CN103214233B - High TcWide temperature range and super high BsMnZn ferrite material and preparation method thereof - Google Patents
High TcWide temperature range and super high BsMnZn ferrite material and preparation method thereof Download PDFInfo
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- CN103214233B CN103214233B CN201310092273.9A CN201310092273A CN103214233B CN 103214233 B CN103214233 B CN 103214233B CN 201310092273 A CN201310092273 A CN 201310092273A CN 103214233 B CN103214233 B CN 103214233B
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- 239000000463 material Substances 0.000 title claims abstract description 85
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002019 doping agent Substances 0.000 claims abstract description 21
- 238000005245 sintering Methods 0.000 claims description 27
- 239000000843 powder Substances 0.000 claims description 26
- 238000000498 ball milling Methods 0.000 claims description 22
- 239000004615 ingredient Substances 0.000 claims description 11
- 229910052742 iron Inorganic materials 0.000 claims description 10
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 8
- 229910052797 bismuth Inorganic materials 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 229910052758 niobium Inorganic materials 0.000 claims description 7
- 229910052715 tantalum Inorganic materials 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 5
- 239000011230 binding agent Substances 0.000 claims description 4
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 1
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 abstract 1
- 230000006698 induction Effects 0.000 description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 13
- 238000000034 method Methods 0.000 description 9
- 229920006395 saturated elastomer Polymers 0.000 description 9
- 239000013078 crystal Substances 0.000 description 8
- 230000005415 magnetization Effects 0.000 description 8
- 230000035699 permeability Effects 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 239000004576 sand Substances 0.000 description 6
- 230000003993 interaction Effects 0.000 description 5
- 239000002131 composite material Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000696 magnetic material Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000009257 reactivity Effects 0.000 description 3
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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Abstract
High TcWide temperature range and super high BsMnZn ferrite material and a preparation method thereof, belonging to the technical field of ferrite material preparation. The ferrite material of the invention consists of main materials and dopants, and is characterized in that the main materials comprise: 58.0-62.0mol% Fe2O310.0-15.0mol% of ZnO, 4.0-6.0mol% of NiO and the balance of MnO; according to the weight percentage, the pre-sintered main material is taken as a reference standard, and the doping agent comprises the following components in percentage by weight calculated by oxides: 0.001-0.30wt% MoO3、0.01-0.40wt%Bi2O3、0.001-0.05wt%SnO2、0.001-0.05wt%Nb2O5、0.001-0.20wt%Ta2O5. The invention has high Curie temperature cNot less than 320 ℃), wide temperature range and high Bs（25℃，Bs≥600mT；100℃，BsNot less than 490 mT) and low loss (100 deg.C, 100kHz, 200mT, P)L≤800kW/m3) And the like.
Description
Technical field
This technology belongs to Ferrite Material preparing technical field, particularly high-curie temperature (T
c), wide temperature super-high saturated magnetic flux density (B
s) MnZn Ferrite Material and preparation method thereof.
Background technology
The stable working temperature of switching mode power supply transformer magnetic core is under the high temperature of 80 ℃-120 ℃.Under hot conditions, the B of Ferrite Material
scompared with there being one significantly to decline under normal temperature.Meanwhile, be manyly applied to electronic devices and components under the large current condition of high temperature and at least need to meet as HID lamp ballast, power supply on vehicle magnetic core etc.: (1) can export enough large power, and (2) can bear the large electric current of temporary impact while starting.Reach the performance that this requires to depend on to a great extent ferrite magnetic material.Because high output rating means large electric current output, if the electric current of coil is excessive, may cause magnetic core magnetization to saturated, thereby its magnetic conduction ability (inductance value) is declined, the inductance value of magnetic core can first be increased to a maximum value along with the increase of magnetizing current in coil, then declines, and now magnetic core just " saturated ", and to make electron device normally work, the disaccommodation of magnetic core inductance value must be less than a definite value.Under large electric current, if the B of magnetic core
sbe worth highlyer, its antisaturation ability is just stronger, and inductance disaccommodation is just less.Simultaneously, the power consumption of material is unsuitable too high, if the power consumption of magnetic core self is high, can make magnetic part heating itself increase, energy transmission efficiency reduces, once working temperature is higher than power consumption valley point, can cause temperature to raise, the loss of magnetic core is larger, forms the higher vicious cycle of magnetic part temperature, and then affects the normal work of device.In addition, although metal soft magnetic material has higher saturation induction density, its cost is higher, resistivity is lower, and its erosion resistance is poor, does not meet the original intention of design high-performance and low-cost, low-loss material.It should be noted that, high Curie temperature is the essential condition that magnetic device is worked in wide temperature range, especially the limited occasion of heat-dissipating space, the reliability what is more important that improves magnetic device and electronic system can guarantee that material has high B in wide temperature range
s; And high B
scan improve the current load amount of electronic system, improve power density, realize miniaturization, therefore, develop a kind of high-curie temperature, wide temperature superelevation B of having concurrently
sthe MnZn Ferrite Material of characteristic has boundless market application foreground.
In recent years, high-curie temperature (T
c), wide temperature high saturated magnetic induction (B
s) power ferrite material become the focus that magnetic material industry is paid close attention to.In the disclosed patent CN1294099A of China, the high B of a kind of high temperature is disclosed
spower ferrite material, it replaces by NiO the B that MnO improves material
sbut, the B under its 100 ℃, 1194A/m
sbe only 440mT.Patent CN101090016A has announced a kind of by regulating the mode of temperature rate, soaking time and oxygen partial pressure size in sintering process to reach raising material B
sobject, the B under its 100 ℃, 1194A/m
sreach 450mT, still less.Patent CN101429016A discloses a kind of MnZn power ferrite material, and its Curie temperature is 280 ℃, the B under 100 ℃, 1194A/m
sfor 460mT, be T in current material
cand B
sall higher material, has the stronger market competitiveness.A kind of high temperature superelevation B is disclosed in patent CN1890197A
smnZn power ferrite material, its main formula is: Fe
2o
3: 63-80mol%, ZnO:3-15mol%, remaining is MnO, ancillary component comprises CaO, SiO
2, at 1175 ℃, be incubated 8 hours.The Ferrite Material performance obtaining is: at 100 ℃, and B
sfor 520mT, but its loss is too high, and at 50kHz, the loss under 150mT is up to 1100kW/m
3.In addition, the MB1H magneticsubstance that JFE company releases, the B at its 25 ℃ and 100 ℃
sbe respectively 540mT and 460mT, Curie temperature is 300 ℃.The 4H47 material of FDK company, the B at its 25 ℃ and 100 ℃
sbe respectively 530mT and 470mT, Curie temperature is about 200 ℃.The BH7 material that NEC/TOKIN company releases, the B at its 25 ℃ and 100 ℃
sbe respectively 600mT and 490mT, 100 ℃, the loss of 100kHz200mT are up to 1350kW/m
3.The BM40 material of NICERA company, the B at its 25 ℃ and 100 ℃
sbe respectively 530mT and 470mT, Curie temperature is up to 300 ℃.
Summary of the invention
Technical problem to be solved by this invention is that a kind of high T is provided
c, wide temperature superelevation B
smnZn Ferrite Material and preparation method, its material has high-curie temperature (T
c>=320 ℃), the high B of wide temperature
s(25 ℃, B
s>=600mT; 100 ℃, B
s>=490mT) and compared with low-loss (100 ℃, 100kHz200mT, P
l≤ 800kW/m
3) etc. characteristic.
The technical scheme that the present invention solve the technical problem employing is, high T
c, wide temperature superelevation B
smnZn Ferrite Material, is comprised of major ingredient and doping agent, it is characterized in that, major ingredient comprises:
58.0-62.0mol%Fe
2o
3, 10.0-15.0mol%ZnO, 4.0-6.0mol%NiO, surplus is MnO;
By weight percentage, and the major ingredient of take after pre-burning is reference data, with oxide compound, calculates, and doping agent comprises: 0.001-0.30wt%MoO
3, 0.01-0.40wt%Bi
2o
3, 0.001-0.05wt%SnO
2, 0.001-0.05wt%Nb
2o
5, 0.001-0.20wt%Ta
2o
5.
High T of the present invention
c, wide temperature superelevation B
sthe preparation method of MnZn Ferrite Material comprises the following steps:
1) formula
Adopt 58.0-62.0mol%Fe
2o
3, 10.0-15.0mol%ZnO, 4.0-6.0mol%NiO, surplus is MnO;
2) ball milling
The material powder of filling a prescription is above mixed to ball milling;
3) pre-burning
By step 2) oven dry of gained ball milling material, under 60-100MPa, suppress, and at 800-1000 ℃ of pre-burning 1-3 hour;
4) doping
Step 3) gained material powder is added to following doping agent: 0.001-0.30wt%MoO by weight
3, 0.01-0.40wt%Bi
2o
3, 0.001-0.05wt%SnO
2, 0.001-0.05wt%Nb
2o
5, 0.001-0.20wt%Ta
2o
5; Described weight ratio is doping agent: material powder.
5) secondary ball milling
By the material powder obtaining in step 4) ball milling 4-8 hour in ball mill;
6) moulding
Step 5) gained material powder is added to 8-12wt% organic binder bond by weight, mix, after granulation, on press, granular powder is pressed into blank;
7) sintering
Step 6) gained blank is placed in to sintering in atmosphere sintering furnace.
Described step 7) is: step 6) gained blank is placed in to sintering in atmosphere sintering furnace, at 1000 ℃ of-1300 ℃ of temperature sections, volume ratio O
2/ N
2=1/999; At 1300 ℃ of-1400 ℃ of temperature sections, O
2/ N
2=4/96, insulation 4-6 hour; At temperature descending section, carry out balanced atmosphere sintering.
8) test
Step 7) gained sample is carried out to electromagnetic performance test.
By the inductance L of same favour TH2828 LCR test set test sample, suitably adjust coiling both end voltage value U
sit is met: U
s=4.44NfA
eb, the initial permeability of sample is calculated according to following formula:
The inductance that wherein L is sample, N is number of turns, and h is thickness of sample, and D is sample external diameter, and d is sample internal diameter, A
enet sectional area for sample.Test condition is: frequency f=10kHz, magnetic induction density B≤0.25mT.In conjunction with temperature control box, draw μ
i-T graphic representation, is used epitaxial method to determine Curie temperature T
c.
With the magnetic hysteresis loop of IWATSU SY-8232B-H analyser test sample, test condition is: f=0.1kHz, H=1200A/m.
With the loss of IWATSU SY-8232B-H analyser test sample, test condition is: f=100kHz, B
m=200mT, T=25 ℃-120 ℃.
The technology of preparing of MnZn Ferrite Material of the present invention, its technical indicator is as follows:
Initial permeability μ
i: 1500 ± 20%
Saturation induction density B
s:>=600mT(25 ℃);>=490mT(100 ℃);>=460mT(120 ℃)
Curie temperature T
c:>=320 ℃
Loss P
l(100kHz200mT) :≤1100kW/m
3(25 ℃); ≤ 800kW/m
3(100 ℃); ≤ 1000kW/m
3(120 ℃);
Density d
m:>=5.0g/cm
3;
High-curie temperature (T
c>=320 ℃), the high B of wide temperature
s(25 ℃, B
s>=600mT; 100 ℃, B
s>=490mT) and compared with low-loss (100 ℃, 100kHz200mT, P
l≤ 800kW/m
3) etc. characteristic.
Embodiment
The present invention is mainly for the existing high-curie temperature of MnZn ferrite and the high B of wide temperature of prior art design
stwo technical barriers that key parameter is difficult to meet simultaneously, provide a kind of high-curie temperature and high B of wide temperature of having concurrently
smnZn Ferrite Material of characteristic and preparation method thereof.
Core concept of the present invention is: adopt the rich iron formula of MnZn ferrite, strengthen magnetic ion quantity in A, B lattice, the superexchange interaction of strongthener, though can improve the Curie temperature of material, but inevitably increased the magnetocrystalline anisotropy constant of material and magnetostriction coefficient (on the occasion of), increased magnetization resistance, be unfavorable for improving magnetic permeability and reduce the wastage; Therefore, the present invention adopts appropriate NiO to substitute MnO, the NiFe being formed by NiO on the one hand
2o
4ferritic Curie temperature is significantly higher than the MnFe being formed by MnO
2o
4ferritic Curie temperature, can improve the Curie temperature of material after replacement, improve the reliability of magnetic device, the NiFe that NiO forms on the other hand
2o
4the MnFe that ferritic magnetocrystalline anisotropy constant and magnetostriction coefficient (negative value) form lower than MnO
2o
4ferritic anisotropic crystalline constant and magnetostriction coefficient (negative value), NiO partly replaces after MnO, and the just magnetization resistance that can partly form with rich iron forms positive and negative compensation, and then makes to magnetize resistance and have lower value, can improve magnetic permeability, reduces the wastage.Meanwhile, in formula, reduce as far as possible ZnO content, and then guarantee that material has high Curie temperature.
On doping agent, adopt MoO
3, Bi
2o
3, SnO
2, Nb
2o
5, Ta
2o
5fluxing and hindering brilliant two property effect Deng doping agent, realize composite mixed dose of interactive control, improve on the one hand sintered density, improve saturation induction density, reduce magnetization resistance, improve magnetic permeability, on the other hand, control grain-size unsuitable excessive, control crystal grain/crystal boundary characteristic of material, reduce spillage of material.Aspect sintering process, in conjunction with extraordinary high reactivity submicron powder preparation technology, prepare high reactivity submicron powder, by the two property effects of composite additive, in sintering process, apply secondary reduction technique, realize the high-density even grained sintering of material.That is: by rich iron formula and Ni replacement technique, strengthen the superexchange interaction of A, B para-crystal compartment, realize the Curie temperature that MnZn Ferrite Material is high; The occupy-place of regulation and control magnetic/non magnetic ion in inferior lattice distributes, increase the Net magnetic moment of material, realize the saturation induction density that material is high, rely on high-curie temperature, can the temperature variant Brillouin's attenuation characteristic of passivating material saturation induction density so that material still has high B when high temperature
s; In conjunction with the effect of two property and the secondary reduction sintering technology of composite additive, control crystal grain/crystal boundary characteristic of material, obtain uniform microstructure, and then improve the magnetic permeability of material, reduce the wastage.
For having at present high-curie temperature T both at home and abroad concurrently
c, wide temperature high saturated magnetic induction B
sand compared with low-loss P
ltechnological gap and the market requirement of the MnZn Ferrite Material of characteristic, the invention provides high T
c, the high B of wide temperature
sand lower P
lmnZn Ferrite Material of characteristic and preparation method thereof.Its guiding theory is: strong superexchange interaction, high magnetization power and lower magnetization resistance, even leading crystal grain/crystal boundary characteristic and the densification sintering technology of microstructure.First, by preferred highly purified Fe
2o
3, Mn
3o
4, ZnO and NiO be starting material, in depth analyzed the superexchange interaction, magnetization power and the magnetization resistance that in MnZn Ferrite Material, exist, adopts rich iron, lower ZnO, appropriate NiO to replace Mn
3o
4take thought as the leading factor, formulate optimum formula range; Secondly, analyse in depth different sorts doping agent to the microstructural interaction mechanism of MnZn Ferrite Material, studied doping agent MoO
3, Bi
2o
3, SnO
2, Nb
2o
5, Ta
2o
5deng the impact on MnZn Ferrite Material crystal boundary, grain properties, formulate optimum doping agent formula; Then, select and prepare by a certain percentage the superhard ball-milling medium of different diameter size, dispersion agent ball milling powder to the 0.5 μ m-0.9 μ m in conjunction with suitable, has prepared high reactivity powder; Finally, under the prerequisite of above-mentioned formula, doping agent and powder optimum preparation condition, in conjunction with densification sintering technique, prepared and there is high-curie temperature T
c, wide temperature high saturated magnetic induction B
sand compared with low-loss P
lthe MnZn Ferrite Material of characteristic.
MnZn Ferrite Material principal constituent of the present invention by mole%, with oxide compound, calculate; Doping agent composition by weight percentage, calculates with oxide compound.High-curie temperature T of the present invention
c, wide temperature high saturated magnetic induction B
sand compared with low-loss P
lthe MnZn Ferrite Material of characteristic is comprised of major ingredient and doping agent, and major ingredient comprises: 58.0-62.0mol%Fe
2o
3, 10.0-15.0mol%ZnO, 4.0-6.0mol%NiO, surplus is MnO;
The major ingredient of take after pre-burning is reference data, by weight percentage, with oxide compound, calculates, and doping agent comprises: 0.001-0.30wt%MoO
3, 0.01-0.40wt%Bi
2o
3, 0.001-0.05wt%SnO
2, 0.001-0.05wt%Nb
2o
5, 0.001-0.20wt%Ta
2o
5.For example,, if the major ingredient quality after pre-burning is a gram, MoO
3quality be the wt% gram of a * (0.001-0.30).
Preparation method of the present invention comprises the following steps:
1, formula
Adopt 58.0-62.0mol%Fe
2o
3, 10.0-15.0mol%ZnO, 4.0-6.0mol%NiO, surplus is MnO;
2, a ball milling
To in ball mill, mix with material loading powder time 1-3 hour;
3, pre-burning
Step 2 gained ball milling material is dried, under 60-100MPa, is pressed into cake, and in 800-1000 ℃ of stove pre-burning 1-3 hour;
4, doping
Step 3 gained material powder is added to following doping agent: 0.001-0.30wt%MoO by weight
3, 0.01-0.40wt%Bi
2o
3, 0.001-0.05wt%SnO
2, 0.001-0.05wt%Nb
2o
5, 0.001-0.20wt%Ta
2o
5;
5, secondary ball milling
In ball mill, prepare by a certain percentage the superhard ball-milling medium of different diameter size, the material powder obtaining in step 4 is mixed according to certain pellet ratio, ball milling 4-8 hour in ball mill;
6, moulding
Step 5 gained material powder is added to 8-12wt% organic binder bond by weight, mix, after granulation, on press, granular powder is pressed into blank;
7, sintering
Step 6 gained blank is placed in to sintering in atmosphere sintering furnace, at 1000 ℃ of-1300 ℃ of temperature sections, volume ratio O
2/ N
2=1/999, at 1300 ℃ of-1400 ℃ of temperature sections, O
2/ N
2=4/96, insulation 4-6 hour; At temperature descending section, carry out balanced atmosphere sintering.
8, test
Step 7 gained sample is carried out to electromagnetic performance test.
By the inductance L of same favour TH2828 LCR test set test sample, suitably adjust coiling both end voltage value U
sit is met: U
s=4.44NfA
eb, the initial permeability of sample is calculated according to following formula:
The inductance that wherein L is sample, N is number of turns, and h is thickness of sample, and D is sample external diameter, and d is sample internal diameter, A
enet sectional area for sample.Test condition is: frequency f=10kHz, magnetic induction density B≤0.25mT.In conjunction with temperature control box, draw μ
i-T graphic representation, is used epitaxial method to determine Curie temperature T
c.
With the magnetic hysteresis loop of IWATSU SY-8232B-H analyser test sample, test condition is: f=0.1kHz, H=1200A/m.
With the loss of IWATSU SY-8232B-H analyser test sample, test condition is: f=100kHz, B
m=200mT, T=25 ℃-120 ℃.
Specific embodiment:
Embodiment 1-4: a kind of high-curie temperature T
c, wide temperature high saturated magnetic induction B
sand compared with low-loss P
lmnZn Ferrite Material of characteristic and preparation method thereof, comprises the following steps:
1, formula
Embodiment 1-4 major ingredient formula sees the following form:
2, a ball milling
To in ball mill, mix with material loading powder time 2 h;
3, pre-burning
Step 2 gained ball milling material is dried, under 60MPa, be pressed into cake, and pre-burning 2 hours in 850 ℃ of stoves;
4, doping
Step 3 gained material powder is added to doping agent shown in following table by weight:
5, secondary ball milling
In ball mill, prepare by a certain percentage the superhard ball-milling medium of different diameter size, the material powder obtaining in step 4 is mixed according to certain pellet ratio, in ball mill, ball milling is 6 hours;
6, moulding
Step 5 gained material powder is added to 10wt% organic binder bond by weight, mix, after granulation, on press, granular powder is pressed into blank;
7, sintering
Step 6 gained blank is placed in to sintering in atmosphere sintering furnace, at 1000 ℃ of-1300 ℃ of temperature sections, volume ratio O
2/ N
2=1/999, at 1360 ℃ of insulations 5 hours, O
2/ N
2=4/96; At temperature descending section, carry out balanced atmosphere sintering.
The high-curie temperature T preparing through above technique
c, wide temperature high saturated magnetic induction B
sand compared with low-loss P
lthe MnZn Ferrite Material of characteristic, its performance index are as follows:
Embodiment 1-4 test result is as follows:
Claims (4)
1. high T
c, wide temperature superelevation B
smnZn Ferrite Material, is comprised of major ingredient and doping agent, it is characterized in that, major ingredient comprises: 58.0-62.0mol%Fe
2o
3, 10.0-15.0mol%ZnO, 4.0-6.0mol%NiO, surplus is MnO;
By weight percentage, and the major ingredient of take after pre-burning is reference data, with oxide compound, calculates, and doping agent comprises: 0.001-0.30wt%MoO
3, 0.01-0.40wt%Bi
2o
3, 0.001-0.05wt%SnO
2, 0.001-0.05wt%Nb
2o
5, 0.001-0.20wt%Ta
2o
5.
2. high T
c, wide temperature superelevation B
smnZn ferrite material preparation method for material, is characterized in that, comprises the following steps:
1) formula
Adopt 58.0-62.0mol%Fe
2o
3, 10.0-15.0mol%ZnO, 4.0-6.0mol%NiO, surplus is MnO;
2) ball milling
The material powder of filling a prescription is above mixed to ball milling;
3) pre-burning
By step 2) oven dry of gained ball milling material, under 60-100MPa, suppress, and at 800-1000 ℃ of pre-burning 1-3 hour;
4) doping
Step 3) gained material powder is added to following doping agent: 0.001-0.30wt%MoO by weight
3, 0.01-0.40wt%Bi
2o
3, 0.001-0.05wt%SnO
2, 0.001-0.05wt%Nb
2o
5, 0.001-0.20wt%Ta
2o
5;
5) secondary ball milling
By the material powder obtaining in step 4) ball milling 4-8 hour in ball mill;
6) moulding
Step 5) gained material powder is added to 8～12wt% organic binder bond by weight, mix, after granulation, on press, granular powder is pressed into blank;
7) sintering
Step 6) gained blank is placed in to sintering in atmosphere sintering furnace.
3. high T as claimed in claim 2
c, wide temperature superelevation B
smnZn ferrite material preparation method for material, is characterized in that, described step 7) is: step 6) gained blank is placed in to sintering in atmosphere sintering furnace, at 1000 ℃ of-1300 ℃ of temperature sections, volume ratio O
2/ N
2=1/999; At 1300 ℃ of-1400 ℃ of temperature sections, O
2/ N
2=4/96, insulation 4-6 hour; At temperature descending section, carry out balanced atmosphere sintering.
4. high T as claimed in claim 2
c, wide temperature superelevation B
smnZn ferrite material preparation method for material, is characterized in that, the formula of step 1) is: 59.0mol%Fe
2o
3, 14.0mol%ZnO, 6.0mol%NiO, 21.0mol%MnO;
In step 3), doping agent is: 0.08wt%MoO
3, 0.03wt%Bi
2o
3, 0.03wt%Nb
2o
5, 0.05wt%Ta
2o
5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310092273.9A CN103214233B (en) | 2013-01-31 | 2013-03-21 | High TcWide temperature range and super high BsMnZn ferrite material and preparation method thereof |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310037163.2 | 2013-01-31 | ||
| CN201310037163 | 2013-01-31 | ||
| CN201310092273.9A CN103214233B (en) | 2013-01-31 | 2013-03-21 | High TcWide temperature range and super high BsMnZn ferrite material and preparation method thereof |
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| CN1649039A (en) * | 2004-01-30 | 2005-08-03 | Tdk株式会社 | Method for producing Mn-Zn ferrite |
| CN1662470A (en) * | 2002-09-26 | 2005-08-31 | Tdk株式会社 | Ferrite material |
| CN1692089A (en) * | 2003-01-10 | 2005-11-02 | Tdk株式会社 | Ferrite material and method of manufacturing the same |
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| CN1692089A (en) * | 2003-01-10 | 2005-11-02 | Tdk株式会社 | Ferrite material and method of manufacturing the same |
| CN1649039A (en) * | 2004-01-30 | 2005-08-03 | Tdk株式会社 | Method for producing Mn-Zn ferrite |
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