CN110467450A - A kind of high frequency Mn-Zn soft magnetic ferrite and its preparation method and application - Google Patents

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

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CN110467450A
CN110467450A CN201910769236.4A CN201910769236A CN110467450A CN 110467450 A CN110467450 A CN 110467450A CN 201910769236 A CN201910769236 A CN 201910769236A CN 110467450 A CN110467450 A CN 110467450A
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high frequency
soft magnetic
magnetic ferrite
principal component
preparation
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刘培元
傅膑
张凯
孔令才
李俊
谢振华
万里云
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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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Abstract

The invention discloses a kind of high frequency Mn-Zn soft magnetic ferrites and its preparation method and application.The high frequency material includes principal component and accessory ingredient, and wherein principal component includes Fe2O3, MnO, ZnO, NiO, the accessory ingredient component are as follows: Ca2CO3、V2O5、Nb2O5、Bi2O3、Co2O3.High frequency Mn-Zn soft magnetic ferrite of the invention in main formula by introducing nickel protoxide, as quaternary formula system, Ni Zn ferrimagnet system is incorporated i.e. in manganese-zinc ferrite system, so as to preferably control the resistivity of product grains size and product, to reduce product high-frequency loss, make product saturation flux density with higher and higher Curie temperature, it is particularly suitable for the high frequency environment of 2MHz~4MHz, preparation method is by control calcined temperature, sintering temperature and powder particle size, to be conducive to improve saturation flux density and reduce function loss.

Description

A kind of high frequency Mn-Zn soft magnetic ferrite and its preparation method and application
Technical field
The present invention relates to technical field of electronic materials, more particularly, to a kind of high frequency Mn-Zn soft magnetic ferrite and Preparation method and application.
Background technique
And with the extension of the development of electronics industry and application field, the requirement to magnetic material is also higher and higher, and right The classificating requirement of material property more refines and specialization, and the working frequency of Ferrite Material is higher and higher, has reached at present The high frequency of 1~3MHZ.And the outdoor facilities such as current communication devices and automobile require experience high temperature and low during the work time Temperature environment, it is ensured that these equipment can normal use, just necessarily require using core material from -20 DEG C to 100 of low temperature DEG C all there is very high magnetic conductivity, and power loss is low.Currently, the applicable frequency of manganese-zinc ferrite is relatively low, CN101857427A A kind of high-frequency low-loss MnZn ferrite material and its manufacturing method are disclosed, is a kind of manganese-zinc ferrite material of ternary system Material, and material, under conditions of 500kHz, 25~120 DEG C of loss is 70kW/m3, it is unable to reach high saturation magnetic flux density and low The material requirements of power loss.Therefore, this field is it is contemplated that provide a kind of high frequency ring that can be applied to 2MHZ~4MHZ Border, while soft magnetic ferrite can also have high saturation magnetic flux density and low power capabilities, meet current communication base station, service The requirement to Ferrite Material performance such as device.
Summary of the invention
The technical problem to be solved by the present invention is to overcome existing Mn-Zn soft magnetic ferrites cannot be applicable in 2MHZ~4MHZ High frequency condition defect and deficiency, a kind of high frequency Mn-Zn soft magnetic ferrite is provided, specific manganese-zinc ferrite system is passed through It is merged with Ni Zn ferrimagnet system, to reach the promotion of good core material comprehensive performance.
Another object of the present invention is to provide a kind of preparation methods of high frequency Mn-Zn soft magnetic ferrite.
Another object of the present invention is to provide a kind of high frequency Mn-Zn soft magnetic ferrite in communication base station, server Application.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
A kind of high frequency Mn-Zn soft magnetic ferrite, including principal component and accessory ingredient, wherein principal component includes following mole The component of percentage: Fe2O354~56%, MnO 38~40%, ZnO 4.5~5.5%, the accessory ingredient of NiO 0.5~1% The mass percent of component are as follows: Ca2CO30.05~0.15%, V2O50.01~0.06%, Nb2O50.01~0.05%, Bi2O30.01~0.03%, Co2O30.1~0.3%, the mass percent of accessory ingredient is relative to principal component gross mass Percentage.
High frequency Mn-Zn soft magnetic ferrite of the invention introduces nickel protoxide in main formula, becomes quaternary formula System, i.e., be melted into Ni Zn ferrimagnet system, the control of control and product resistivity to product grains size in manganese-zinc ferrite system Fixture has preferable effect, to reduce product high-frequency loss.
High frequency material of the invention is mainly used for 2MHz to 4MHz range, in 3MHz, 10mT, the power consumption at 80 DEG C Level is lower than 50mW/cm3, in the case where 3MHz, 30mT, power consumption levels are lower than 500mW/cm at 80 DEG C3, have excellent Power consumption levels and higher saturation flux density.
Wherein, Fe of the invention2O3, MnO, ZnO and NiO quaternary component content determination basis are as follows:
Preferably, the density of the high frequency Mn-Zn soft magnetic ferrite is 4.70~4.80g/cm3, control the close of material Degree obtains small crystallite dimension.It such as can be 4.70g/cm3, 4.75g/cm3Or 4.80g/cm3。
Preferably, the grain size of the high frequency Mn-Zn soft magnetic ferrite is 2.5~4.5 μm, controls crystallite dimension In one-domain structure, high frequency eddy current losses are reduced.It such as can be 2.5 μm, 3.5 μm, 4.5 μm or 3 μm.
Preferably, the resistivity of the high frequency Mn-Zn soft magnetic ferrite is 15~20 ρ (Ω .m).High resistivity has Conducive to reduction high frequency eddy current losses.It such as can be 15 ρ (Ω .m), 18 ρ (Ω .m) or 20 ρ (Ω .m).
As a kind of implementation of the invention, above-mentioned high frequency Mn-Zn soft magnetic ferrite can be made by the following method It is standby to obtain:
S1: matching principal component by mole content, and mixing is broken, and it is molten that polyvinyl alcohol is added after circulation mixing Liquid is pre-sintered after drying；
S2: the principal component being pre-sintered in S1 combining second-time breakage with accessory ingredient, and the mill that partial size is 0.5~0.7 μm is made Fine powder material；
S3: levigate powder is subjected to mist projection granulating, 50~200 μm of spraying powder is made；It then will spraying powder pressing Molding, it is 3.0~3.1g/cm that density, which is made,3Green compact；
S4: under inert gas protection by green compact described in S3, it is sintered sizing at 1130~1160 DEG C, institute is made after cooling State high frequency Mn-Zn soft magnetic ferrite.
In powder production, material of the invention by average grain diameter control than conventional small, 0.6um or so (D50), it is conventional to produce Product, cannot be too big convenient for the control final crystal grain of product in 0.9um or so, to control the high frequency eddy current losses of product.Such as S2 In levigate powder particle size can be 0.5 μm, 0.55 μm, 0.65 μm or 0.7 μm.
In product sintering, control product sintering temperature at 1130~1160 DEG C, make the control of product final densities 4.7~ 4.80g/cm3.It such as can be 4.7g/cm3、4.75g/cm3Or 4.80g/cm3。
Preferably, the heating rate of sintering sizing described in S3 is 1~2 DEG C/min.
Preferably, it is 40~50min that the time is crushed described in S1, and circulation incorporation time is 10~20min.
Preferably, pre-sintering temperature described in S1 is 880~920 DEG C, keeps the temperature 2~3h.With conventional manganese-zinc power ferrite It compares, the calcined temperature of preparation method of the invention is 880~920 DEG C, higher than conventional 860~880 DEG C, is on the one hand conducive to It is saturated the raising of magnet density, is on the other hand conducive to the consistency control of powder particle diameter.Such as can for 880 DEG C, 890 DEG C, 900 DEG C or 920 DEG C.
Preferably, pre-sintering heating rate described in S1 is 2~2.5 DEG C/min.
Preferably, second-time breakage time described in S3 is 180~240min.
Preferably, H12.5-7.5-5.0 sample ring is suppressed using molding hydraulic press in S3.
A kind of high frequency Mn-Zn soft magnetic ferrite prepare communication base station, the application in server is also in guarantor of the invention It protects in range.High frequency magnetic core material of the invention is particularly suitable for the high frequency environment of 2MHZ~4MHZ, can be widely applied to prepare Communication base station, server etc..
Compared with prior art, the beneficial effects of the present invention are:
(1) the present invention provides a kind of high frequency Mn-Zn soft magnetic ferrites, by introducing nickel protoxide in main formula, As quaternary formula system, i.e., in manganese-zinc ferrite system incorporate Ni Zn ferrimagnet system, product grains size at 2.5~4.5 μm, Resistivity is 15~20 ρ (Ω .m), and density is 4.70~4.80g/cm3, at 80 DEG C, 3MHz, 10mT power consumption levels are lower than 50mW/ cm3, at 80 DEG C, 3MHz, 30mT power consumption levels are lower than 500mW/cm3。
(2) preparation method of high frequency Mn-Zn soft magnetic ferrite of the invention, by controlling calcined temperature, sintering temperature The resistivity of product is reduced so as to preferably control product grains size with the control of powder grain, to reduce product height Frequency is lost, and so that product is had lower power consumption levels and higher saturation flux density, is particularly suitable for the height of 2MHz~4MHz Frequency environment.
Specific embodiment
The present invention is further illustrated With reference to embodiment, but embodiment the present invention is not done it is any The restriction of form.Unless otherwise indicated, source chemicals used in the embodiment of the present invention are the source chemicals routinely bought.
Embodiment 1
A kind of high frequency magnetic core material, raw material include principal component and accessory ingredient, and wherein principal component includes following Mole percent The component of ratio: Fe2O355%, MnO 39%, ZnO 4.5%, NiO 0.5%, the mass percent of accessory ingredient component are as follows: Ca2CO30.08%, V2O50.03%, Nb2O50.02%, Bi2O30.02%, Co2O30.15%, the quality hundred of accessory ingredient Divide than being the percentage relative to principal component gross mass.
Embodiment 2
A kind of high frequency magnetic core material, raw material include principal component and accessory ingredient, and wherein principal component includes following Mole percent The component of ratio: Fe2O356%, MnO 38%, ZnO 4.5%, NiO 0.5%, the mass percent of accessory ingredient component are as follows: Ca2CO30.1%, V2O50.03%, Nb2O50.02%, Bi2O30.02%, Co2O3The quality percentage of 0.2% its accessory ingredient Than being the percentage relative to principal component gross mass.
Embodiment 3
A kind of high frequency magnetic core material, raw material include principal component and accessory ingredient, and wherein principal component includes following Mole percent The component of ratio: Fe2O355%, MnO 39%, ZnO 4.5%, NiO 1%, the mass percent of accessory ingredient component are as follows: Ca2CO3 0.1%, V2O50.03%, Nb2O50.03%, Bi2O30.01%, Co2O3The mass percent of 0.3% its accessory ingredient is phase For the percentage of principal component gross mass.
Embodiment 4
A kind of high frequency magnetic core material, raw material include principal component and accessory ingredient, and wherein principal component includes following Mole percent The component of ratio: Fe2O355.5%, MnO 38%, ZnO 5.5%, NiO 0.5%, the mass percent of accessory ingredient component are as follows: Ca2CO30.05%, V2O50.02%, Nb2O50.02%, Bi2O30.03%, Co2O30.15%, the quality hundred of accessory ingredient Divide than being the percentage relative to principal component gross mass.
Embodiment 5
A kind of high frequency magnetic core material, raw material include principal component and accessory ingredient, and wherein principal component includes following Mole percent The component of ratio: Fe2O354%, MnO 40%, ZnO 5%, NiO 0.5%, the mass percent of accessory ingredient component are as follows: Ca2CO3 0.1%, V2O50.03%, Nb2O50.02%, Bi2O30.02%, Co2O30.25%, the mass percent of accessory ingredient is Percentage relative to principal component gross mass.
Embodiment 6
A kind of preparation method of the high frequency magnetic core material of embodiment 1, includes the following steps:
S1: matching principal component by mole content, and mixing is broken, and it is molten that polyvinyl alcohol is added after circulation mixing Liquid is pre-sintered after drying, and pre-sintering temperature is 920 DEG C, and heating rate is 2 DEG C/min；
S2: the principal component being pre-sintered in S1 combining second-time breakage with accessory ingredient, and the pulverized powder that granularity is 0.65 μm is made Material；
S3: levigate powder is subjected to mist projection granulating, 100 μm of spraying powder is made；Then it will be sprayed powder compression moulding, It is 2.95g/cm that density, which is made,3Green compact；
S4: under inert gas protection by green compact described in S3, it is sintered sizing at 1160 DEG C, the high frequency is made after cooling Mn-Zn soft magnetic ferrite, the density of high frequency magnetic material are 4.75g/cm3, the crystal grain of high frequency Mn-Zn soft magnetic ferrite is big Small is 4 μm, and resistivity is 15 ρ (Ω .m).
Embodiment 7
A kind of preparation method of the high frequency magnetic core material of embodiment 1, includes the following steps:
S1: matching principal component by mole content, and mixing is broken, and it is molten that polyvinyl alcohol is added after circulation mixing Liquid is pre-sintered after drying, and pre-sintering temperature is 880 DEG C, and heating rate is 2 DEG C/min；
S2: the principal component being pre-sintered in S1 combining second-time breakage with accessory ingredient, and the pulverized powder that granularity is 0.55 μm is made Material；
S3: levigate powder is subjected to mist projection granulating, 50 μm of spraying powder is made；Then it will be sprayed powder compression moulding, It is 2.95g/cm that density, which is made,3Green compact；
S4: under inert gas protection by green compact described in S3, it is sintered sizing at 1130 DEG C, the high frequency is made after cooling Mn-Zn soft magnetic ferrite, the density of high frequency magnetic material are 4.75g/cm3, the crystal grain of high frequency Mn-Zn soft magnetic ferrite is big Small is 3 μm, and resistivity is 18 ρ (Ω .m).
Embodiment 8
A kind of preparation method of the high frequency magnetic core material of embodiment 1, includes the following steps:
S1: matching principal component by mole content, and mixing is broken, and it is molten that polyvinyl alcohol is added after circulation mixing Liquid is pre-sintered after drying, and pre-sintering temperature is 900 DEG C, and heating rate is 2 DEG C/min；
S2: the principal component being pre-sintered in S1 combining second-time breakage with accessory ingredient, and the pulverized powder that granularity is 0.65 μm is made Material；
S3: levigate powder is subjected to mist projection granulating, 50 μm of spraying powder is made；Then it will be sprayed powder compression moulding, It is 2.95g/cm that density, which is made,3Green compact；
S4: under inert gas protection by green compact described in S3, it is sintered sizing at 1130 DEG C, the high frequency is made after cooling Mn-Zn soft magnetic ferrite, the density of high frequency magnetic material are 4.7g/cm3, the crystal grain of high frequency Mn-Zn soft magnetic ferrite is big Small is 2.5 μm, and resistivity is 20 ρ (Ω .m).
Embodiment 9
A kind of preparation method of the high frequency magnetic core material of embodiment 1, includes the following steps:
S1: matching principal component by mole content, and mixing is broken, and it is molten that polyvinyl alcohol is added after circulation mixing Liquid is pre-sintered after drying, and pre-sintering temperature is 890 DEG C, and heating rate is 2 DEG C/min；
S2: the principal component being pre-sintered in S1 combining second-time breakage with accessory ingredient, and the pulverized powder that granularity is 0.65 μm is made Material；
S3: levigate powder is subjected to mist projection granulating, 50 μm of spraying powder is made；Then it will be sprayed powder compression moulding, It is 2.95g/cm that density, which is made,3Green compact；
S4: under inert gas protection by green compact described in S3, it is sintered sizing at 1140 DEG C, the high frequency is made after cooling Mn-Zn soft magnetic ferrite, the density of high frequency magnetic material are 4.75g/cm3, the crystal grain of high frequency Mn-Zn soft magnetic ferrite is big Small is 3 μm, and resistivity is 20 ρ (Ω .m).
As a result it detects
The performance of the high frequency magnetic core material of embodiment 1 is detected, testing result is as shown in table 1.Wherein Bs is saturation Magnetic flux density, Pv are power loss.
Power consumption data detection method are as follows: use the rugged SY8218 instrument test of rock.
Testing result is shown in Table 1.
Table 1
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all this Made any modifications, equivalent replacements, and improvements etc., should be included in the claims in the present invention within the spirit and principle of invention Protection scope within.

Claims (10)

1. a kind of high frequency Mn-Zn soft magnetic ferrite, which is characterized in that including principal component and accessory ingredient, wherein principal component includes The component of following molar percentage: Fe2O354~56%, MnO 38~40%, ZnO 4.5~5.5%, 0.5~1% institute of NiO State the mass percent of accessory ingredient component are as follows: Ca2CO30.05~0.15%, V2O50.01~0.06%, Nb2O50.01~ 0.05%, Bi2O30.01~0.03%, Co2O30.1~0.3%, the mass percent of accessory ingredient is relative to principal component The percentage of gross mass.
2. high frequency Mn-Zn soft magnetic ferrite as described in claim 1, which is characterized in that the high frequency Mn-Zn soft magnetic ferrite The density of material is 4.70~4.80g/cm3。
3. high frequency Mn-Zn soft magnetic ferrite as claimed in claim 2, which is characterized in that the high frequency Mn-Zn soft magnetic ferrite The grain size of material is 2.5~4.5 μm.
4. high frequency Mn-Zn soft magnetic ferrite as claimed in claim 3, which is characterized in that the high frequency Mn-Zn soft magnetic ferrite The resistivity of material is 15~20 ρ (Ω .m).
5. a kind of preparation method of high frequency Mn-Zn soft magnetic ferrite described in Claims 1 to 4 any one, feature exist In including the following steps:
S1: matching principal component by mole content, and mixing is broken, and poly-vinyl alcohol solution is added after circulation mixing, It is pre-sintered after drying；
S2: the principal component being pre-sintered in S1 combining second-time breakage with accessory ingredient, and the pulverized powder that partial size is 0.5~0.7 μm is made Material；
S3: levigate powder is subjected to mist projection granulating, 50~200 μm of spraying powder is made；Then it will be sprayed powder compression moulding, It is 3.0~3.10g/cm that density, which is made,3Green compact；
S4: under inert gas protection by green compact described in S3, it is sintered sizing at 1130~1160 DEG C, the height is made after cooling Frequency Mn-Zn soft magnetic ferrite.
6. preparation method according to claim 5, which is characterized in that being crushed the time described in S1 is 40~50min, circulation Incorporation time is 10~20min.
7. preparation method according to claim 5, which is characterized in that pre-sintering temperature described in S1 is 880~920 DEG C, Keep the temperature 2~3h.
8. preparation method according to claim 5, which is characterized in that second-time breakage time described in S3 be 180~ 240min。
9. preparation method according to claim 5, which is characterized in that using molding hydraulic press in S3, suppress H12.5- 7.5-5.0 sample ring.
10. high frequency Mn-Zn soft magnetic ferrite described in a kind of Claims 1 to 4 any one is preparing communication base station, service Application in device, which is characterized in that the frequency in the communication base station, server is 2MHZ~4MHZ.
CN201910769236.4A 2019-08-20 2019-08-20 A kind of high frequency Mn-Zn soft magnetic ferrite and its preparation method and application Withdrawn CN110467450A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113024240A (en) * 2021-05-17 2021-06-25 湖北微硕新材料有限公司 High-superposition and high-permeability ferrite material and preparation method thereof
CN115286378A (en) * 2022-07-06 2022-11-04 东台市杰磁电子有限公司 High-strength soft magnetic ferrite magnetic core

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113024240A (en) * 2021-05-17 2021-06-25 湖北微硕新材料有限公司 High-superposition and high-permeability ferrite material and preparation method thereof
CN113024240B (en) * 2021-05-17 2021-12-07 湖北微硕新材料有限公司 High-superposition and high-permeability ferrite material and preparation method thereof
CN115286378A (en) * 2022-07-06 2022-11-04 东台市杰磁电子有限公司 High-strength soft magnetic ferrite magnetic core

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