CN108129143A - High superimposed characteristics wide temperature low-power consumption Mn-Zn soft magnetic ferrite and preparation method thereof - Google Patents

High superimposed characteristics wide temperature low-power consumption Mn-Zn soft magnetic ferrite and preparation method thereof Download PDF

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CN108129143A
CN108129143A CN201810049072.3A CN201810049072A CN108129143A CN 108129143 A CN108129143 A CN 108129143A CN 201810049072 A CN201810049072 A CN 201810049072A CN 108129143 A CN108129143 A CN 108129143A
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power consumption
soft magnetic
magnetic ferrite
oxygen
wide temperature
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CN108129143B (en
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黄有东
李申华
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Nantong Sanjia Magnetic Industry Co ltd
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CHANGSHU SANJIA MAGNETIC Co Ltd
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Abstract

The invention discloses a kind of high superimposed characteristics wide temperature low-power consumption Mn-Zn soft magnetic ferrite and preparation method thereof, including host component and doping component；Host component includes Fe2O3 68.5~69.8wt%, 4.2~4.8wt% of ZnO, surplus MnO, total amount 100%；Doping component includes NiO, CaCO3、Nb2O5、TiO2、SnO2、Co2O3、Ta2O5、K2CO3And Li2CO3；Doping component accounts for 2~4wt% of host component.The present invention is on the basis of formula adjusts, regulated and controled by grinding micronized particles material and appropriate pre-burning and sintering forming process twice, effectively reduce stomata quantity, and so that crystal grain is fully refined, the probability of irregular big crystal grain is reduced, effectively improves the power attenuation and superimposed characteristics of Mn-Zn soft magnetic ferrite, the density of material of gained is big, Curie temperature is high, Applicable temperature is wide, has excellent performance.

Description

High superimposed characteristics wide temperature low-power consumption Mn-Zn soft magnetic ferrite and preparation method thereof
Technical field
The present invention relates to soft magnetic ferrite field, more particularly to a kind of high superimposed characteristics wide temperature low-power consumption MnZn soft magnet Oxysome and preparation method thereof.
Background technology
MnZn Ferrite Materials have both excellent soft magnet performance and high resistivity double grading, excellent combination property, so There is very extensive purposes and application prospect, and be the preferred soft magnetism material when these fields are applied in medium, high frequency field One of material.In recent years in high frequency switch power field as power material（That is magnetic core of transformer）, soft magnetism MnZn ferrite materials Material has obtained very extensive application, and its usage amount is also increasing year by year.
At present, as voltage device is to smaller, more light-weighted development, higher requirement is also proposed to Ferrite Material, It is required that it has wide temperature using characteristic, is superimposed performance, and it is especially DC stacked to have excellent performance, in addition should also have excellent height The low magnetic hystersis loss of temperature is specific.Soft magnetic ferrite prepared by prior art method, scanned Electronic Speculum observation, in crystal grain and on crystal boundary There are many stomatas, and there are also excrescent coarse grains, lead to the micro-structure lack of homogeneity of soft magnetic ferrite.
Invention content
The invention mainly solves the technical problem of providing a kind of high superimposed characteristics wide temperature low-power consumption Mn-Zn soft magnetic ferrites And preparation method thereof, the excellent superimposed characteristics of core material and relatively low high temperature power consumption can be assigned, while improve its micro-structure.
In order to solve the above technical problems, one aspect of the present invention is：A kind of wide temperature of high superimposed characteristics is provided Low-consumption Mn-Zn soft magnetic ferrite, including：Host component and doping component；The host component includes following mass percentage Ingredient：Fe2O3 68.5~69. 8%, ZnO 4.2~4.8%, surplus MnO, total amount 100%；The doping component includes NiO、CaCO3、Nb2O5、TiO2、SnO2、Co2O3、Ta2O5、K2CO3And Li2CO3；Wherein, the doping component accounts for the main body group Divide the 2~4% of gross mass.
In a preferred embodiment of the present invention, in the doping component, the NiO accounts for the doping component gross mass 50~65%；The Co2O3Account for the 8~10% of the doping component gross mass；The CaCO3、Nb2O5、TiO2、SnO2、Ta2O5、 K2CO3And Li2CO3It is identical in quality.
In a preferred embodiment of the present invention, the Fe2O3Purity for 99.8%, specific surface area 4.3m2/g；It is described The purity of MnO is more than 99.8%, specific surface area 16.8m2/g。
In order to solve the above technical problems, another technical solution used in the present invention is：It is wide to provide a kind of high superimposed characteristics The preparation method of temperature low-power consumption Mn-Zn soft magnetic ferrite, includes the following steps：
（1）Weighing：Host component is weighed by formula ratio and doping component is spare；
（2）Primary grinding：By NiO, CaCO in the host component and doping component of formula ratio3、K2CO3、Li2CO3It is added to ball It in grinding machine, adds in deionized water and carries out ball-milling treatment, dried after taking-up, obtain the mixture that average grain diameter is 1~3 μm；
（3）Pre-burning：By step（2）The middle mixed material after primary grinding and drying is added in pre-burning stove, and preheating obtains Preburning powdered material；
（4）Secondary grinding：To step（3）In add in the Nb in doping component in obtained pre-burning powder2O5、TiO2、SnO2、Ta2O5 And Co2O3, then add in deionized water and carry out ball-milling treatment, take out, drying, obtain the mixing that average grain diameter is 0.5~0.8 μm Material；
（5）Base：To step（4）Binding sizing agent is added in the middle mixture through obtained by secondary grinding, after mixing, cake of press is ground Broken and the sieve of 35~45 mesh excessively, the particle airing aftershaping after sieving are base sample；
（6）Sinter molding：By step（5）The base sample of middle gained is put into clock hood type furnace, and heating burning is carried out under certain partial pressure of oxygen Knot and cooling down processing, obtain the high DC stacked characteristic MnZn ferrite material of the wide temperature low-power consumption.
In a preferred embodiment of the present invention, the step（2）In, the mass ratio of the material, ball and deionized water is 1 : 3.5~4: 1.2~1.5；The time of the ball-milling treatment is more than 6h；The step（4）In, the material, ball and deionized water Mass ratio be 1: 3.5~4: 0.8~1.0；The time of the ball-milling treatment is more than 12h.
In a preferred embodiment of the present invention, the step（3）In, the process conditions of the preheating are：Air Under atmosphere, 2~3h of Isothermal sinter, then passes to nitrogen at 950~1000 DEG C, and it is being 5~8% to make partial pressure of oxygen, is cooled to stove 500 DEG C, then it is 2~3% to control partial pressure of oxygen, continues to be cooled to room temperature.
In a preferred embodiment of the present invention, the step（5）In, the binding sizing agent is that mass concentration is 6~8% PVA slurries, add in quality account for the 8~10% of the host component and doping component gross mass.
In a preferred embodiment of the present invention, the step（6）In, the sintering process conditions are：First in air gas In atmosphere, 650 DEG C are risen to from room temperature with the heating rate of 1~1.5 DEG C/min, then under conditions of partial pressure of oxygen is 0.05%, with 2 The heating rate of~3 DEG C/min rises to 1000 DEG C from 650 DEG C, then adjusts oxygen and be depressed into 1%, with the heating rate of 5~8 DEG C/min 1150 DEG C are risen to from 1000 DEG C, then 1380 DEG C are warming up to from 1150 DEG C with the heating rate of 10 DEG C/min, keeps the temperature 3.5~6.5h； Under 1~3% partial pressure of oxygen, 1100 DEG C are cooled to from 1380 DEG C with the rate of temperature fall of 2~2.5 DEG C/min for temperature-fall period, then Partial pressure of oxygen is 0.5~1.5%, 500 DEG C is down to from 1100 DEG C with the rate of temperature fall of 5~8 DEG C/min, finally with 0.01~0.05% Partial pressure of oxygen, the near room temperature of rate of 2.5~3 DEG C/min.
The beneficial effects of the invention are as follows：A kind of preparation of high superimposed characteristics wide temperature low-power consumption Mn-Zn soft magnetic ferrite of the present invention Method on the basis of formula adjusts, is regulated and controled by grinding micronized particles material and appropriate pre-burning and sintering forming process twice, Stomata quantity is effectively reduced, and so that crystal grain is fully refined, the probability of irregular big crystal grain is reduced, effectively improves manganese The power attenuation and superimposed characteristics of Zn soft magnetic ferrite material, its excellent DC superposition characteristic are effectively improved, the material of gained Expect that density is big, Curie temperature is high, Applicable temperature is wide, has excellent performance.
Specific embodiment
The preferred embodiments of the present invention will be described in detail below so that advantages and features of the invention can be easier to by It will be appreciated by those skilled in the art that so as to make a clearer definition of the protection scope of the present invention.
The embodiment of the present invention includes：
Embodiment 1
Present invention is disclosed a kind of high superimposed characteristics wide temperature low-power consumption Mn-Zn soft magnetic ferrite, including：Host component and doping group Point；The host component includes the ingredient of following mass percentage：Fe2O3 68.5%th, ZnO 4.2%, MnO 27.3；It is described to mix Miscellaneous component includes NiO, CaCO3、Nb2O5、TiO2、SnO2、Co2O3、Ta2O5、K2CO3And Li2CO3；Wherein, the doping component accounts for The 2% of the host component gross mass.Specifically, in doping component, the NiO accounts for the 50% of the doping component gross mass；Institute State Co2O3Account for the 8% of the doping component gross mass；The CaCO3、Nb2O5、TiO2、SnO2、Ta2O5、K2CO3And Li2CO3Matter It measures identical.
Wherein, raw materials are high-purity, and with high specific surface area, ensure that magnetic core has high saturation flux Density Bs and low power consumption.Specifically, the Fe2O3Purity for 99.8%, specific surface area 4.3m2/g；The purity of the MnO More than 99.8%, specific surface area 16.8m2/g。
The preparation method of above-mentioned high superimposed characteristics wide temperature low-power consumption Mn-Zn soft magnetic ferrite, includes the following steps：
（1）Weighing：Host component is weighed by formula ratio and doping component is spare；
（2）Primary grinding：By NiO, CaCO in the host component and doping component of formula ratio3、K2CO3、Li2CO3It is added to ball In grinding machine, adding in deionized water makes the mass ratio of material, ball and deionized water be 1: 3.5: 1.2, and then more than ball-milling treatment 6h, takes It is dried after going out, obtains the mixture that average grain diameter is 1~3 μm；
（3）Pre-burning：By step（2）The middle mixed material after primary grinding and drying is added in pre-burning stove, under air atmosphere, Isothermal sinter 2h, then passes to nitrogen at 950 DEG C, and it is being 5% to make partial pressure of oxygen, and 500 DEG C are cooled to stove, then controls the partial pressure of oxygen to be 2%, continue to be cooled to room temperature, obtain preburning powdered material；
（4）Secondary grinding：To step（3）In add in the Nb in doping component in obtained pre-burning powder2O5、TiO2、SnO2、Ta2O5 And Co2O3, deionized water is then added in, makes the mass ratio of material, ball and deionized water for 1: 3.5: 0.8, more than ball-milling treatment 12h, It takes out, drying, obtains the mixture that average grain diameter is 0.5~0.8 μm；
（5）Base：To step（4）Addition accounts for the host component in the middle mixture through obtained by secondary grinding and doping component is total The PVA slurries that 80% mass concentration of quality is 6% are as binding sizing agent, and after mixing, cake of press pulverizes and crosses 35~45 mesh Sieve, the particle airing aftershaping after sieving are base sample；
（6）Sinter molding：By step（5）The base sample of middle gained is put into clock hood type furnace, and heating burning is carried out under certain partial pressure of oxygen Knot and cooling down processing, obtain the high DC stacked characteristic MnZn ferrite material of the wide temperature low-power consumption.The sintering process Condition is：First in air atmosphere, 650 DEG C are risen to from room temperature with the heating rate of 1 DEG C/min, is then 0.05% in partial pressure of oxygen Under conditions of, 1000 DEG C are risen to from 650 DEG C with the heating rate of 2 DEG C/min, then adjust oxygen and be depressed into 1%, with the liter of 5 DEG C/min Warm rate rises to 1150 DEG C from 1000 DEG C, then 1380 DEG C are warming up to from 1150 DEG C with the heating rate of 10 DEG C/min, keeps the temperature 3.5h； Under 1% partial pressure of oxygen, 1100 DEG C are cooled to, then be in partial pressure of oxygen with the rate of temperature fall of 2 DEG C/min from 1380 DEG C for temperature-fall period 0.5%, 500 DEG C are down to from 1100 DEG C with the rate of temperature fall of 5 DEG C/min, finally with 0.015% partial pressure of oxygen, the speed of 2.5 DEG C/min The near room temperature of rate.
Embodiment 2
Present invention is disclosed a kind of high superimposed characteristics wide temperature low-power consumption Mn-Zn soft magnetic ferrite, including：Host component and doping group Point；The host component includes the ingredient of following mass percentage：Fe2O3 69.8%th, ZnO 4.8%, MnO 25.4；It is described to mix Miscellaneous component includes NiO, CaCO3、Nb2O5、TiO2、SnO2、Co2O3、Ta2O5、K2CO3And Li2CO3；Wherein, the doping component accounts for The 4% of the host component gross mass.Specifically, in doping component, the NiO accounts for the 65% of the doping component gross mass；Institute State Co2O3Account for the 10% of the doping component gross mass；The CaCO3、Nb2O5、TiO2、SnO2、Ta2O5、K2CO3And Li2CO3's It is identical in quality.
Wherein, raw materials are high-purity, and with high specific surface area, ensure that magnetic core has high saturation flux Density Bs and low power consumption.Specifically, the Fe2O3Purity for 99.8%, specific surface area 4.3m2/g；The purity of the MnO More than 99.8%, specific surface area 16.8m2/g。
The preparation method of above-mentioned high superimposed characteristics wide temperature low-power consumption Mn-Zn soft magnetic ferrite, includes the following steps：
（1）Weighing：Host component is weighed by formula ratio and doping component is spare；
（2）Primary grinding：By NiO, CaCO in the host component and doping component of formula ratio3、K2CO3、Li2CO3It is added to ball In grinding machine, adding in deionized water makes the mass ratio of material, ball and deionized water be 1: 4: 1.5, and then more than ball-milling treatment 6h, takes out After dry, it is 1~3 μm of mixture to obtain average grain diameter；
（3）Pre-burning：By step（2）The middle mixed material after primary grinding and drying is added in pre-burning stove, under air atmosphere, Isothermal sinter 2h, then passes to nitrogen at 1000 DEG C, and it is being 8% to make partial pressure of oxygen, and 500 DEG C are cooled to stove, then controls the partial pressure of oxygen to be 3%, continue to be cooled to room temperature, obtain preburning powdered material；
（4）Secondary grinding：To step（3）In add in the Nb in doping component in obtained pre-burning powder2O5、TiO2、SnO2、Ta2O5 And Co2O3, deionized water is then added in, the mass ratio for making material, ball and deionized water is 1: 4: 1.0, and more than ball-milling treatment 12h takes Go out, dry, obtain the mixture that average grain diameter is 0.5~0.8 μm；
（5）Base：To step（4）Addition accounts for the host component in the middle mixture through obtained by secondary grinding and doping component is total The PVA slurries that 10% mass concentration of quality is 8% are as binding sizing agent, and after mixing, cake of press is pulverized and is sieved, and sieve is 35~45 mesh, the particle airing aftershaping after sieving are base sample；
（6）Sinter molding：By step（5）The base sample of middle gained is put into clock hood type furnace, and heating burning is carried out under certain partial pressure of oxygen Knot and cooling down processing, obtain the high DC stacked characteristic MnZn ferrite material of the wide temperature low-power consumption.The sintering process Condition is：First in air atmosphere, 650 DEG C are risen to from room temperature with the heating rate of 1.5 DEG C/min, is then in partial pressure of oxygen Under conditions of 0.05%, 1000 DEG C are risen to from 650 DEG C with the heating rate of 3 DEG C/min, then adjust oxygen and be depressed into 1%, with 8 DEG C/min Heating rate rise to 1150 DEG C from 1000 DEG C, then 1380 DEG C are warming up to from 1150 DEG C with the heating rate of 10 DEG C/min, heat preservation 6.5h；Under 3% partial pressure of oxygen, 1100 DEG C are cooled to, then in oxygen with the rate of temperature fall of 2.5 DEG C/min from 1380 DEG C for temperature-fall period It is 1.5% to divide, and 500 DEG C are down to from 1100 DEG C with the rate of temperature fall of 8 DEG C/min, finally with 0.05% partial pressure of oxygen, 3 DEG C/min's The near room temperature of rate.
The high superimposed characteristics wide temperature low-power consumption Mn-Zn soft magnetic ferrite that the above method obtains, after tested, density 4.98g/ cm3, the initial permeability at 25 DEG C is more than or equal to 3050；Power attenuation at 100KHZ, 200mT, 25 DEG C is less than 425KW/ m3；Power attenuation at 100KHZ, 200mT, 100 DEG C is less than 325KW/m3；Curie temperature is more than or equal to 240 DEG C；1194A/m, 25 The saturation flux density that saturation flux density at DEG C is higher than at 550mT, 1194A/m, 100 DEG C is higher than 480mT；In 1KHZ, 0.3V, room temperature under the conditions of adding electric current 6A, are detected using 4284A inductance bridges tester, and inductance is 2.8~3.8mH, is superimposed Inductance is 41~44 μ H.
The Mn-Zn soft magnetic ferrite of gained of the invention, on the basis of formula adjusts, by grinding refinement twice Pellet and appropriate pre-burning and sintering forming process regulation and control, effectively reduce stomata quantity, and so that crystal grain is fully refined, and subtract The probability of few irregular big crystal grain, effectively improves the power attenuation and superimposed characteristics of Mn-Zn soft magnetic ferrite, excellent Its DC superposition characteristic is effectively improved, and the density of material of gained is big, Curie temperature is high, and Applicable temperature is wide, has excellent performance.
The foregoing is merely the embodiment of the present invention, are not intended to limit the scope of the invention, every to utilize this hair The equivalent structure or equivalent flow shift that bright description is made directly or indirectly is used in other relevant technology necks Domain is included within the scope of the present invention.

Claims (8)

1. a kind of high superimposed characteristics wide temperature low-power consumption Mn-Zn soft magnetic ferrite, which is characterized in that including：Host component and doping group Point；The host component includes the ingredient of following mass percentage：Fe2O3 68.5~69. 8%, ZnO 4.2~4.8%, it is remaining It measures as MnO, total amount 100%；The doping component includes NiO, CaCO3、Nb2O5、TiO2、SnO2、Co2O3、Ta2O5、K2CO3With Li2CO3；Wherein, the doping component accounts for the 2~4% of the host component gross mass.
2. high superimposed characteristics wide temperature low-power consumption Mn-Zn soft magnetic ferrite according to claim 1, which is characterized in that described to mix In miscellaneous component, the NiO accounts for the 50~65% of the doping component gross mass；The Co2O3Account for the 8 of the doping component gross mass ~10%；The CaCO3、Nb2O5、TiO2、SnO2、Ta2O5、K2CO3And Li2CO3It is identical in quality.
3. high superimposed characteristics wide temperature low-power consumption Mn-Zn soft magnetic ferrite according to claim 1, which is characterized in that described Fe2O3Purity for 99.8%, specific surface area 4.3m2/g；More than 99.8%, specific surface area is the purity of the MnO 16.8m2/g。
It is 4. a kind of such as the preparation side of the high superimposed characteristics wide temperature low-power consumption Mn-Zn soft magnetic ferrite of claim 1-3 any one of them Method, which is characterized in that include the following steps：
（1）Weighing：Host component is weighed by formula ratio and doping component is spare；
（2）Primary grinding：By NiO, CaCO in the host component and doping component of formula ratio3、K2CO3、Li2CO3It is added to ball It in grinding machine, adds in deionized water and carries out ball-milling treatment, dried after taking-up, obtain the mixture that average grain diameter is 1~3 μm；
（3）Pre-burning：By step（2）The middle mixed material after primary grinding and drying is added in pre-burning stove, and preheating obtains Preburning powdered material；
（4）Secondary grinding：To step（3）In add in the Nb in doping component in obtained pre-burning powder2O5、TiO2、SnO2、Ta2O5 And Co2O3, then add in deionized water and carry out ball-milling treatment, take out, drying, obtain the mixing that average grain diameter is 0.5~0.8 μm Material；
（5）Base：To step（4）Binding sizing agent is added in the middle mixture through obtained by secondary grinding, after mixing, cake of press is ground Broken and the sieve of 35~45 mesh excessively, the particle airing aftershaping after sieving are base sample；
（6）Sinter molding：By step（5）The base sample of middle gained is put into clock hood type furnace, and heating burning is carried out under certain partial pressure of oxygen Knot and cooling down processing, obtain the high DC stacked characteristic MnZn ferrite material of the wide temperature low-power consumption.
5. the preparation method of high superimposed characteristics wide temperature low-power consumption Mn-Zn soft magnetic ferrite according to claim 4, feature It is, the step（2）In, the mass ratio of the material, ball and deionized water is 1: 3.5~4: 1.2~1.5；At the ball milling The time of reason is more than 6h；The step（4）In, the mass ratio of the material, ball and deionized water for 1: 3.5~4: 0.8~ 1.0；The time of the ball-milling treatment is more than 12h.
6. the preparation method of high superimposed characteristics wide temperature low-power consumption Mn-Zn soft magnetic ferrite according to claim 4, feature It is, the step（3）In, the process conditions of the preheating are：Under air atmosphere, constant temperature is burnt at 950~1000 DEG C 2~3h of knot, then passes to nitrogen, and it is being 5~8% to make partial pressure of oxygen, and 500 DEG C are cooled to stove, then it is 2~3% to control partial pressure of oxygen, after It is continuous to be cooled to room temperature.
7. the preparation method of high superimposed characteristics wide temperature low-power consumption Mn-Zn soft magnetic ferrite according to claim 4, feature It is, the step（5）In, the binding sizing agent is the PVA slurries that mass concentration is 6~8%, adds in quality and accounts for the master The 8~10% of body component and doping component gross mass.
8. the preparation method of high superimposed characteristics wide temperature low-power consumption Mn-Zn soft magnetic ferrite according to claim 4, feature It is, the step（6）In, the sintering process conditions are：First in air atmosphere, with the heating rate of 1~1.5 DEG C/min 650 DEG C are risen to from room temperature, then under conditions of partial pressure of oxygen is 0.05%, is risen to the heating rate of 2~3 DEG C/min from 650 DEG C 1000 DEG C, then adjust oxygen and be depressed into 1%, 1150 DEG C are risen to from 1000 DEG C, then with the heating rate of 5~8 DEG C/min with 10 DEG C/min Heating rate be warming up to 1380 DEG C from 1150 DEG C, keep the temperature 3.5~6.5h；Temperature-fall period, under 1~3% partial pressure of oxygen, with 2~ The rate of temperature fall of 2.5 DEG C/min is cooled to 1100 DEG C from 1380 DEG C, then in partial pressure of oxygen is 0.5~1.5%, with 5~8 DEG C/min's Rate of temperature fall is down to 500 DEG C from 1100 DEG C, finally with 0.01~0.05% partial pressure of oxygen, the near room of rate of 2.5~3 DEG C/min Temperature.
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