CN109133903A - A kind of Br has the high-performance permanent-magnet ferrite and preparation method thereof of excessive temperature stability - Google Patents
A kind of Br has the high-performance permanent-magnet ferrite and preparation method thereof of excessive temperature stability Download PDFInfo
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Abstract
The invention discloses the high-performance permanent-magnet ferrites that a kind of Br has excessive temperature stability, are hexagonal crystal M type ferrite main phase, form expression are as follows: (A1O)1‑x(A2O)x•(Fe2O3)k‑y‑z(B1O)y(B2O)zWherein A1For one of elements Sr, Ba, Pb or several, A2For one of Elements C a, La, Bi or several；B1For Co, Zn, one of Cr or several, B2Ionic compartmentation is carried out to Fe for several combination addition of Cu, Ge, Si, V, Nb, Ta；And 0≤x≤0.6,3≤k≤6,0≤y≤0.6,0≤z≤0.4；Preparation method specifically comprises the following steps: the processing of (1) ingredient, (2) mixing, (3) pre-burning, (4) secondary grinding, (5) molding, (6) double sintering.The present invention is directed to the α of existing permanent-magnet ferriteBrIt is worth larger problem, it crosses several combination addition of Cu, Ge, Si, V, Nb, Ta and ionic compartmentation is carried out to Fe ion, granularity processing has been carried out to raw material, keep raw materials granularity close, progress solid phase reaction is more abundant at high temperature, and the permanent-magnet ferrite Br value produced has high temperature stability.
Description
Technical field:
The present invention relates to permanent magnetic ferrite magnet technical fields, relate generally to a kind of high-performance of the Br with excessive temperature stability
Permanent-magnet ferrite and preparation method thereof.
Background technique:
Permanent-magnet ferrite is a kind of hexagonal structure compound with uniaxial anisotropy, mainly three kinds of barium, strontium, lead ferrites
And its compound solid solution.This kind of ferrite after the disappearance of extraneous magnetizing field, remain to it is permanent maintain it is stronger constant surplus
Magnetic property can be used for generating exterior space in permanent steady magnetic field.
For permanent-magnet ferrite because its raw material is cheap, from a wealth of sources, manufacturing process is simple, can largely be produced, and because
It has very high resistivity, can use under high frequency occasion, and chemical stability is good, and problem of oxidation is not present, is answered extensively
For industries such as automobile, household electrical appliance, industrial automations, but in permanent-magnet ferrite, temperature is lower, and temperature stability is poor, tight
It should not be used under the occasion of lattice.Especially the height such as car motor rotor and frequency-changeable compressor performance ferrite is because in enclosed environment
It uses, ferrite work environmental area temperature is caused to increase, and ferritic performance Br value increases with temperature and is declined, from
And cause under high temperature environment ferrite have lost a part of performance, although as environment temperature declines, a part of property of loss
Energy Br value is restored therewith, but makes the severe to improve to ferritic performance requirement of forming environment, considerably increases iron oxygen
The difficulty and production cost of body production.
The temperature stability of permanent-magnet ferrite Br value can use remanent magnetism reversible temperature coefficient αBrIt indicates, is by material itself
Property determine, be defined as αBr=Δ Br/Br Δ T, the α of general permanent-magnet ferriteBrIt is worth between -0.18% ~ -0.2%, due to
This temperature coefficient is larger, greatly limits ferritic use scope.
Summary of the invention:
α of the object of the invention aiming at existing permanent-magnet ferriteBrIt is worth larger problem, it is steady with excessive temperature provides a kind of Br
Qualitative high-performance permanent-magnet ferrite is held essentially constant ferrite Br between room temperature and 50 DEG C, 50 DEG C and 100 DEG C it
Between αBrValue by -0.2%/DEG C be increased to not less than -0.1%/DEG C.
The present invention is achieved by the following technical solutions:
A kind of Br has the high-performance permanent-magnet ferrite of excessive temperature stability, it is characterised in that: it is hexagonal crystal M type ferrite
Main phase forms expression are as follows: (A1O)1-x(A2O)x•(Fe2O3)k-y-z(B1O)y(B2O)z
Wherein A1For one of elements Sr, Ba, Pb or several, A2For one of Elements C a, La, Bi or several；B1For
One of Co, Zn, Cr are several, B2Ionic compartmentation is carried out to Fe for several combination addition of Cu, Ge, Si, V, Nb, Ta；
And 0≤x≤0.6,3≤k≤6,0≤y≤0.6,0≤z≤0.4.
The Br has the preparation method of the high-performance permanent-magnet ferrite of excessive temperature stability, it is characterised in that: tool
Body includes the following steps:
(1) ingredient is handled
According to ingredient formula (A1O)1-x(A2O)x•(Fe2O3)k-y-z(B1O)y(B2O)zMolar ratio, calculate A1、A2、Fe、B1With
B2Quality needed for the oxide or metallic salt ingredient of five elements is simultaneously weighed, and the average particle size of each ingredient is less than
10um, purity are greater than 96.5%；Then in addition to croci starting material with water ball milling or sand mill carry out fine grinding processing,
Wet lapping in 5 ~ 10 hours is carried out, the quality proportioning of steel ball, water and material is (8-20): (1.5-3): 1, make to obtain mixture
Expect that average particle size is not more than 1.5 um；
(2) it mixes
Croci will be added in mixed material that step (1) obtains, and an additive is added, one time additive is
SiO2, H3BO3, NH4HCO3 are one or more of, and adding proportion is SiO2:0%~0.6%, H3BO3:0~0.3%, NH4HCO3:0
~0.3%；It is mixed and is crushed by water for ball milling or sand mill again, carry out wet lapping in 1 ~ 4 hour, steel ball, water and material
Quality proportioning is (8-20): (1.5-3): 1, make to obtain mixed material average particle size no more than 1.5 um；
(3) pre-burning
By mixed material that step (2) obtains in drying at a temperature of 250-300 DEG C in baking oven, keep moisture content after drying small
In 5%；Then pre-burning is carried out, calcined temperature is 1100 ~ 1360 DEG C, and high temperature burn-in time is 50 minutes ~ 150 minutes；Finally carry out
Pulverization process makes 2 ~ 6 μm of smashed average particle size；
(4) secondary grinding
The preburning powdered material that step (3) obtains is weighed, secondary additive is added, secondary additive includes calcium carbonate powder, strontium carbonate
Powder, silicon oxide powder, boric acid powder, the one or more of NH4HCO3 powder, dispersing agent, by resulting mixture water polo
Mill or sand mill carry out fine grinding processing, carry out wet lapping in 6 ~ 12 hours, the quality proportioning of steel ball, water and material is (8-20):
(1.5-3): 1, average particle size is obtained in the slurry of 0.8-1.2um；
(5) it forms
The ground slurry precipitating or Direct Dehydration to pulp density that step (4) is obtained is 55% ~ 70%, then in 500-
Compression forming in the magnetic field 800kA/M, being pressed into density is 3.0 ~ 3.6g/cm3Rule body；
(6) double sintering
Moisture is carried out and organic dispersing agent volatilization is handled in 100-400 °C of the at a temperature of rule body that obtains to step (5), then
It is the high-performance that 4.9 ~ 5.2g/cm3 has excessive temperature stability to get Br that density is fired at a temperature of 1150 ~ 1250 DEG C
Permanent-magnet ferrite.
The secondary additive preferred embodiment being added in the step (4) into preburning powdered material are as follows: be added by weight ratio
Calcium carbonate powder 0.3%~1.2%, strontium carbonate powder 0.2%~1.0%, silicon oxide powder 0.0.05~0.5%, boric acid powder 0.05
~0.2%, dispersing agent total amount 0.1~0.8%.
The dispersing agent is D-sorbite, calcium gluconate or ascorbic acid.
It is 1200 °C~1250 °C that preferred sintering temperature, which is sintering temperature, in the step (6).
The invention has the advantages that
1, granularity processing has been carried out to raw material, has kept raw materials granularity close, it is more abundant to carry out solid phase reaction at high temperature；
An additive is added before pre-burning, H3BO3 plays the role of promoting crystallization in pre-burning, and SiO2 plays inhibition in pre-burning
The effect of crystallization can be improved calcined temperature, increase product density, and then mention performance Br by adding H3BO3 and SiO2
It is high；
2, ionic compartmentation, the permanent magnet oxygen produced are carried out to Fe ion by several combination addition of Cu, Ge, Si, V, Nb, Ta
Body Br value has high temperature stability；
3, as prioritization scheme, secondary additive preferred embodiment from step (4) to preburning powdered material that be added in are as follows: by weight ratio
Calcium carbonate powder 0.3%~1.2%, strontium carbonate powder 0.2%~1.0%, silicon oxide powder 0.0.05~0.5%, boric acid powder is added
0.05~0.2%, dispersing agent total amount 0.1~0.8%.
4, as prioritization scheme, dispersing agent is D-sorbite, calcium gluconate or ascorbic acid.
5, as prioritization scheme, it is 1200 °C~1250 °C that the sintering temperature in step (6), which is sintering temperature,.
Specific embodiment:
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, the present invention is carried out
It is further described.It should be appreciated that the specific embodiments described herein are only used to explain the present invention, it is not used to limit
The fixed present invention.
Embodiment 1:
A kind of Br has the high-performance permanent-magnet ferrite of excessive temperature stability, forms expression:
(SrO)0.5(CaO)0.2(La2O3)0.15•(Fe2O3)5.2(Co2O3)0.1(CuO)0.1(GeO2)0.1
The preparation method of above-mentioned high-performance permanent-magnet ferrite, includes the following steps:
(1) ingredient is handled
According to composition expression: (SrO)0.5(CaO)0.2(La2O3)0.15•(Fe2O3)5.2(Co2O3)0.1(CuO)0.1(GeO2)0.1
Molar ratio, and consider loss ratio, raw material additive amount calculated, by total amount of feeding 2KG, in which:
Fe2O3Powder: 1647.6 grams；SrCO3Powder: 146.4 grams；CaCO3Powder: 39.7 grams；La2O3Powder: 97 grams；Co2O3
Powder: 32.9 grams；CuO powder: 15.8 grams；GeO2Powder: 20.8 grams；
The average particle size of each ingredient is less than 10um, and purity is greater than 96.5%；Then to the starting material with water ball in addition to croci
Mill carries out fine grinding processing, carries out wet lapping in 6 hours, and the quality proportioning of steel ball, water and material is 10:2:1, makes to be mixed
Material average particle size is not more than 1.5 um；
(2) it mixes
Croci will be added in mixed material that step (1) obtains, and an additive is added, one time additive is
SiO2、H3BO3、NH4HCO3, additive amount SiO2: 5 grams, H3BO3: 2 grams, NH4HCO3: 4 grams；Again by water for ball milling carry out mixing and
It crushes, carries out wet lapping in 2 hours, the quality proportioning of steel ball, water and material is 10:2:1, makes to obtain mixed material and is averaged grain
Degree is not more than 1.5 um；
(3) pre-burning
By mixed material that step (2) obtains in drying at a temperature of 260 DEG C in baking oven, it is less than moisture content after drying
5%；Then pre-burning is carried out, calcined temperature is 1280 DEG C, and high temperature burn-in time is 120 minutes；Pulverization process is finally carried out, powder is made
Average particle size after broken is 2 ~ 6 μm;
(4) secondary grinding
Weigh the preburning powdered material 1KG that step (3) obtains, be added secondary additive, secondary additive includes, strontium carbonate powder,
SiO2: 1.5 grams, NH4HCO3: 2 grams, resulting mixture is subjected to fine grinding processing with water for ball milling, the wet type carried out 10 hours is ground
The quality proportioning of mill, steel ball, water and material is 10:2:1, obtains average particle size in the slurry of 0.8-1.2um；
(5) it forms
The ground slurry precipitating or Direct Dehydration to pulp density that step (4) is obtained is 60%, then in 700kA/M
Compression forming in magnetic field, being pressed into density is 3.5g/cm3Rule body.
(6) double sintering
Moisture is carried out and organic dispersing agent volatilization is handled in 300 °C of the at a temperature of rule body that obtains to step (5), is then existed
The high-performance permanent-magnet ferrite that the Br that density is 5.1g/cm3 has excessive temperature stability is fired at a temperature of 1230 DEG C.
Br made from embodiment 1 has the high-performance permanent-magnet ferrite of excessive temperature stability through detecting Br:4421Gs；
Hcb:326kA/m；Hcj:398kA/m；(BH) max:38.1kJ/m3;αBrCoefficient: -0.08%/DEG C.
Embodiment 2:
A kind of Br has the high-performance permanent-magnet ferrite of excessive temperature stability, forms expression: (SrO)0.48(CaO)0.14
(La2O3)0.19•(Fe2O3)5.29(Co2O3)0.09(4CuO)0.04(V2O5)0.04
The preparation method of above-mentioned high-performance permanent-magnet ferrite, includes the following steps:
(1) ingredient is handled
According to composition expression: (SrO)0.48(CaO)0.14(La2O3)0.19•(Fe2O3)5.29(Co2O3)0.09(4CuO)0.04
(V2O5)0.04
Molar ratio, and consider loss ratio, raw material additive amount calculated, by total amount of feeding 2KG, in which:
Fe2O3Powder: 1646 grams；SrCO3Powder: 138.1 grams；CaCO3Powder: 27.3 grams；La2O3Powder: 120.6 grams；Co2O3
Powder: 29.1 grams；CuO powder: 24.8 grams；V2O5Powder: 14.2 grams；
The average particle size of each ingredient is less than 10um, and purity is greater than 96.5%；Then to the starting material with water ball in addition to croci
Mill carries out fine grinding processing, carries out wet lapping in 6 hours, and the quality proportioning of steel ball, water and material is 10:2:1, makes to be mixed
Material average particle size is not more than 1.5 um；
(2) it mixes
Croci will be added in mixed material that step (1) obtains, and an additive is added, one time additive is
SiO2、H3BO3、NH4HCO3, additive amount SiO2: 5 grams, H3BO3: 2 grams, NH4HCO3: 4 grams；Again by water for ball milling carry out mixing and
It crushes, carries out wet lapping in 2 hours, the quality proportioning of steel ball, water and material is 10:2:1, makes to obtain mixed material and is averaged grain
Degree is not more than 1.5 um；
(3) pre-burning
By mixed material that step (2) obtains in drying at a temperature of 260 DEG C in baking oven, it is less than moisture content after drying
5%；Then pre-burning is carried out, calcined temperature is 1280 DEG C, and high temperature burn-in time is 120 minutes；Pulverization process is finally carried out, powder is made
Average particle size after broken is 2 ~ 6 μm;
(4) secondary grinding
Weigh the preburning powdered material 1KG that step (3) obtains, be added secondary additive, secondary additive include strontium carbonate powder,
SiO2: 1.5 grams, NH4HCO3: 2 grams, resulting mixture is subjected to fine grinding processing with water for ball milling, the wet type carried out 10 hours is ground
The quality proportioning of mill, steel ball, water and material is 10:2:1, obtains average particle size in the slurry of 0.8-1.2um；
(5) it forms
The ground slurry precipitating or Direct Dehydration to pulp density that step (4) is obtained is 60%, then in 700kA/M
Compression forming in magnetic field, being pressed into density is 3.5g/cm3Rule body.
(6) double sintering
Moisture is carried out and organic dispersing agent volatilization is handled in 300 °C of the at a temperature of rule body that obtains to step (5), is then existed
The high-performance permanent-magnet ferrite that the Br that density is 5.08g/cm3 has excessive temperature stability is fired at a temperature of 1230 DEG C.
Br made from embodiment 2 has the high-performance permanent-magnet ferrite of excessive temperature stability through detecting Br:4435Gs；
Hcb:321kA/m；Hcj:394kA/m；(BH) max:38.3kJ/m3;αBrCoefficient: -0.07%/DEG C.
As can be seen from the above embodiments, Br produced by the present invention has the high-performance permanent-magnet ferrite of excessive temperature stability
Br value is not less than 4400Gs, and Hcj value is not less than 394kA/m, and αBrCoefficient not less than -0.1%/DEG C.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (5)
1. the high-performance permanent-magnet ferrite that a kind of Br has excessive temperature stability, it is characterised in that: it is hexagonal crystal M sections oxygen
Body main phase forms expression are as follows: (A1O)1-x(A2O)x•(Fe2O3)k-y-z(B1O)y(B2O)z
Wherein A1For one of elements Sr, Ba, Pb or several, A2For one of Elements C a, La, Bi or several；B1For
One of Co, Zn, Cr are several, B2Ionic compartmentation is carried out to Fe for several combination addition of Cu, Ge, Si, V, Nb, Ta；
And 0≤x≤0.6,3≤k≤6,0≤y≤0.6,0≤z≤0.4.
2. Br according to claim 1 has the preparation method of the high-performance permanent-magnet ferrite of excessive temperature stability,
It is characterized in that: specifically comprising the following steps:
(1) ingredient is handled
According to ingredient formula (A1O)1-x(A2O)x•(Fe2O3)k-y-z(B1O)y(B2O)zMolar ratio, calculate A1、A2、Fe、B1With
B2Quality needed for the oxide or metallic salt ingredient of five elements is simultaneously weighed, and the average particle size of each ingredient is less than
10um, purity are greater than 96.5%；Then in addition to croci starting material with water ball milling or sand mill carry out fine grinding processing,
Wet lapping in 5 ~ 10 hours is carried out, the quality proportioning of steel ball, water and material is (8-20): (1.5-3): 1, make to obtain mixture
Expect that average particle size is not more than 1.5 um；
(2) it mixes
Croci will be added in mixed material that step (1) obtains, and an additive is added, one time additive is
SiO2, H3BO3, NH4HCO3 are one or more of, and adding proportion is SiO2:0%~0.6%, H3BO3:0~0.3%, NH4HCO3:0
~0.3%；It is mixed and is crushed by water for ball milling or sand mill again, carry out wet lapping in 1 ~ 4 hour, steel ball, water and material
Quality proportioning is (8-20): (1.5-3): 1, make to obtain mixed material average particle size no more than 1.5 um；
(3) pre-burning
By mixed material that step (2) obtains in drying at a temperature of 250-300 DEG C in baking oven, keep moisture content after drying small
In 5%；Then pre-burning is carried out, calcined temperature is 1100 ~ 1360 DEG C, and high temperature burn-in time is 50 minutes ~ 150 minutes；Finally carry out
Pulverization process makes 2 ~ 6 μm of smashed average particle size；
(4) secondary grinding
The preburning powdered material that step (3) obtains is weighed, secondary additive is added, secondary additive includes calcium carbonate powder, strontium carbonate
Powder, silicon oxide powder, boric acid powder, the one or more of NH4HCO3 powder, dispersing agent, by resulting mixture water polo
Mill or sand mill carry out fine grinding processing, carry out wet lapping in 6 ~ 12 hours, the quality proportioning of steel ball, water and material is (8-20):
(1.5-3): 1, average particle size is obtained in the slurry of 0.8-1.2um；
(5) it forms
The ground slurry precipitating or Direct Dehydration to pulp density that step (4) is obtained is 55% ~ 70%, then in 500-
Compression forming in the magnetic field 800kA/M, being pressed into density is 3.0 ~ 3.6g/cm3Rule body；
Double sintering
Moisture is carried out and organic dispersing agent volatilization is handled in 100-400 °C of the at a temperature of rule body that obtains to step (5), then
It is the high-performance that 4.9 ~ 5.2g/cm3 has excessive temperature stability to get Br that density is fired at a temperature of 1150 ~ 1250 DEG C
Permanent-magnet ferrite.
3. Br according to claim 2 has the preparation method of the high-performance permanent-magnet ferrite of excessive temperature stability,
It is characterized in that: the secondary additive preferred embodiment being added in the step (4) into preburning powdered material are as follows: be added by weight ratio
Calcium carbonate powder 0.3%~1.2%, strontium carbonate powder 0.2%~1.0%, silicon oxide powder 0.0.05~0.5%, boric acid powder 0.05
~0.2%, dispersing agent total amount 0.1~0.8%.
4. Br according to claim 3 has the preparation method of the high-performance permanent-magnet ferrite of excessive temperature stability,
Be characterized in that: the dispersing agent is D-sorbite, calcium gluconate or ascorbic acid.
5. Br according to claim 2 has the preparation method of the high-performance permanent-magnet ferrite of excessive temperature stability,
Be characterized in that: it is 1200 °C~1250 °C that preferred sintering temperature, which is sintering temperature, in the step (6).
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Citations (3)
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|---|---|---|---|---|
| CN101106001A (en) * | 2006-06-19 | 2008-01-16 | 李凌峰 | Low-temperature coefficient permanent magnet ferrite material and its production method |
| CN103342552A (en) * | 2013-07-01 | 2013-10-09 | 上海应用技术学院 | Nanocrystal M-shaped ferrite powder and synthesis method thereof |
| CN107673755A (en) * | 2017-10-31 | 2018-02-09 | 安徽龙磁科技股份有限公司 | A kind of preparation method of permanent-magnet ferrite |
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2018
- 2018-11-08 CN CN201811322223.4A patent/CN109133903A/en active Pending
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|---|---|---|---|---|
| CN101106001A (en) * | 2006-06-19 | 2008-01-16 | 李凌峰 | Low-temperature coefficient permanent magnet ferrite material and its production method |
| CN103342552A (en) * | 2013-07-01 | 2013-10-09 | 上海应用技术学院 | Nanocrystal M-shaped ferrite powder and synthesis method thereof |
| CN107673755A (en) * | 2017-10-31 | 2018-02-09 | 安徽龙磁科技股份有限公司 | A kind of preparation method of permanent-magnet ferrite |
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| 王自敏: "《铁氧体生产工艺技术》", 31 January 2013, 重庆大学出版社 * |
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Application publication date: 20190104 |