowest loss is lower than 300kW/m
3, and also there is the saturation magnetic flux density up to 450mT in the time of 100 ℃.This magnetic core, with respect to conventional power ferrite magnetic core, has the dual nature of the high Bs of high temperature and wide-temperature and low-consumption concurrently, is that existing ferrite magnetic is the most all-round a kind of in the heart, and product performance are better than the import hit product, can be widely used in various occasions.
MnZn ferrite core material of the present invention,, containing noble metal Ni, can significantly not reduce the production material cost.
The effect of the first auxiliary material of the present invention is and Fe
2+the magnetocrystalline constant K of the conventional Mn-Zn ferrite of ion hybrid compensation
1, realize K
1value levels off to 0 at wide temperature range Inner, thereby realizes the performance of wide-temperature and low-consumption.The first auxiliary material addition during lower than limited range of the present invention, can't be realized performance index of the present invention, particularly below 60 ℃ and the loss meeting more than 100 ℃ enlarge markedly; When the first auxiliary material addition surpasses limited range of the present invention, will make loss-temperature curve too smooth, and cause the overall losses level to increase, near the loss 90 ℃ can't reach lower than 300kW/m
3level.
The present invention, by controlling the interpolation scope of main formula and the first auxiliary material, has realized that the MnZn ferrite core has the dual nature of high Bs and wide-temperature and low-consumption concurrently.
The effect of second, third auxiliary material of the present invention is to reduce power loss, the raising sintered density of magnetic core.
The accompanying drawing explanation
The loss temperature curve that Fig. 1 is different core materials.
Embodiment
A kind of MnZn ferrite core, be comprised of major ingredient and auxiliary material, the consisting of with Fe of major ingredient
2o
3the meter 53mol%-54mol% ferric oxide, in the manganese oxide of MnO 39mol%-42mol%, in the zinc oxide of ZnO 4mol%-7mol%, three's sum is counted 100 mol%; Auxiliary material comprises the first auxiliary material, the second auxiliary material and the 3rd auxiliary material, wherein, the oxide compound that the first auxiliary material is Co, at ferrite magnetic, content in the heart is 1000～4500ppm for it; The second auxiliary material is the SiO that addition is 30～300 ppm
2with the addition CaCO that is 50～900 ppm
3; The 3rd auxiliary material is selected from MoO
3, TiO
2, SnO
2, Nb
2o
5, V
2o
5, Sm
2o
3, ZrO
2, its addition is 0～1500 ppm.
Preferably, the first auxiliary material is the Co that addition is 1500～4500 ppm
2o
3, the CoO of 1000～4000 ppm or the Co of 1000～4500 ppm
3o
4.
The manufacture method of above-mentioned MnZn ferrite core, comprise the steps:
1) according to the composition of MnZn ferrite core, take major ingredient, or major ingredient and the first auxiliary material, add water and stir, be ground, spraying drying obtains powder, the gained powder is warming up to 800 ℃～1000 ℃ with the heat-up rate of 200～300 ℃/h, is incubated 1～3 hour, the cooling Preburning material of coming out of the stove to obtain;
2) auxiliary material, water, dispersion agent, the defoamer that by Preburning material, not yet add and do not add fully mix, regrind to powder particle size is D50=0.8～1.2 μ m, D90<2.5 μ m, add organic binder bond, mix, spraying drying obtains 60 orders～200 purpose particulate material;
3) aqueous solution of particulate material and organic binder bond is carried out to batch mixing, the water ratio of controlling particulate material is 0.2～0.4%, is pressed into green compact;
4) green sintering, cooling are come out of the stove, grinding, obtain the MnZn ferrite core.
Preferably, the sintered heat insulating temperature of green compact is 1300 ℃～1360 ℃, and the sintered heat insulating time of green compact is 5～10h.
Preferably, adopt the secondary reduction sintering process during green sintering, sintering and temperature-fall period keep equilibrium oxygen partial pres-sure, and further, the calculation formula of equilibrium oxygen partial pres-sure is lg (P (O
2))=a-b/T, wherein, a value 4～15, b value 10000～19000, the kelvin rating that T is holding temperature, 0≤P (O
2)≤21%.
Below in conjunction with embodiment, further illustrate the present invention.
example 1-9
1) adopt commercially available Fe
2o
3, Mn
3o
4, ZnO is as major ingredient, according to the amount shown in table 1 by Fe
2o
3, the MnO(raw material is Mn
3o
4), ZnO and the Co based on major ingredient 2500ppm
2o
3be placed in sand mill, to the water that adds the 90wt% of described powder gross weight in the aforementioned powder taken, stir and ground and mixed even; Speed with 250 ℃/h after spraying drying is warming up to 900 ℃ of lower pre-burning 2h;
2) gross weight of the powder based on after pre-burning adds additive: the Co of 1500ppm
2o
3, 80ppm SiO
2, 500ppm CaCO
3, 200ppm MoO
3, 600ppm TiO
2and the deionized water of 67wt%, the dispersion agent of 1.0wt%, the defoamer of 0.8wt% carry out regrind together, being ground to powder particle size is D50=0.92 μ m, D90<2.3 μ m;
3) gross weight of the powder based on after ball milling, to adding the polyvinyl alcohol solution of 7.5wt% in this powder, mix granulation, adopts 30 tons of dry powder press that particulate material is pressed into to green compact sample;
4) last under the sintering temperature at 1320 ℃ sintering, and be incubated 9 hours under sintering temperature, and being cooled to 180 ℃ and coming out of the stove under balanced atmosphere, the holding-zone oxygen partial pressure adapts to adjustment according to the difference of main formula two peak temperatures, specifically, in Table in 1, temperature-fall period adopts equilibrium oxygen partial pres-sure.
The calculating of two peak temperatures can be with reference to the carrying out of putting down in writing in prior art CN102219486 A.Calculate two peak temperature positions of different main formulas according to two peak calculation formula, the scheme that two peak temperatures are relatively high suitably reduces the holding-zone oxygen partial pressure, the relatively low scheme of two peak temperatures needs suitably to improve the holding-zone oxygen partial pressure, and the amplitude that oxygen partial pressure is adjusted need to be set according to the kiln practical situation.
Adopt the normal temperature inductance L under HP4294A electric impedance analyzer (Agilent Technology 4294A) and unit clamp (Agilent Technology 16047E) measure sample magnet ring 10kHz feeble field, calculate the initial permeability of material; Bs with SY-8258 type B-H tester at 50Hz, 1200A/m, 100 ℃ of lower specimen magnet rings; By the power loss of Model 2335 Watt Meter specimen magnet rings under 100kHz, 200mT, condition of different temperatures, result is listed in table 1.
Table 1
Annotate: numbering is comparative example with the scheme of No. *.
In table 1 example illustrated, 1～5 is the embodiment of the present invention, and 6～9 is comparative example.
Known by the data in table 1:
1) all, within limited range of the present invention, the magnetic core performance index are fully up to standard for embodiment 1～4 major ingredient.
2) comparative example 6～7 is Fe
2o
3content exceeds limited range of the present invention, wherein the Fe of comparative example 6
2o
3content exceeds the present invention and limits lower limit, causes the Bs of 100 ℃ on the low side; The Fe of comparative example 7
2o
3content exceeds the present invention and limits the upper limit, the power loss severe exacerbation.
3) comparative example 8～9 for ZnO content exceeds limited range of the present invention, wherein the ZnO content of comparative example 8 exceeds the present invention and limits the upper limit, the temperature stability of Bs worsens, and causes the Bs of 100 ℃ obviously on the low side; The ZnO content of comparative example 9 exceeds the present invention and limits lower limit, and power loss is higher.
The product of the product of embodiment 3 and TDK company is carried out to performance comparison, record its loss temperature curve.Test-results as shown in Figure 1.As seen from the figure, damage curve and the PC95 of magnetic core of the present invention are suitable, but high temperature Bs is the 410mT of 450mT apparently higher than PC95, are conducive to the power that carrying is larger; High temperature Bs and the PC90 of magnetic core of the present invention are suitable, but the loss temperature curve obviously is better than PC90, and particularly the normal temperature loss is only half of PC90, is conducive to improve the efficiency of electron device; Product performance of the present invention obviously are better than the product of TDK company.
example 10～15
1) with Fe
2o
353.4mol%, MnO 40.3mol%, ZnO 6.3mol% is that the principal constituent formula takes Fe
2o
3, Mn
3o
4, the ZnO starting material are placed in sand mill, to the water that adds the first auxiliary material and the 90wt% based on described powder gross weight in the above-mentioned powder taken, stir and ground and mixed even, the auxiliary material addition is as shown in table 2; Speed with 280 ℃/h after spraying drying is warming up to 1000 ℃ of lower pre-burning 1.5h;
2) gross weight of the powder based on after pre-burning, add remaining auxiliary material according to the addition shown in table 2, add the deionized water of 65wt%, the dispersion agent of 1.2wt%, the defoamer of 0.9wt% to carry out together regrind, being ground to powder particle size is D50=0.85 μ m, D90<2.1 μ m again;
3) gross weight of the powder based on after ball milling, to adding the polyvinyl alcohol solution of 7.9wt% in this powder, mix granulation, adopts 45 tons of dry powder press that particulate material is pressed into to green compact sample;
4) last under the sintering temperature at 1340 ℃ sintering, and insulation 7 hours under sintering temperature, holding-zone oxygen partial pressure 5.5% is cooled to 180 ℃ and comes out of the stove under balanced atmosphere, temperature-fall period adopts equilibrium oxygen partial pres-sure.
Table 2
Adopt the normal temperature inductance L under HP4294A electric impedance analyzer (Agilent Technology 4294A) and unit clamp (Agilent Technology 16047E) measure sample magnet ring 10kHz feeble field, calculate the initial permeability of material; Bs with SY-8258 type B-H tester at 50Hz, 1200A/m, 100 ℃ of lower specimen magnet rings; By the power loss of Model 2335 Watt Meter specimen magnet rings under 100kHz, 200mT, condition of different temperatures, result is listed in table 3.
Table 3
In table 2, table 3 example illustrated, 10～12 is the embodiment of the present invention, and 13～15 is comparative example.
Data in table 2, table 3 are known:
1) embodiment 10～12 dopings are within limited range of the present invention, and the magnetic core performance index are fully up to standard;
Comparative example 13-15 doping exceeds limited range of the present invention: the first auxiliary material Co of comparative example 13 wherein
2o
3the lower limit that addition limits lower than the present invention, K
1value complement is repaid deficiency, fails to realize the wide-temperature and low-consumption characteristic; The first auxiliary material Co of comparative example 14
2o
3the upper limit that addition limits higher than the present invention, K
1value complement is repaid excessively, makes loss-temperature curve too smooth, and overall losses worsens; The second auxiliary material SiO of comparative example 15
2, CaCO
3the lower limit that addition limits lower than the present invention, overall losses is higher.
example 16～18
Raw material composition and preparation, moulding process be with example 11, and difference is that sintering temperature, soaking time, oxygen partial pressure are as shown in table 4.
Adopt the normal temperature inductance L under HP4294A electric impedance analyzer (Agilent Technology 4294A) and unit clamp (Agilent Technology 16047E) measure sample magnet ring 10kHz feeble field, calculate the initial permeability of material; Bs with SY-8258 type B-H tester at 50Hz, 1200A/m, 100 ℃ of lower specimen magnet rings; By the power loss of Model 2335 Watt Meter specimen magnet rings under 100kHz, 200mT, condition of different temperatures, result is listed in table 4.
Table 4
Sintering temperature and soaking time are one section the most key in ferrite sintered temperature curve, it directly has influence on, and whether the material internal solid state reaction is complete, size and the integrity of crystal grain, and sintering temperature and soaking time have certain mutual restriction between the two, mutual compensation that can be to a certain degree.Because sintering temperature and soaking time are mainly that the speed of the solid state reaction of sample and degree are exerted an influence, thereby cause the number of the size of crystal grain and homogeneity, pore and exist form variant, finally causing the performance of sample different.For the MmZn Ferrite Material, in sintering process, also to control sintering atmosphere well, should control the appraising at the current rate of Mn and Fe ion well, control in the ferrite generated and contain a certain amount of Fe again
2+ion, also will prevent Zn
2+the vaporization at high temperature of ion.For different ingredients, required the highest sintering temperature, soaking time and the oxygen partial pressure of the blank that different flouring technologies are prepared is all discrepant.
In table 4 example illustrated, 16～18 is the embodiment of the present invention, and 19～22 is comparative example.
Known by the data in table 4:
1) embodiment 16～18 sintering process conditions are within limited range of the present invention, and the magnetic core performance index are fully up to standard;
2) comparative example 19-20 sintering temperature exceeds limited range of the present invention: the lower limit that wherein sintering temperature of comparative example 19 limits lower than the present invention, the grain growing deficiency, grain-size is less than normal, and sintered density is on the low side, although the wide-temperature and low-consumption characteristic good, Bs is on the low side; Burning, occur in the upper limit that the sintering temperature of comparative example 20 limits higher than the present invention, although crystal grain grow up, due to Fe
2o
3reduction and the volatilization of Zn, the pore of crystal boundary and crystal grain inside expands rapidly, and overall losses is worsened.
3) comparative example 21-22 soaking time exceeds limited range of the present invention: underburnt occurs, the grain size great disparity in the lower limit that wherein soaking time of comparative example 21 limits lower than the present invention, pore is dispersed in crystal boundary and crystal grain inside, make sintered density descend, overall losses is higher, and Bs is on the low side; The upper limit that the soaking time of comparative example 22 limits higher than the present invention, sintering time is long, after the part grain growth, is decomposed into again little crystal grain, causes the grain size great disparity, makes overall losses higher.
The above has exemplarily described the present invention by preferred embodiment, still, should be appreciated that these embodiment are not limiting the scope of the present invention.On the contrary, any modification of doing, be equal to replacement, improvement etc., within all should being included in the protection scope of the present invention be defined by the following claims within purport of the present invention and principle.
Claims (6)
1. one kind containing the MnZn ferrite core that has dual nature concurrently of Ni, consists of the consisting of with Fe of major ingredient major ingredient and auxiliary material
2o
3the meter 53mol%-54mol% ferric oxide, in the manganese oxide of MnO 39mol%-42mol%, in the zinc oxide of ZnO 4mol%-7mol%, three's sum is counted 100 mol%; Auxiliary material is comprised of the first auxiliary material, the second auxiliary material and the 3rd auxiliary material, wherein, the oxide compound that the first auxiliary material is Co, at ferrite magnetic, content in the heart is 1000～4500ppm for it; The second auxiliary material is the SiO that addition is 30～300 ppm
2with the addition CaCO that is 50～900 ppm
3; The 3rd auxiliary material is selected from MoO
3, TiO
2, SnO
2, Nb
2o
5, V
2o
5, Sm
2o
3, ZrO
2, its addition is 0～1500 ppm.
2. MnZn ferrite core according to claim 1, it is characterized in that: the first auxiliary material is the Co that addition is 1500～4500 ppm
2o
3, the CoO of 1000～4000 ppm or the Co of 1000～4500 ppm
3o
4.
3. the manufacture method of the described MnZn ferrite core of claim 1～2 any one, comprise the steps:
1) according to the composition of MnZn ferrite core, take major ingredient, or major ingredient and the first auxiliary material, add water and stir, be ground, spraying drying obtains powder, the gained powder is warming up to 800 ℃～1000 ℃ with the heat-up rate of 200～300 ℃/h, is incubated 1～3 hour, the cooling Preburning material of coming out of the stove to obtain;
2) auxiliary material, water, dispersion agent, the defoamer that by Preburning material, not yet add and do not add fully mix, regrind to powder particle size is D50=0.8～1.2 μ m, D90<2.5 μ m, add organic binder bond, mix, spraying drying obtains 60 orders～200 purpose particulate material;
3) aqueous solution of particulate material and organic binder bond is carried out to batch mixing, the water ratio of controlling particulate material is 0.2～0.4%, is pressed into green compact;
4) green sintering insulation, cooling are come out of the stove, grinding, obtain the MnZn ferrite core.
4. method according to claim 3, it is characterized in that: the sintering temperature of green compact is 1300 ℃～1360 ℃.
5. according to the described method of claim 3 or 4, it is characterized in that: the sintered heat insulating time of green compact is 5～10h.
6. method according to claim 5 is characterized in that: in insulation and temperature-fall period, stove inner equilibrium oxygen partial pressure is controlled according to being formula lg (P (O
2))=a-b/T, wherein, a value 4～15, b value 10000～19000, the kelvin rating that T is holding temperature, 0≤P (O
2)≤21%.
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