CN102219487B - Wide-temperature low-loss MnZn ferrite material and preparation method thereof - Google Patents
Wide-temperature low-loss MnZn ferrite material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a wide-temperature low-loss MnZn ferrite material. The wide-temperature low-loss MnZn ferrite material comprises main ingredients and auxiliary ingredients, wherein the main ingredients comprise 51 to 54 mole percent of ferric oxide, 33 to 41 mole percent of manganese oxide and 8 to 13 mole percent of zinc oxide; the manganese oxide content is counted on the basis of Mn; and the auxiliary ingredients are at least four of 0.02 to 0.06 weight percent of CaCO3, 0.002 to 0.01 weight percent of SiO2, 0.02 to 0.06 weight percent of Nb2O5, 0.01 to 0.05 weight percent of V2O5, 0.20 to 0.50 weight percent of CoO, 0.05 to 0.30 weight percent of NiO, 0.05 to 0.25 weight percent of Ni2O3 and 0.06 to 0.20 weight percent of TiO2 on the basis of the total weight of the main ingredients.
Description
Technical field
The present invention relates to a kind of MnZn Ferrite Material and manufacture method thereof, and relate in particular to a kind of wide-temperature low-loss MnZn ferrite material and manufacture method thereof.
Background technology
Along with electronics arranges lightening development, the Mn-Zn soft magnetic ferrite magneticsubstance obtains using more and more widely in these equipment.Wherein have high magnetic permeability, high Bs, the manganese-zinc ferrite magnetic material of wide-temperature and low-consumption more and more becomes supply transformer, automatization, the indispensable integral part in the communications field.Generally speaking, the magneticsubstance that switching mode power supply transformer uses all comes development and Design and production according to operating ambient temperature (100 ℃), but, a lot of device standby temperature are normal temperature, this material is under normal temperature (25 ℃) ideal case, power consumption penalty is very large, generally up to 600kW/m
3Above, the power consumption when the normal temperature holding state is very serious.
In addition, in industries such as automotive electronics, along with the variation of Working environment, the temperature around the magneticsubstance device is also along with variation, and the power consumption penalty of himself is also along with variation.At communication field, along with the north and south areal variation, four seasons climate change can cause that also the loss of magneticsubstance device oneself power consumption changes.At this moment, just need to have in the wide temperature range, loss is low and change little material, comes assurance equipment under any circumstance can both work.Because the magnetic part major part is in the situation that have large electric current or dc bias field to work, and wishes that also material has high Bs.
Japan TDK company developed wide-temperature and low-consumption material PC95 in 2003, at 100kHz, under the 200mT condition, power consumption is all less than 350kW/m in 25 ℃ of-120 ℃ of temperature ranges
3, Japanese FDK company, the companies such as German EPCOS company, Ferrocube also successively develop similar wide-temperature and low-consumption material, but all do not have performance to reach in 25 ℃ of-140 ℃ of temperature ranges power consumption all less than 350kW/m
3, at 25 ℃, 100 ℃, under the 1200A/m condition, Bs reaches respectively 530mT, similar the reporting for work that 410mT is above.
Summary of the invention
An object of the present invention is to provide a kind of wide-temperature low-loss MnZn ferrite material.
MnZn Ferrite Material of the present invention comprises principal constituent and ancillary component, and wherein said principal constituent is the ferric oxide of 51mol%-54mol%, the manganese oxide of 33mol%-41mol% and the zinc oxide of 8mol%-13mol%, and wherein the content of manganese oxide is in Mn; And described ancillary component is selected from CaCO
3, SiO
2, Nb
2O
5, V
2O
5, CoO, NiO, Ni
2O
3, TiO
2In at least four kinds, based on the gross weight of described principal constituent, CaCO
3: 0.02-0.06wt%, SiO
2: 0.002-0.01wt%, Nb
2O
5: 0.02-0.06wt%, V
2O
5: 0.01-0.05wt%, CoO:0.20-0.50wt%, NiO:0.05-0.30wt%, Ni
2O
3: 0.05-0.25wt%, TiO
2: 0.06-0.20wt%.
The present invention also provides a kind of manufacture method of MnZn Ferrite Material, and the method comprising the steps of:
1) with Fe
2O
3, Mn
3O
4With ZnO evenly mixed and oven dry in described ratio wet-milling;
2) with 800-920 ℃ of lower pre-burning 1-3 of step 1) gained powder hour;
3) to step 2) the gained powder adds at least four kinds of described ancillary components in described ratio, add again to account for the deionized water of the 60wt%-120wt% of described main component gross weight meter, the dispersion agent of 0.5wt%-3wt%, the defoamer of 0.5wt%-3wt% and carry out together ball milling, make the powder particle size behind the ball milling reach 1.0 ± 0.2 μ m;
4) based on the powder gross weight of described step 3) gained, add the organic binder bond of 7wt%-12wt% in the powder of described step 3) gained, mix granulation and get particulate material;
5) pressure of employing 50MPa-200MPa is pressed into green compact sample with particulate material;
6) with green compact sample sintering under 1300 ℃-1350 ℃ sintering temperature of step 5) gained, and under described sintering temperature, be incubated 3-5 hour, then be cooled to 180 ℃ and come out of the stove, wherein the holding-zone oxygen partial pressure is 1%-15%, and temperature-fall period adopts equilibrium oxygen partial pres-sure.
The organic binder bond that uses among the present invention is polyvinyl alcohol.
The dispersion agent that uses among the present invention and defoamer can be dispersion agent and defoamers commonly used in this area, can select n-caprylic acid, stearic acid etc. such as defoamer, and dispersion agent can be selected poly-propionic acid, glyconic acid, citric acid etc.
Equilibrium oxygen partial pres-sure in the inventive method is according to formula lg (P (O
2))=a-b/T calculates, a value 5-10 wherein, and b value 10000～15000, T is absolute temperature.
Wide-temperature and low-consumption MnZn ferrite of the present invention, uniform crystal particles is fine and close, and average grain size is 10 μ m-15 μ m approximately, its magnetic property after tested, index is as follows:
1. wide-temperature and low-consumption MnZn ferrite of the present invention has and is higher than 3000 initial permeability.
2. high Bs low waste MnZn ferrite of the present invention is made OR25 * 8-15mm standard rings, and at 20Ts, 200mT tests loss characteristic under the 100kHz condition, is lower than 350kW/m 25 ℃ of-140 ℃ of losses
3, be lower than 300kW/m 100 ℃ of losses
3
3. wide-temperature and low-consumption MnZn ferrite of the present invention is made OR25 * 8-15mm standard rings, and under the 1194A/m condition, 25 ℃, 100 ℃ Bs is higher than respectively 530mT, 410mT.
The present invention is by adding four or more ancillary component CaCO
3, SiO
2, Nb
2O
5, V
2O
5, CoO, NiO, Ni
2O
3, TiO
2, and addition is optimized combination, utilize at a low price that ion waters down high valence ion to the impact at two peaks, realize that the MnZn Ferrite Material has under the prerequisite of high Bs at normal temperature and high temperature, 25 ℃ of-140 ℃ of losses are lower than 350kW/m
3, be lower than 300kW/m 100 ℃ of losses
3Thereby effectively solved wide temperature range and be difficult to realize low-loss problem.
The present invention is optimized combination to additive and the addition thereof with fusing assistant effect, has effectively reduced sintering temperature, and the highest holding temperature of sintering is reduced to below 1350 ℃.Under relatively low sintering temperature, grain growing is even, fine and close, average grain size is 10 μ m-15 μ m approximately, size to fit, avoided the abnormal growth of crystal grain, thereby produce a kind of MnZn ferrite of wide-temperature and low-consumption, especially in 25 ℃ of-140 ℃ of scopes, show the MnZn ferrite of low loss characteristic.
In addition, utilize the low price ion to water down the high valence ion technology among the present invention, stablized two peak temperatures of material, realize that the MnZn Ferrite Material has under the prerequisite of high Bs at normal temperature and high temperature, in 25 ℃ of-140 ℃ of scopes, reduced MnZn Ferrite Material power consumption, thereby energy efficient is more practical.
The details of one or more embodiments of the present invention has been proposed in the following description.Require from specification sheets and Accessory Right, other features of the present invention, purpose and advantage will be obvious.
Embodiment
Below each material among each embodiment all be commercially available.
Embodiment 1:
Be the Fe of 53.2mol% with principal constituent with sand mill
2O
3, in the Mn of Mn 36.0mol%
3O
4Mix with the ZnO wet-milling of 10.8mol% and to place loft drier to dry.Use chamber type electric resistance furnace, with the gained powder 880 ℃ of lower pre-burnings 2 hours.Then the powder after the pre-burning is put into ball mill, based on the gross weight of described principal constituent, add the CaCO of ancillary component: 0.03wt% in the gained powder
3, 0.006wt% SiO
2, 0.03wt% Nb
2O
5, the CoO of 0.38wt%, the V of 0.04wt%
2O
5, the NiO of 0.15wt%, the Ni of 0.02wt%
2O
3The TiO of 0.15wt%
2Add again to account for the deionized water of the 66wt% of described principal constituent gross weight meter, the dispersion agent of 1wt%, the defoamer of 1wt% and carry out together ball milling.Be about 1.0 ± 0.2 μ m with this powder ball milling to mean particle size; Based on the gross weight of the powder behind the ball milling, add the polyvinyl alcohol solution of 8wt% in this powder, mix granulation, adopt the pressure of 50-200MPa that particulate material is pressed into green compact sample; In the last programme controlled clock hood type furnace of active computer, sintering under 1320 ℃ temperature, and under sintering temperature, be incubated 4.5 hours, and under balanced atmosphere, be cooled to 180 ℃ and come out of the stove, insulation oxygen partial pressure 5.8%, temperature-fall period adopts equilibrium oxygen partial pres-sure.
The material of aforementioned manufacturing is made the standard rings of OR25 * 8-15mm, at 20Ts, 200mT detects initial permeability and power consumption, test b s under the 1194A/m condition under the condition of 100kHz.Detected result is listed in the following table 2, that is: initial permeability: 3332; Be respectively 331.5kW/m 25 ℃, 100 ℃, 140 ℃ losses
3, 303.6kW/m
3, 343.6kW/m
325 ℃, 100 ℃ Bs is respectively 538mT, 415mT.
Embodiment 2-5:
Each component of embodiment 2-5 is referring to following table 1, and implementation step is with above-mentioned embodiment 1.The magnetic property detected result of the material that embodiment 2-5 is prepared is listed in the following table 2.
Comparing embodiment 1-2:
Each component of comparing embodiment 1-2 is referring to following table 1, and implementation step is with above-mentioned embodiment 1.The magnetic property detected result of the material that comparing embodiment 1 is prepared is listed in the following table 2.
Table 1
Annotate:
*The expression ancillary component adds scope and has exceeded preferred interpolation scope of the present invention.
The magnetic property detected result data of embodiment 1-5 and comparing embodiment 1-2 see the following form 2.
Table 2
Annotate:
*The expression ancillary component adds scope and has exceeded preferred interpolation scope of the present invention.
Test out the power consumption of prepared material.As can be seen from Table 2, wide-temperature and low-consumption material of the present invention has higher initial permeability, all is lower than 350kW/m 25 ℃ and 140 ℃ of losses
3, be lower than 300kW/m 100 ℃ loss
3Bs at 25 ℃, 100 ℃ is higher than respectively 530mT and 410mT.The wide temperature range internal loss is very low.
On the basis of principal constituent ferric oxide, manganese oxide and zinc oxide, add ancillary component CaCO
3, SiO
2, Nb
2O
5, V
2O
5, CoO, NiO, Ni
2O
3, TiO
2In at least four kinds.Wherein, SiO
2, CaCO
3Can precipitate into grain boundary layer, increase the grain boundary resistance rate, improve sintered density; Nb
2O
5Has Grain refinement; V
2O
5Be fusing assistant, help solid state sintering, improve sintered density; Co has been adjusted in the interpolation of CoO
2+And Fe
2+Content ratio, make K
1Value levels off to zero, can improve significantly the temperature profile of material, works as Co
2+With Fe
2+Under suitable combination condition, adopt Co
2+With Fe
2+The method of compensation can obtain low-temperature coefficient in very wide temperature range simultaneously; NiO and Ni
2O
3The high valence ion that then utilizes low price ion pair CoO to bring compensates, and guarantees that two peak positions of material are suitable, has the effect that reduces high temperature consumption.TiO
2Can form electron pair by iron ion, be conducive to improve the resistivity of material, reduce the wastage, guarantee that material has practical value.
Described as embodiment 1-5, suitable main formula has added the optimum combination of four or more described ancillary component and ancillary component addition, has effectively realized low loss characteristic in the wide temperature range.Ancillary component with fusing assistant effect has improved sintered density effectively.Under relatively low sintering temperature, grain growing is even, and size to fit has been avoided the abnormal growth of crystal grain, has improved sintered density, has reduced spillage of material.The ion pair high valence ion advances and compensates at a low price, has watered down the impact of high valence ion on material two peak positions, has solved and has reduced the difficult problem that high low temperature loss can not take into account.
Among the comparative example 1-2, ancillary component adds and to exceed optimization range, causes moving behind two peaks of material, and the magnetic permeability of material is low, the loss rising of 25 ℃ and 100 ℃; Excessive interpolation also causes the Bs of material to descend.
Can find out from the above results, the MnZn Ferrite Material of making compared to existing technology, wide-temperature low-loss MnZn ferrite material of the present invention shows and is higher than 3000 initial permeability; At 200mT, under the 100kHz condition, 25 ℃ to 140 ℃ have all shown the wide-temperature and low-consumption characteristic.
Although explained and described the preferred embodiments of the invention, not showing each embodiment explaination and described institute of the present invention might form.Or rather, using the vocabulary in specification sheets is descriptive vocabulary, rather than restrictive vocabulary, and should be appreciated that, can carry out various variations and does not depart from the spirit and scope of the invention that is defined by following claim.
Claims (4)
1. wide-temperature low-loss MnZn ferrite material, it is characterized in that: described MnZn Ferrite Material comprises principal constituent and ancillary component, wherein said principal constituent is the ferric oxide of 51mol%-54mol%, the manganese oxide of 33mol%-41mol% and the zinc oxide of 8-13mol%, and wherein the content of manganese oxide is in Mn; And described ancillary component is selected from CaCO
3, SiO
2, Nb
2O
5, V
2O
5, CoO, NiO, Ni
2O
3, TiO
2In at least four kinds, based on the gross weight of described principal constituent, CaCO
3: 0.02-0.06wt%, SiO
2: 0.002-0.01wt%, Nb
2O
5: 0.02-0.06wt%, V
2O
5: 0.01-0.05wt%, CoO:0.20-0.50wt%, NiO:0.05-0.30wt%, Ni
2O
3: 0.05-0.25wt%, TiO
2: 0.06-0.20wt%, wherein said Ferrite Material be at 20Ts, 200mT, and under the condition of 100kHz, 25 ℃-140 ℃ loss is lower than 350kW/m
3, wherein 100 ℃ loss is lower than 300kW/m
3
2. MnZn Ferrite Material as claimed in claim 1, it is characterized in that: described Ferrite Material is under the 1194A/m condition, and 25 ℃, 100 ℃ Bs is higher than respectively 530mT, 410mT.
3. the manufacture method of a wide-temperature low-loss MnZn ferrite material as claimed in claim 1 is characterized in that: may further comprise the steps:
1) with Fe
2O
3, Mn
3O
4With ZnO evenly mixed and oven dry in described ratio wet-milling;
2) with 800-920 ℃ of lower pre-burning 1-3 of step 1) gained powder hour;
3) to step 2) the gained powder adds at least four kinds of described ancillary components in described ratio, add again to account for the deionized water of the 60wt%-120wt% of described principal constituent gross weight meter, the dispersion agent of 0.5wt%-3wt%, the defoamer of 0.5wt%-3wt% and carry out together ball milling, make the powder particle size behind the ball milling reach 1.0 ± 0.2 μ m;
4) based on the powder gross weight of described step 3) gained, add the organic binder bond of 7wt%-12wt% in the powder of described step 3) gained, mix granulation and get particulate material;
5) pressure of employing 50MPa-200MPa is pressed into green compact sample with particulate material;
6) with green compact sample sintering under 1300 ℃-1360 ℃ sintering temperature of step 5) gained, and under described sintering temperature, be incubated 3-5 hour, then be cooled to 180 ℃ and come out of the stove, wherein the holding-zone oxygen partial pressure is 1%-15%, and temperature-fall period adopts equilibrium oxygen partial pres-sure.
4. manufacture method as claimed in claim 3, it is characterized in that: the described organic binder bond in the described step 4) is polyvinyl alcohol.
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| CN101241791A (en) * | 2007-02-06 | 2008-08-13 | 昆山尼赛拉电子器材有限公司 | Wide-temperature and low-consumption Mn-Zn soft magnetic ferrite and its production method |
| CN101409124A (en) * | 2008-08-02 | 2009-04-15 | 广东风华高新科技股份有限公司 | MnZn ferrite material and method for preparing magnet core |
| CN101857427B (en) * | 2009-04-08 | 2012-10-10 | 广东江粉磁材股份有限公司 | High-frequency low-loss MnZn ferrite material and manufacturing method thereof |
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