CN107352993A - A kind of high frequency Mn-Zn soft magnetic ferrite and preparation method thereof - Google Patents

A kind of high frequency Mn-Zn soft magnetic ferrite and preparation method thereof Download PDF

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Publication number
CN107352993A
CN107352993A CN201710568388.9A CN201710568388A CN107352993A CN 107352993 A CN107352993 A CN 107352993A CN 201710568388 A CN201710568388 A CN 201710568388A CN 107352993 A CN107352993 A CN 107352993A
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soft magnetic
high frequency
magnetic ferrite
preparation
principal component
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刘培元
傅膑
张凯
孔令才
谢振华
赵辉
李俊
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RUYUAN DONG YANG GUANG MATERIALS CO Ltd
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RUYUAN DONG YANG GUANG MATERIALS CO Ltd
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    • C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
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    • C04B35/2633—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead containing barium, strontium or calcium
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    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
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Abstract

The present invention relates to a kind of high frequency Mn-Zn soft magnetic ferrite and preparation method thereof, the high frequency Mn-Zn soft magnetic ferrite includes the principal component of following content：Fe2O3：54.5~57.5mol%, MnO：37~40mol%, ZnO：5.3~5.8mol%；Gross weight with respect to principal component also includes the additive of following content：Ca2CO3：0.1~0.2wt%, NiO：0.5~1.0wt%, Nb2O5：0.01~0.05wt%, SnO2：0.01~0.06wt%, Bi2O3：0.02~0.06wt%, Co2O3：0.2~0.3wt%.Compared to prior art, high frequency Mn-Zn soft magnetic ferrite of the present invention has obtained many liftings in terms of the parameters such as Chang Gaowen saturation flux densities, high-frequency loss.

Description

A kind of high frequency Mn-Zn soft magnetic ferrite and preparation method thereof
Technical field
The present invention relates to electronic equipment and its preparing technical field, more particularly to a kind of high-frequency low-consumption high magnetic flux density, Mn-Zn soft magnetic ferrite of high-curie temperature and preparation method thereof.
Background technology
Social informatization constantly advances, along with to electronic product device efficient, high frequency, miniaturized application Tight demand, higher and higher requirement, high DC stacked Ferrite Material are proposed with Ferrite Material therein to application The ability of anti-D.C. magnetic field interference can be improved, high saturation magnetic flux density is advantageous to device miniaturization.Possess higher Curie's temperature Degree is applied to wider use temperature range after being easy to miniaturization, can not be timely after reduction device small space or planarization heating The risk of device cisco unity malfunction caused by radiating.
Usual device need to integrate to work with together with other devices on circuit boards, at work inevitably by other The interference of the DC fields of device output, disturbed by the different magnetic field that other device works are formed, device such as wants normal work, needs The antijamming capability of itself, such as inductor are improved, need to be under the magnetic field of interference, the inductance of itself, which can not have, significantly to be fallen, It need to ensure to remain to keep enough inductance values normal work together with other devices under disturbance.
Therefore, it is badly in need of working out one kind while possesses high saturation magnetic flux density, high-curie temperature, high DC stacked performance Manganese-zinc ferrite, it can possess high resistivity simultaneously, can be applied to higher frequency range, it is possible to achieve device it is small-sized Change, integrated, multifunction.
The content of the invention
The invention aims to overcome the deficiencies in the prior art, there is provided a kind of high frequency Mn-Zn soft magnetic ferrite, The soft magnetic materials is respectively provided with higher saturation flux density in normal temperature and high temperature, be particularly suitable for high-frequency, high current it is a variety of Realize more stable inductive function in application scenario.
It is a further object to provide a kind of preparation method of above-mentioned high frequency Mn-Zn soft magnetic ferrite.
The present invention is made up of following technical scheme：A kind of high frequency Mn-Zn soft magnetic ferrite, includes following content Principal component：Fe2O3：54.5~57.5mol%, MnO：37~40mol%, ZnO：5.3~5.8mol%；With respect to principal component Gross weight also includes the additive of following content：Ca2CO3：0.1~0.2wt%, NiO：0.5~1.0wt%, Nb2O5：0.01~ 0.05wt%, SnO2：0.01~0.06wt%, Bi2O3：0.02~0.06wt%, Co2O3：0.2~0.3wt%.
Further, under 1190A/m test conditions, the saturation magnetic of high frequency Mn-Zn soft magnetic ferrite at 25 DEG C Flux density Bs reaches 542mT~549mT, and its residual flux density Br is 107mT~117mT, the saturation of soft magnetic materials at 100 DEG C Magnetic flux density Bs reaches 454mT~458mT, and its residual flux density Br is 111mT~116mT.It can be seen that the high frequency MnZn soft magnet oxygen Body material is respectively provided with higher saturation flux density in normal temperature and high temperature.
Further, the Curie temperature Tc of the high frequency Mn-Zn soft magnetic ferrite reaches 300 DEG C, and its density p= 4.76 × 103kg/m3~4.81 × 103kg/m3.It can be seen that the high frequency Mn-Zn soft magnetic ferrite has higher Curie's temperature Degree.
Further, under 1M, 50MT test condition, the power damage of 25 DEG C of the high frequency Mn-Zn soft magnetic ferrite Consumption Pcv is 145mW/cm3~175mW/cm3, the loss Pcv of 100 DEG C of the soft magnetic materials is 176mW/cm3~195mW/ cm3.It can be seen that the high frequency Mn-Zn soft magnetic ferrite has relatively low loss.
Compared to prior art, high-frequency low-consumption high magnetic flux density of the invention, the MnZn soft magnet oxygen of high-curie temperature Body material, using ternary system main formula, and coordinate and add additive combination, ternary system composition of raw materials therein is follow-up combination Additive make basis, additive combination plays auxiliary and facilitation so that the green compact of compacting be easy to sintering, crystal grain it is uniform, gas Porosity reduces, and sintered density improves, and then obtains high-frequency low-consumption high magnetic flux density, the Mn-Zn soft magnetic ferrite of high-curie temperature Material.Compared to existing soft magnetic materials, high frequency Mn-Zn soft magnetic ferrite of the present invention is in Chang Gaowen saturation flux densities, height In terms of the parameters such as frequency loss, many liftings have been obtained.Therefore, high frequency Mn-Zn soft magnetic ferrite of the invention can be with more Stable DC stacked conformability, broader temperature applicable range, ensure that applied device is more stably run, especially It is adapted to promoting the use of in many occasions such as DC stacked inductors very big, frequency is higher.
The invention further relates to a kind of preparation method of above-mentioned high frequency Mn-Zn soft magnetic ferrite, comprise the following steps：
S1：Principal component is matched by mole content, deionized water is then added in sand mill is mixed Close and broken, PVA solution is added after recycling mixing；
S2：Pre-burning is carried out by being put into after the principal component drying of broken mixing in pre-burning stove；
S3：Additive combination is added to the principal component through pre-burning, is then put into the powder that principal component combines with additive Deionized water, PVA and defoamer are added in sand mill and carries out secondary sand milling, the levigate powder that granularity is 0.60~0.8 μm is made；
S4：Levigate powder is subjected to mist projection granulating, 50~200 μm of spraying powder is made；Then will spray powder pressing Shaping, it is 2.95~3.05g/cm that density, which is made,3Sample ring green compact；
S5：Green compact are sintered into sizing in nitrogen protection atmosphere stove under 1150~1180 DEG C of temperature conditionss, made after cooling Obtain the high frequency Mn-Zn soft magnetic ferrite.
Compared to prior art, the preparation method of high frequency Mn-Zn soft magnetic ferrite of the present invention is in ternary system On the basis of formula, matching component formula promotes crystal grain refinement, homogenization distribution, by the mixed once of three kinds of raw material, in advance Burn, add additive combination after it is secondary mixing, shaping, sintering etc. step, it is simple and direct, efficiently production be made there is higher saturation magnetic Flux density is high DC stacked, the Mn-Zn soft magnetic ferrite of high-curie temperature；On sintering process：By controlling heating speed Rate, with slow heating, further the densification of rush guarantor crystal grain grows；Protected by warming-up section nitrogen and carry out densification sintering, to control material Pore opening and quantity in material；Proper extension soaking time, promote solid phase reaction is complete, grain growth uniformly, reduce stomata and Out-phase；With obtain high density, high saturation magnetic flux density Mn-Zn soft magnetic ferrite.Soft magnetism made from preparation method of the present invention Material is particularly suitable in DC stacked applications very big, frequency is higher.
Further, crushed in step S1 and continue 40~50min, circulation mixing continues 10~20min.
Further, for temperature control at 880~950 DEG C, pre-burning stove insulation continues 2~3h in pre-burning stove in step S2.
Further, the secondary sand milling duration is 120~150min in step S3.
Further, in step S4, using shaping hydraulic press, H12.5-7.5-5.0 sample rings are suppressed.
Further, in step S5, in nitrogen protection atmosphere stove, oxygen content 0.5-1.0%, surplus is nitrogen；Cooling It is to be carried out in controlled nitrogen oxygen atmosphere, is cooled to room temperature.
Embodiment
Embodiment 1：
The Mn-Zn soft magnetic ferrite of the present embodiment is made according to following processing step：
1st, dispensing：
By mole weighing Fe2O3For three kinds of raw materials that 56mol%, MnO 38.5mol%, ZnO are 5.5mol%, Then certain proportion deionized water is added in sand mill and carries out mixing and breaking up, crushed 50 minutes, carry out 15 points of circulation mixing A certain amount of PVA solution is added after clock, carries out mist projection granulating.
2nd, pre-burning：
Spraying material is put into pre-burning stove, 2 hours are incubated at 920 DEG C and carries out pre-burning.
3rd, secondary sand milling：
The following auxiliary element for pressing Preburning material (raw material) percentage by weight is added in Preburning material：Ca2CO3For 0.1wt%, NiO is 1.0wt%, Nb2O5For 0.03wt%, SnO2For 0.04wt%, Bi2O3For 0.05wt%, Co2O3For 0.3wt%.Then Powder is put into sand mill and adds the secondary sand milling of deionized water progress, it is 150 minutes that the time, which is sanded, and powder particles control exists 0.6~0.8 μm.
4th, mist projection granulating and shaping：
A certain proportion of PVA and defoamer are added in secondary sand milling, mist projection granulating is then carried out in spray tower into 50 ~200 μm of particle；Then it is molded, sample ring green density is in 3.00g/cm3Left and right；
5th, sinter：
Under nitrogen protection atmosphere, 5 hours are incubated under 1160 DEG C of temperature conditionss and is sintered, room is cooled under nitrogen protection Temperature.
The sample sintered is tested with the rugged SY8218 and HP4284A inductance instrument of rock, specific performance is shown in Table 1：
The test result of sintered sample in the embodiment 1 of table 1
From table 1 it follows that under the conditions of 1194A/m, high frequency Mn-Zn soft magnetic ferrite 25 made from embodiment 1 DEG C Bs be 543mT, 100 DEG C of Bs is 456mT.Therefore the material is well positioned to meet in 25 DEG C~100 DEG C temperature ranges The DC stacked requirement to magnetic material, it is a kind of soft ferromagnetic powder of the high DC stacked characteristic of high saturation magnetic flux density.
Embodiment 2：
1st, dispensing：
By mole weighing Fe2O3For 55.7mol%, MnO 38.8mol%, ZnO 5.5mol%, three kinds of originals Material, certain proportion deionized water is then added in sand mill and carries out mixing and breaking up, is crushed 50 minutes, carries out circulation mixing 15 A certain amount of PVA solution is added after minute, carries out mist projection granulating.
2nd, pre-burning：
Spraying material is put into pre-burning stove, 2 hours are incubated at 880 DEG C and carries out pre-burning.
3rd, secondary sand milling：
The following auxiliary element for pressing Preburning material percentage by weight is added in Preburning material：Ca2CO3It is for 0.2wt%, NiO 1.0wt%, Nb2O5For 0.05wt%, SnO2For 0.04wt%, Bi2O3For 0.02wt%, Co2O3For 0.15wt%.Then by powder Material, which is put into sand mill, to be added deionized water and carries out secondary sand milling, and it is 150 minutes that the time, which is sanded, powder particles control 0.6~ 0.8μm。
4th, mist projection granulating and shaping：
A certain proportion of PVA and defoamer are added in secondary sand milling, mist projection granulating is then carried out in spray tower into 50 ~200 μm of particle；Then it is molded, sample ring green density is in 3.00g/cm3Left and right；
5th, sinter：
Under nitrogen protection atmosphere, 5 hours are incubated under 1150 DEG C of temperature conditionss and is sintered, room is cooled under nitrogen protection Temperature.
The sample sintered is tested with the rugged SY8218 and HP4284A inductance instrument of rock, specific performance is shown in Table 2：
The test result of sintered sample in the embodiment 2 of table 2
From Table 2, it can be seen that under the conditions of 1194A/m, high frequency Mn-Zn soft magnetic ferrite 25 made from embodiment 2 DEG C Bs be 542mT, 100 DEG C of Bs is 454mT.Therefore the material is well positioned to meet in 25 DEG C~100 DEG C temperature ranges The DC stacked requirement to magnetic material, it is a kind of soft ferromagnetic powder of the high DC stacked characteristic of high saturation magnetic flux density.
Embodiment 3：
1st, dispensing：
By mole weighing Fe2O3For 54.5mol%, MnO 39.7mol%, ZnO 5.8mol%, three kinds of originals Material, certain proportion deionized water is then added in sand mill and carries out mixing and breaking up, is crushed 50 minutes, carries out circulation mixing 15 A certain amount of PVA solution is added after minute, carries out mist projection granulating.
2nd, pre-burning：
Spraying material is put into pre-burning stove, 2 hours are incubated at 880 DEG C and carries out pre-burning.
3rd, secondary sand milling：
The following auxiliary element for pressing Preburning material percentage by weight is added in Preburning material：Ca2CO3It is for 0.1wt%, NiO 0.5wt%, Nb2O5For 0.03wt%, SnO2For 0.06wt%, Bi2O3For 0.05wt%, Co2O3For 0.3wt%.Then by powder Material, which is put into sand mill, to be added deionized water and carries out secondary sand milling, and it is 120 minutes that the time, which is sanded, powder particles control 0.6~ 0.8μm。
4th, mist projection granulating and shaping：
A certain proportion of PVA and defoamer are added in secondary sand milling, mist projection granulating is then carried out in spray tower into 50 ~200 μm of particle；Then it is molded, sample ring green density is in 3.00g/cm3Left and right；
5th, sinter：
Under nitrogen protection atmosphere, 5 hours are incubated under 1160 DEG C of temperature conditionss and is sintered, room is cooled under nitrogen protection Temperature.
The sample sintered is tested with the rugged SY8218 and HP4284A inductance instrument of rock, specific performance is shown in Table 3：
The test result of sintered sample in the embodiment 3 of table 3
From table 3 it is observed that under the conditions of 1194A/m, high frequency Mn-Zn soft magnetic ferrite 25 made from embodiment 3 DEG C Bs be 543mT, 100 DEG C of Bs is 456mT.Therefore the material is well positioned to meet in 25 DEG C~100 DEG C temperature ranges The DC stacked requirement to magnetic material, it is a kind of soft ferromagnetic powder of the high DC stacked characteristic of high saturation magnetic flux density.
Comparative example
Compared with above-mentioned 3 embodiments, the respective performances of the typical soft ferromagnetic powder of tradition are as shown in the following Table 4：
The performance of the traditional soft ferromagnetic powder comparative example of table 4
It can be demonstrate,proved with the contrast of table 1~3 item by item by the properties of upper table 4：The present invention soft magnetic materials it is DC stacked require compared with Various application occasions high, frequency is higher, have higher, more stable inductive function.
Using traditional in high frequency Mn-Zn soft magnetic ferrite made from the embodiment of the present invention 1,2,3 and comparative example Soft ferromagnetic powder is pressed into UU magnetic core products, and inductance coil is made, respectively under 25 DEG C, 100 DEG C of operating temperature, Direct current is superimposed on to inductance coil, meanwhile, direct current~inductive data such as He of table 5 of each inductance coil is measured using inductance measuring meter Shown in 6.Superimposed current before generally dropping into superimposed current using inductance in the industry during inductance 60% or so is bordering on mistake as magnetic core performance The critical current of effect.
As can be seen from Table 5,25 DEG C when all magnetic core products 60% inductance value be about 2.62 μ H, from table it can be seen that Critical current corresponding to UU26 magnetic cores sample inductance value made from the embodiment of the present invention 1~3 is 24A, and traditional UU26 magnetic cores Critical current corresponding to the sample inductance value is 19A, and the difference rate for calculating the two critical current is (24A-19A)/19A*100= 26.3%.
As can be seen from Table 6,100 DEG C when all magnetic core products 60% inductance value be about 2.62 μ H, can from table It is 18A to critical current corresponding to UU26 magnetic cores sample made from the embodiment of the present invention 1~3, and traditional UU26 magnetic cores sample pair The critical current answered is 16A, and the difference rate for calculating the two critical current is (28A-16A)/16A*100=12.5%.
Sequitur is contrasted by table 5 and table 6, the DC superposition characteristic of soft magnetic ferrite of the present invention is better than traditional sample really Product.And the every as shown by data of the above：The DC superposition characteristic of material of the present invention is excellent, in addition higher saturation flux density and compared with Low residual magnetic flux density, relatively low high-frequency loss, it can preferably meet high Bs, Gao Zhi in 25 DEG C~100 DEG C wide temperature ranges Stream superposition, the material property requirement of low high-frequency loss；The high frequency Mn-Zn soft magnetic ferrite of the present invention is in the folded big, frequency of direct current High various application occasions, there is higher, more stable inductive function, more than the work for the design device that client can be increased considerably Amount, the stability and service life for increasing electronic device, also help the miniaturization of device and reduce cost.
The preferred embodiments of the present invention are these are only, are not intended to limit the invention, for those skilled in the art For member, any modification, equivalent substitution and improvements done within the spirit and principles of the invention etc., this should be included in Within the protection domain of invention.

Claims (10)

1. a kind of high frequency Mn-Zn soft magnetic ferrite, include the principal component of following content：Fe2O3：54.5~57.5mol%, MnO：37~40mol%, ZnO：5.3~5.8mol%；Gross weight with respect to principal component also includes the additive of following content： Ca2CO3：0.1~0.2wt%, NiO：0.5~1.0wt%, Nb2O5：0.01~0.05wt%, SnO2：0.01~0.06wt%, Bi2O3：0.02~0.06wt%, Co2O3：0.2~0.3wt%.
2. high frequency Mn-Zn soft magnetic ferrite according to claim 1, it is characterised in that：In 1190A/m test conditions Under, the saturation flux density Bs of the high frequency Mn-Zn soft magnetic ferrite reaches 542mT~549mT at 25 DEG C, and its remanent magnetism is close Degree Br is 107mT~117mT, and the saturation flux density Bs of the soft magnetic materials reaches 454mT~458mT at 100 DEG C, its remanent magnetism Density Br is 111mT~116mT.
3. high frequency Mn-Zn soft magnetic ferrite according to claim 1, it is characterised in that：The high frequency MnZn soft magnet The Curie temperature Tc of ferrite reaches 300 DEG C, its density p=4.76 × 103kg/m3~4.81 × 103kg/m3。
4. high frequency Mn-Zn soft magnetic ferrite according to claim 1, it is characterised in that：In 1M, 50MT test condition Under, the power attenuation Pcv of 25 DEG C of the high frequency Mn-Zn soft magnetic ferrite is 145mW/cm3~175mW/cm3, 100 DEG C The loss Pcv of the soft magnetic materials is 176mW/cm3~195mW/cm3。
5. a kind of preparation method of high frequency Mn-Zn soft magnetic ferrite as described in any one of Claims 1 to 4, including it is following Step：
S1：Principal component is matched by mole content, then in sand mill add deionized water carry out mixing and It is broken, add PVA solution after recycling mixing；
S2：Pre-burning is carried out by being put into after the principal component drying of broken mixing in pre-burning stove；
S3：Additive combination is added to the principal component through pre-burning, the powder that principal component combines with additive is then put into sand milling Deionized water, PVA and defoamer are added in machine and carries out secondary sand milling, the levigate powder that granularity is 0.60~0.8 μm is made；
S4：Levigate powder is subjected to mist projection granulating, 50~200 μm of spraying powder is made；Then the powder that will spray is compressing, It is 2.95~3.05g/cm that density, which is made,3Sample ring green compact；
S5：Green compact are sintered into sizing in nitrogen protection atmosphere stove under 1150~1180 DEG C of temperature conditionss, institute is made after cooling State high frequency Mn-Zn soft magnetic ferrite.
6. preparation method according to claim 5, it is characterised in that：Crushed in step S1 and continue 40~50min, circulation is mixed Conjunction continues 10~20min.
7. preparation method according to claim 5, it is characterised in that：In step S2 in pre-burning stove temperature control 880~ 950 DEG C, pre-burning stove insulation continues 2~3h.
8. preparation method according to claim 5, it is characterised in that：In step S3 it is secondary sand milling the duration be 120~ 150min。
9. preparation method according to claim 5, it is characterised in that：In step S4, using shaping hydraulic press, compacting H12.5-7.5-5.0 sample rings.
10. preparation method according to claim 5, it is characterised in that：In step S5, in nitrogen protection atmosphere stove, oxygen contains It is nitrogen to measure as 0.5-1.0%, surplus；Cooling is carried out in controlled nitrogen oxygen atmosphere, is cooled to room temperature.
CN201710568388.9A 2017-07-13 2017-07-13 A kind of high frequency Mn-Zn soft magnetic ferrite and preparation method thereof Pending CN107352993A (en)

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CN107540360A (en) * 2016-06-25 2018-01-05 临沂春光磁业有限公司 It is a kind of that there is high saturated magnetic induction, high DC stacked Ferrite Material
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CN109851346A (en) * 2018-12-29 2019-06-07 乳源东阳光磁性材料有限公司 A kind of high frequency Mn-Zn soft magnetic ferrite and its preparation method and application
CN109851346B (en) * 2018-12-29 2022-06-17 乳源东阳光磁性材料有限公司 High-frequency manganese-zinc soft magnetic ferrite material and preparation method and application thereof
CN110436911A (en) * 2019-08-20 2019-11-12 乳源东阳光磁性材料有限公司 A kind of soft magnetic materials and preparation method thereof and the application in automobile electronic system
CN113284731A (en) * 2021-05-17 2021-08-20 湖北微硕电子科技有限公司 High-frequency large-magnetic-field soft magnetic ferrite material and preparation method thereof
CN115745588A (en) * 2022-09-23 2023-03-07 西南应用磁学研究所(中国电子科技集团公司第九研究所) Manganese-zinc ferrite material with high performance factor and preparation method thereof
CN115745588B (en) * 2022-09-23 2023-11-03 西南应用磁学研究所(中国电子科技集团公司第九研究所) High-performance factor manganese zinc ferrite material and preparation method thereof
CN116444259A (en) * 2023-03-20 2023-07-18 乳源东阳光磁性材料有限公司 High-frequency high-direct-current superimposed low-loss manganese zinc ferrite material and preparation method thereof
CN116891376A (en) * 2023-08-07 2023-10-17 广东肇庆微硕电子有限公司 Bias-reduction-resistant lean iron-manganese-zinc ferrite material and preparation method thereof

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