CN109678486A - A kind of wide warm low-temperature coefficient low-consumption Mn-Zn ferrite material - Google Patents
A kind of wide warm low-temperature coefficient low-consumption Mn-Zn ferrite material Download PDFInfo
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- CN109678486A CN109678486A CN201910141689.2A CN201910141689A CN109678486A CN 109678486 A CN109678486 A CN 109678486A CN 201910141689 A CN201910141689 A CN 201910141689A CN 109678486 A CN109678486 A CN 109678486A
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Abstract
The present invention provides a kind of wide warm low-temperature coefficient low-consumption Mn-Zn ferrite material, and the MnZn ferrite material is within the temperature range of -40 DEG C to 140 DEG C than temperature coefficient≤1.5 × 10‑6/ DEG C, which is made of principal component and auxiliary element, wherein the principal component: Fe2O3It is 8.6~9.6mol%, GeO for 52.7~53.5mol%, ZnO2It is surplus for 0.007~0.022mol%, MnO;The auxiliary element: CaCO3For 0.03~0.04wt%, K2O is 0.02~0.03wt%, Cu2O3For 0.4~0.5wt%.The present invention by adjusting main formula composition and impurity addition manner, prepared saturation flux density greater than 440mT, at 100kHz power consumption Pcv coefficient in 340kW/m3MnZn Ferrite Material below.
Description
Technical field
The invention belongs to the advanced preparation and application fields of high performance soft magnetic ferrite material, are related to a kind of wide warm low temperature system
Number low-consumption Mn-Zn ferrite material.
Background technique
With the continuous rise of the industries such as photovoltaic industry, electronic information technology, electric car and hybrid-electric car, answer
Electronic equipment for these new industries will obtain unprecedented development, this will be to the Ferrite Material for being applied to these fields
Play sizable impetus.MnZn Ferrite Material has the characteristics such as low-loss, high Bs, high magnetic permeability, high resistivity, extensively
It is general to be applied in various electronic components, such as power transformer, choking-winding, pulse broadband transformer, present MnZn iron
Ferrite has become computer, communication, TV, video recorder, office automation and the indispensable base of other electronic equipments
Plinth element.As technology continues to develop, MnZn Ferrite Material is also evolving.To adapt to different field to MnZn ferrite
The requirement of material, magnetic core production firm have to constantly develop the high-performance MnZn ferrite material with various new functions
Material.The development in each field is made a general survey of, the characteristics such as ultra-low loss, high-temperature stability, superelevation Bs and high frequency are China MnZn power iron
The inexorable trend of ferrite development.
Since the electronic product in these above-mentioned fields is substantially all work under relatively high environment temperature, and temperature range
Width, so more stringent requirements are proposed to our low-power Ferrite Material, manganese zinc ferrites for power supplies be information technology,
The widely applied material in the fields such as electron electric power needs strict control of material to guarantee device systems stabilization, reliable, efficient operation
Power consumption this important indicator.The power consumption index of power ferrite is not only to be determined by its chemical component and crystal structure
, internal stress, pore volume, impurity and the dislocation of material are reduced, magnetic hysteresis damage can be reduced by improving the measures such as saturation magnetization Ms
Consumption;The resistivity and grain boundary resistivity, reduction crystallite dimension for improving intra-die can reduce eddy-current loss;Control the content of Fe2+
Residual loss can be reduced.This requires strict control technical process, keep the ferrite polycrystalline structure of production fine, uniform, gas
Hole, impurity, the percent by volume of defect are as small as possible, reduce the internal stress of material, it is also necessary to study and control they density,
Crystallite dimension, the porosity and their distributions between intra-die and crystal grain etc..Therefore, high performance power ferrite is prepared
Material, formula be basis, sintering be it is crucial, mix effective additive and match with sintering process appropriate, then to iron oxygen
The performance tool of body is marginal.
A kind of wide warm MnZn power ferrite material of CN102693802A disclosure of the invention and preparation method thereof, by principal component
It is formed with auxiliary element, wherein principal component and content are calculated with oxide are as follows: Fe2O3 is 52.1~52.6mol%, ZnO 9
~11.5mol%, MnO surplus;Auxiliary element based on principal component raw material gross weight is calculated with oxide are as follows: CaCO3, ZrO2,
Nb2O5, SiO2 and Co2O3, and Co2O3 raw material has to be larger than 0.35wt%.The material temperature is in 25~140 DEG C of range loss ratios
It is lower, but saturation flux density is relatively low.
CN201610767923.9 disclosure of the invention wide temperature low-power consumption MnZn ferrite material, by principal component and auxiliary element
Composition, wherein the molar percentage of each component of the principal component are as follows: Fe2O3 be 52.7~53.5mol%, ZnO be 8.6~
9.6mol%, MnO are surplus;By accounting for principal component total weight, auxiliary element each component content are as follows: CaCO3 is 0.03~
It is 0.4~0.5%, SnO2 is 0.05~0.15%, NaO2 0.0074 that 0.04%, Nb2O5, which are 0.02~0.03%, Co2O3,
~0.022% (being added in the form of sodium bicarbonate).In 1200 DEG C of isothermal holdings for carrying out controlling atmosphere of sintering temperature-fall period.
The Ferrite Material is relatively low in 25~140 DEG C of temperature range losses, but temperature coefficient is undesirable.
A kind of high magnetic permeability, high impedance, low-temperature coefficient and the excellent MnZn of frequency characteristic are had both in conclusion researching and developing
Ferrite Material certainly will become the hot spot that the following research and development institution and company competitively chase, with important engineering background and
Market value.
Summary of the invention
Object of the present invention is to propose a kind of wide warm low-temperature coefficient low-consumption Mn-Zn ferrite material.
The technical scheme is that a kind of wide warm low-temperature coefficient low-consumption Mn-Zn ferrite material, the manganese-zinc ferrite
Body material is within the temperature range of -40 DEG C to 140 DEG C than temperature coefficient≤1.5 × 10-6/ DEG C, the MnZn ferrite material is by leading
Ingredient and auxiliary element composition, wherein the principal component: Fe2O3It is 8.6~9.6mol% for 52.7~53.5mol%, ZnO,
GeO2It is surplus for 0.007~0.022mol%, MnO;
The auxiliary element: CaCO3For 0.03~0.04wt%, K2O is 0.02~0.03wt%, Cu2O3For 0.4~
0.5wt%.
Preferably, the principal component: Fe2O3It is 8.6~9.6mol%, GeO for 52.7~53.5mol%, ZnO2For
0.01~0.02mol%, MnO are surplus;
The auxiliary element: CaCO3For 0.03~0.04wt%, K2O is 0.02~0.03wt%, Cu2O3For 0.4~
0.5wt%, SiO2For 0.05~0.15wt%, TiO2For 0.08~0.12wt%, Sm2O3For 0.005~0.04wt%.
Preferably, the principal component: Fe2O3For 52.7mol%, ZnO 8.6mol%, GeO2For 0.007mol%,
MnO is 38.693mol%;
The auxiliary element: CaCO3For 0.03wt%, K2O is 0.02wt%, Cu2O3For 0.4wt%, SiO2For
0.15wt%, TiO2 0.08wt%, Sm2O3For 0.005wt%.
Preferably, the principal component: Fe2O3For 52.7mol%, ZnO 8.7mol%, GeO2For 0.012mol%,
MnO is 38.588mol%;
The auxiliary element: CaCO3For 0.03wt%, K2O is 0.02wt%, Cu2O3For 0.5wt%, SiO2For
0.05wt%, TiO2For 0.08wt%, Sm2O3For 0.04wt%.
Preferably, the principal component: Fe2O3For 53.5mol%, ZnO 9.6mol%, GeO2For 0.022mol%,
MnO is 36.878mol%;
The auxiliary element: CaCO3For 0.04wt%, K2O is 0.03wt%, Cu2O3For 0.5wt%, SiO2For
0.1wt%, TiO2For 0.08wt%, Sm2O3For 0.02wt%.
Preferably, K is with potassium carbonate (K soluble easily in water2CO3) form addition;K2CO3Additive amount is total by principal component is accounted for
Weight is calculated as 0.01~0.03%.
Preferably, the wide temperature low-power consumption MnZn ferrite material is in -40~140 DEG C of wide temperature ranges, 100kHz,
Power consumption Pcv≤340kW/m under the conditions of 200mT3;Saturation flux density Bs >=440mT under the conditions of 1194A/m, 50Hz;
It is 3650 ± 20% that initial permeability under the conditions of -40 DEG C -150 DEG C, which is μ i,.
Due to being influenced by crystal anisotropy constant K the last 1 temperature dependent properties, MnZn ferrite material is only capable of in K1
The temperature spot that compensation is zero is implemented around low magnetic hystersis loss and high magnetic permeability.Using the low zinc formula of more iron, it is greatly improved saturation
Magnetic flux density Bs, but PCV-T curve tail upwarps, and high temperature power consumption is odd big, and inventor, which is based on further investigation, influences magnetocrystalline
The mechanism and various other influence factors of each opposite sex constant K1 temperature dependent properties, by being formed to materials chemistry, micro addition
The further investigation of agent doping, sintering process and microstructure, the preferably various micro constitutents of the present invention, using mutual between additive
It restrains and balances.The temperature that the compensation of crystal anisotropy constant K 1 is zero is divided by innovative ground by usual single temperature spot
High and low two temperature spots, thus greatly reduce material magnetocrystalline anisotropy to the dependence of temperature, make MnZn ferrite material
There is flat power consumption~temperature characterisitic in wider temperature range.
Beneficial effects of the present invention:
1. the warm low-temperature coefficient low-consumption Mn-Zn ferrite material of width of the invention used the low zinc formula of iron, keep magnetocrystalline each
Anisotropy constant and saturation magnetostriction constant As go to zero, and saturation magnetization is big, while reducing the internal stress of material, obtain
The grain structure of dense uniform.
2. inventor is analyzed by the temperature characterisitic (PL~T characteristic) to loss, meeting Curie temperature requirement
In the case where, it reduces ZnO content x (ZnO)=8.6~9.6%, increases GeO in principal component2Content, with Fe2O3/GeO2Ratio
Increase, domain wall resonance frequency is shifted to high-end, and residual loss is caused to reduce;The present invention adds by adjusting the composition and impurity of main formula
Add mode has prepared saturation flux density and has been greater than 440mT, -40 DEG C of -140 DEG C of range internal ratio temperature coefficient≤1.5 × 10-6/
DEG C and at 100kHz power consumption Pcv coefficient in 340kW/m3MnZn Ferrite Material below.
3. the present invention obtains crystal using the regulating and controlling effect of micro additive K, Cu material microstructure formed to sintering
The sintered body of fine structure, crystallite dimension more evenly reduces the magnetic hystersis loss and eddy-current loss of material, so that material is total
Loss reduces, while improving saturation flux density.The part that the present invention is able to solve MnZn ferrite material application aspect is existing
There is technical problem, the addition of certain auxiliary element also has meaning to final products performance.
4. the warm low-temperature coefficient low-consumption Mn-Zn ferrite material of width of the invention, by germanium, samarium, potassium, copper admixture, and
The control of additive amount, to substantially increase Bs under conditions of realizing low temperature high temperature, and high and low frequency loss all obtains
Very big improvement has preferable frequency characteristic.Ge of the present invention4+、Cu3+、Ti4+、K1+Synergy, make complex ferrite
K1-T obtain compensation adjustment, to reach wide warm high saturation magnetic flux density Bs, DC superposition characteristic is good, and high temperature is low in energy consumption.
Present invention reduces power consumption of manganese-zinc ferrite under the conditions of 50Hz, and initial permeability with higher.
Specific embodiment
The present invention is further explained in the light of specific embodiments:
Embodiment 1:
First, in accordance with prescribed formula ingredient: Fe2O3For 53.5mol%, ZnO 9.6mol%, GeO2For 0.022mol%,
MnO is 36.878mol%, mixing, and in sand mill, the deionized water of the weight such as addition, it is 90 minutes that the time, which is sanded, a sand
Cu is mixed when mill2O3For 0.5wt%;
Above-mentioned sand milling material is dried, 950 DEG C pre-burning 120 minutes, it is cooling, carry out secondary sand milling, when secondary sand milling mixes
CaCO3For 0.03wt%, K2O is 0.02wt%, and the deionized water for expecting weight equivalent is added, and is sanded 4 hours, makes being averaged for Preburning material
Granularity is less than 0.8 μm;
Gained feed powder is mixed by weight 12wt% polyvinyl alcohol (PVA) and zinc stearate 1.0wt% is added, and is used
45 mesh sub-sieves are granulated, and are pressed into 25 sample ring of φ, are subsequently placed in atmosphere sintering furnace, are sintered under nitrogen protection, 600~
800 DEG C of temperature sections, partial pressure of oxygen 0.005% heat up 45 minutes;In 800~1000 DEG C of temperature sections, partial pressure of oxygen 0.5%, heating
1 hour;It is balanced atmosphere sintering in temperature descending section, whole process maintains equilibrium oxygen partial pres-sure 0.2%, furnace cooling to room temperature.
Embodiment 2
First, in accordance with prescribed formula ingredient: Fe2O3For 53.5mol%, ZnO 9.6mol%, GeO2For 0.022mol%,
MnO is 36.878mol%, mixing, and in sand mill, the deionized water of the weight such as addition, it is 90 minutes that the time, which is sanded, a sand
Cu is mixed when mill2O3For 0.5wt%, Sm2O3For 0.02mol%;
Above-mentioned sand milling material is dried, 950 DEG C pre-burning 120 minutes, it is cooling, carry out secondary sand milling, when secondary sand milling mixes
CaCO3For 0.04wt%, K2O is 0.03wt%, SiO2For 0.1wt%, TiO2For 0.08wt%, be added expect weight equivalent go from
Sub- water is sanded 4 hours, makes the average particle size of Preburning material less than 0.8 μm;
Gained feed powder is mixed by weight 12wt% polyvinyl alcohol (PVA) and zinc stearate 1.0wt% is added, and is used
45 mesh sub-sieves are granulated, and are pressed into 25 sample ring of φ, are subsequently placed in atmosphere sintering furnace, are sintered under nitrogen protection, 600~
800 DEG C of temperature sections, partial pressure of oxygen 0.005% heat up 45 minutes;In 800~1000 DEG C of temperature sections, partial pressure of oxygen 0.5%, heating
1 hour;It is balanced atmosphere sintering in temperature descending section, whole process maintains equilibrium oxygen partial pres-sure 0.2%, furnace cooling to room temperature.
Embodiment 3
First, in accordance with prescribed formula ingredient: Fe2O3For 52.7mol%, ZnO 8.6mol%, GeO2For 0.007mol%,
MnO is 38.693mol%, mixing, and in sand mill, the deionized water of the weight such as addition, it is 90 minutes that the time, which is sanded, a sand
Cu is mixed when mill2O3For 0.4wt%, Sm2O3For 0.005wt%;
Above-mentioned sand milling material is dried, 950 DEG C pre-burning 120 minutes, it is cooling, carry out secondary sand milling, when secondary sand milling mixes
CaCO3For 0.03wt%, K2O is 0.02wt%, TiO2For 0.08wt%, the deionized water for expecting weight equivalent is added, is sanded 4 hours,
Make the average particle size of Preburning material less than 0.8 μm;
Gained feed powder mixes by weight 8wt% polyvinyl alcohol (PVA) and zinc stearate 1.0wt% is added, uses 45
Mesh sub-sieve is granulated, and is pressed into 25 sample ring of φ, is subsequently placed in atmosphere sintering furnace, is sintered under nitrogen protection, 600~
800 DEG C of temperature sections, partial pressure of oxygen 0.005% heat up 45 minutes;In 800~1000 DEG C of temperature sections, partial pressure of oxygen 0.5%, heating
1 hour;It is balanced atmosphere sintering in temperature descending section, whole process maintains equilibrium oxygen partial pres-sure 0.2%, furnace cooling to room temperature.
Comparative example 1: weigh principal component raw material by following principal component contents: Fe2O3 content is 53.1mol%, ZnO content is
9.2mol%, MnO content are 37.7mol%, be sanded mixing and spraying it is dry after pre-burning, calcined temperature is 900 DEG C, and the time is
120 minutes.Weighed auxiliary element raw material in proportion is added in Preburning material.By the auxiliary element content of principal component total weight
For CaCO3: 0.04%, Nb2O5:0.03%, Co2O3: 0.4%, SiO2: 0.1%, sand milling crushing is carried out, the time is 120 minutes,
Sand average grit diameter is 0.9 μm.Then material is sanded to this and carries out mist projection granulating, with molding machine compacting H25/15/10 annular examination
Sample.
The magnetism testing of the sample ring prepared in embodiment 1-3 and comparative example 1 is enterprising in Hp4284A impedance analyzer
The density of row, sample uses Measure by buoyancy method.Survey sample ring performance, obtained ferrite torroidal core sample characteristics of for example comparison result
It is shown in Table 1.
Table 1
As it can be seen from table 1 the present invention has prepared saturation magnetic by adjusting the composition and impurity addition manner of main formula
Flux density is greater than 440mT, -40 DEG C of -140 DEG C of range internal ratio temperature coefficient≤1.5 × 10-6/℃.The present invention by germanium, samarium,
The control of potassium, the admixture of copper and additive amount, to substantially increase Bs under conditions of realizing low temperature high temperature, and high frequency and
Frequency Power Loss is all greatly improved, and has preferable frequency characteristic.
See Table 2 for details for the relationship of actual measurement sample ring power consumption, embodiment 1-3 and comparative sample power consumption Pcv and temperature.
Table 2
From table 2 it can be seen that crystal anisotropy constant K 1 is compensated the temperature for being zero by usual single temperature by the present invention
Point is divided into high and low two temperature spots, thus greatly reduces material magnetocrystalline anisotropy to the dependence of temperature, makes manganese-zinc ferrite
Body material has flat power consumption~temperature characterisitic in wider temperature range.
The present invention is by adjusting the composition and impurity addition manner of main formula, and the material developed is (- 40 in wide temperature range
~140 DEG C) with the temperature coefficient of very little, extremely low loss.MnZn Ferrite Material saturation flux density of the invention is greater than
440mT, -40 DEG C of -140 DEG C of range internal ratio temperature coefficient≤1.5 × 10-6/ DEG C and power consumption Pcv coefficient exists at 100kHz
340kW/m3Below.
Specific embodiment described herein is only an example for the spirit of the invention.The neck of technology belonging to the present invention
The technical staff in domain can make various modifications or additions to the described embodiments or replace by a similar method
In generation, however, it does not deviate from the spirit of the invention or beyond the scope of the appended claims.
Claims (7)
1. a kind of wide warm low-temperature coefficient low-consumption Mn-Zn ferrite material, it is characterized in that the MnZn ferrite material is at -40 DEG C
Than temperature coefficient≤1.5 × 10 within the temperature range of to 140 DEG C-6/ DEG C, the MnZn ferrite material is by principal component and auxiliary element
Composition, wherein the principal component: Fe2O3It is 8.6~9.6mol%, GeO for 52.7~53.5mol%, ZnO2For 0.007~
0.022mol%, MnO are surplus;
The auxiliary element: CaCO3For 0.03~0.04wt%, K2O is 0.02~0.03wt%, Cu2O3For 0.4~0.5wt%.
2. a kind of wide warm low-temperature coefficient low-consumption Mn-Zn ferrite material according to claim 1, characterized in that described
Principal component: Fe2O3It is 8.6~9.6mol%, GeO for 52.7~53.5mol%, ZnO2It is remaining for 0.01~0.02mol%, MnO
Amount;
The auxiliary element: CaCO3For 0.03~0.04wt%, K2O is 0.02~0.03wt%, Cu2O3For 0.4~0.5wt%,
SiO2For 0.05~0.15wt%, TiO2For 0.08~0.12wt%, Sm2O3For 0.005~0.04wt%.
3. a kind of wide warm low-temperature coefficient low-consumption Mn-Zn ferrite material according to claim 2, characterized in that described
Principal component: Fe2O3For 52.7mol%, ZnO 8.6mol%, GeO2For 0.007mol%, MnO 38.693mol%;
The auxiliary element: CaCO3For 0.03wt%, K2O is 0.02wt%, Cu2O3For 0.4wt%, SiO2For 0.15wt%,
TiO2 is 0.08wt%, Sm2O3For 0.005wt%.
4. a kind of wide warm low-temperature coefficient low-consumption Mn-Zn ferrite material according to claim 2, characterized in that described
Principal component: Fe2O3For 52.7mol%, ZnO 8.7mol%, GeO2For 0.012mol%, MnO 38.588mol%;
The auxiliary element: CaCO3For 0.03wt%, K2O is 0.02wt%, Cu2O3For 0.5wt%, SiO2For 0.05wt%,
TiO2For 0.08wt%, Sm2O3For 0.04wt%.
5. a kind of wide warm low-temperature coefficient low-consumption Mn-Zn ferrite material according to claim 2, characterized in that described
Principal component: Fe2O3For 53.5mol%, ZnO 9.6mol%, GeO2For 0.022mol%, MnO 36.878mol%;
The auxiliary element: CaCO3For 0.04wt%, K2O is 0.03wt%, Cu2O3For 0.5wt%, SiO2For 0.1wt%,
TiO2For 0.08wt%, Sm2O3For 0.02wt%.
6. a kind of wide warm low-temperature coefficient low-consumption Mn-Zn ferrite material according to claim 1 or 2, it is characterized in that K
With potassium carbonate (K soluble easily in water2CO3) form addition;K2CO3Additive amount by account for principal component total weight be 0.01~
0.03%.
7. a kind of wide warm low-temperature coefficient low-consumption Mn-Zn ferrite material according to claim 2, it is characterized in that described
Power consumption Pcv under the conditions of wide temperature low-power consumption MnZn ferrite material is in -40~140 DEG C of wide temperature ranges, 100kHz, 200mT≤
340kW/m3;Saturation flux density Bs >=440mT under the conditions of 1194A/m, 50Hz;Rising under the conditions of -40 DEG C -150 DEG C
Beginning magnetic conductivity is that μ i is 3650 ± 20%.
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