CN106145918B - A kind of preparation method of high-performance permanent-magnet ferrite - Google Patents
A kind of preparation method of high-performance permanent-magnet ferrite Download PDFInfo
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- CN106145918B CN106145918B CN201610527418.7A CN201610527418A CN106145918B CN 106145918 B CN106145918 B CN 106145918B CN 201610527418 A CN201610527418 A CN 201610527418A CN 106145918 B CN106145918 B CN 106145918B
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Abstract
A kind of preparation method of high-performance permanent-magnet ferrite is that the active carbonic acid strontium used existing in formulation material is replaced with to the mixture of silicon carbide and common strontium carbonate in the ball milling stage of existing manufacture permanent-magnet ferrite.The method of the present invention realizes the stability that magnetic property is kept in broader temperature range, it can reach magnetic property effect identical with addition active carbonic acid strontium, formulation material cost at least declines 300 yuan/ton simultaneously, and the production cost that can be greatly reduced improves the market competitiveness.
Description
Technical field
The present invention relates to a kind of preparation methods of permanent-magnet ferrite, and in particular to a kind of preparation of high-performance permanent-magnet ferrite
Method.
Background technique
With social development, market competition is more and more fierce, is influenced by store financial crisis, and manufacturing industry starts to go down hill
The market competitiveness is improved to reduce operation cost of enterprises in road, requires production cost control very high.
Permanent-magnet ferrite formulation material cost relative magnetism material leading enterprise, our company, such as imperial magnetic, Bei Kuang, it is higher,
In order to improve production pattern, need to reduce the cost of permanent-magnet ferrite, especially formulation material.
The existing method for reducing permanent-magnet ferrite formulation material cost is mainly to subtract in the ball milling stage of manufacture permanent-magnet ferrite
Few formulation material uses or selects cheap formulation material.In formulation material cost it is highest be active carbonic acid strontium (active carbonic acid strontium, i.e.,
Activated treated strontium carbonate), if it is possible to it reduces and does not use it even, will greatly reduce production cost.But at this
In the concrete practice of company, if the permanent-magnet ferrite of the existing high-performance trade mark does not use active carbonic acid strontium, and it is used only commonly
Strontium carbonate (common strontium carbonate, i.e., without any pretreated strontium carbonate), the coercivity of magnet can not increase substantially even
It keeps.It is to lose more than gain for the existence of enterprise if cost brings the risk of product quality variation while reduction
's.
Therefore, in the prior art, formulation material is reduced to use or in the case where selecting cheap formulation material, magnet performance compared with
Low or magnet stability is not high, needs to find that one kind can reduce production cost and even to improve magnet comprehensive
The formulation material of energy.
Summary of the invention
The technical problem to be solved by the present invention is to overcome drawbacks described above of the existing technology, provide one kind and be produced into
This is low, the preparation method for the high-performance permanent-magnet ferrite that permanent-magnet ferrite comprehensive magnetic can be good.
The technical solution adopted by the present invention to solve the technical problems is as follows: a kind of preparation side of high-performance permanent-magnet ferrite
The active carbonic acid strontium used existing in formulation material is replaced with silicon carbide in the ball milling stage of existing manufacture permanent-magnet ferrite by method
With the mixture of common strontium carbonate.Active carbonic acid strontium is a kind of typical additives of permanent-magnet ferrite material, in certain sintering
Within the scope of warm area, magnet can be made to obtain the comprehensive performance of high remanent magnetism, high-coercive force, but price is higher, generally 100,000 yuan/
Ton, and common strontium carbonate price is only 0.6 ten thousand yuan/ton.Common strontium carbonate is thermally decomposed into strontium oxide strontia, can play compact ferrite work
With when n < 6(n is Fe2O3With the molar ratio of SrO) when, superfluous strontium oxide strontia, which has, promotes ferrite solid phase reaction, promotes crystal grain long
Big effect, strontium carbonate can be sintered after being added in wider sintering temperature；Silicon-carbide particle can restrain dislocation at high temperature
Movement is formed " domain wall pinning ", and coercivity is improved, while inhibiting ferrite crystal grains to grow up during the sintering process, increases single domain ratio
Example improves coercivity.The present inventor is the study found that when the mixture using silicon carbide and common strontium carbonate is as formula additive
When, it can further improve the comprehensive performance of permanent-magnet ferrite.
Further, the additive amount of the silicon carbide and common strontium carbonate mixture is preferably permanent ferrite prefiring material quality
0.4~0.8%.The adding too much of the mixture is too low, will lead to permanent-magnet ferrite comprehensive performance and is declined.
Further, in the mixture of the silicon carbide and common strontium carbonate, the mass ratio of silicon carbide and common strontium carbonate is excellent
It is selected as 1:2.5~3.5.Present inventor is found by experiment that common strontium carbonate dosage is too high or too low, and permanent-magnet ferrite is comprehensive
It can all decrease.Since common strontium carbonate price is only 0.6 ten thousand yuan/ton, silicon carbide price is only 10,000 yuan/ton, formulation material
Only about 700 yuan/ton of overall cost in permanent-magnet ferrite preparation.
Further, the concrete operations of the preparation method of the high-performance permanent-magnet ferrite are as follows: by permanent ferrite prefiring material,
The mixture of silicon carbide and common strontium carbonate and other formulation materials are placed in ball mill, add water, ball milling, filtering；Filtering is precipitated
Slurry injection mold afterwards is press-formed into molding green compact under magnetic field condition；Molding green compact are sintered, are polished, i.e.,
At.
In the method for the present invention, the cake of the preferred diameter of phi 30.1mm of shape of the molding green compact of the extrusion forming.
Further, the additional amount of other formulation materials is the 2~3% of permanent ferrite prefiring material quality.Formulation material is added
Amount will excessively improve production cost, and the too low magnetic property that will lead to of additional amount is unable to reach desired effect.
Further, other formulation materials are made of following components and parts by weight: 3~5 parts of calcium carbonate, quartz sand 1~2
Part, 2~4 parts of chromium oxide, 1~3 part of cobalt sesquioxide.The formulation material is to obtain higher permanent magnetic ferrite residual magnetization, coercive
On the basis of power equimagnetic performance indicator, while considering that production cost carries out proportion addition.
Further, described plus water amount is 1.5~2.5 times of permanent ferrite prefiring material quality.Ball milling water is with permanent magnetism
Ferrite prefiring material mass concentration is greater than 40% and is added, while considering ball milling inventory no more than ball mill container volume
2/3。
Further, the average particle size for being milled to slurry is 0.6~1.0 μm.If average particle size is too small, it is tired to will lead to molding
Difficulty can be substantially reduced magnet coercivity if average particle size is excessive.
Further, filtering to the moisture content of precipitating is 32~35wt%.If moisture content is excessively high, size mistake after sintering will lead to
It is small, grinding is influenced, if moisture content is too low, slurry mobility is poor, influences green compact compacting.
Further, the intensity in the magnetic field is 500~600kA/m；The pressure of pressurization be 13~18MPa, the time be 60~
80s。
Further, the temperature of the sintering is 1170~1190 DEG C, and the time of sintering is 100~150min, the speed of heating
Rate is 2~4 DEG C/min.Higher temperature is sintered the permanent-magnet ferrite that can get high remanent magnetism, low-coercivity performance, and lower temperature is burnt
The permanent-magnet ferrite that can get high-coercive force, low remanent magnetism performance is tied, sintering temperature is regulated and controled according to specific needs.
The method of the present invention has the beneficial effect that by replacing active carbonic acid with the mixture of silicon carbide and common strontium carbonate
Strontium realizes the stability that magnetic property is kept in broader temperature range, can reach magnetic identical with addition active carbonic acid strontium
The impact of performance, while formulation material cost at least declines 300 yuan/ton, greatly reduces production cost, improves market competition
Power.
Specific embodiment
Below with reference to embodiment, the invention will be further described.
Permanent ferrite prefiring material used in the embodiment of the present invention, comparative example is that had by the Zhejiang ZMS-7H(An Te magnetic material
Limit company) with HMS-6(Wuhan Steel Group Refractory Materials Co., Ltd.) with the mass ratio of 1:1 mix gained；The present invention
Strontium carbonate used in embodiment is purchased from Wuhan Steel Group Refractory Materials Co., Ltd.；Used in comparative example of the present invention
Active carbonic acid strontium is purchased from the Miluo River source of students Chemical Co., Ltd.；Chemical reagent used in other, unless otherwise specified, by normal
Commercial sources are advised to obtain.
Examples 1 to 3
In Examples 1 to 3, respectively by 500g permanent ferrite prefiring material, mixture (each reality of silicon carbide and strontium carbonate
Applying a dosage, see Table 1 for details), 4g calcium carbonate, 1.5g quartz sand, 3g chromium oxide and 2g cobalt sesquioxide are placed in ball mill, add water
1000g is milled to the slurry that average particle size is 0.8 μm, and it is 33wt% that the good slurry filtration of ball milling, which is precipitated to water content,；Incited somebody to action
Slurry after filter precipitating injects mold, is 530kA/m in magnetic field strength, under conditions of pressure is 15Mpa, pressurization 65s is shaped to
The round pie of diameter of phi 30.1mm forms green compact；Molding green compact are put into sintering electrical kiln, with heating rate for 3 DEG C/min,
Under 1170~1190 DEG C (see Table 1 for details for each embodiment temperature), it is sintered 120min, the upper and lower surfaces of the cake through oversintering are ground
Polishing is cut, permanent-magnet ferrite is obtained.
Using TYU-2000 type auto measurement equipment for magnetic material, test can be carried out to the magnetism of obtained product, test
It the results are shown in Table 1.
Permanent-magnet ferrite magnetic property tables of data obtained by 1 Examples 1 to 3 of table
Comparative example 1~3
Comparative example 1~3 is only that with the difference of Examples 1 to 3: the silicon carbide+strontium carbonate added in ball milling is mixed
Object replaces with active carbonic acid strontium (see Table 2 for details for each comparative example dosage).It is remaining corresponding identical as Examples 1 to 3.
Using TYU-2000 type auto measurement equipment for magnetic material, test can be carried out to the magnetism of obtained product, survey
Test result is referring to table 2.
2 comparative example of table, 1~3 gained permanent-magnet ferrite magnetic property tables of data
Table 1,2 is compared it is found that active carbonic acid strontium institute is substituted with silicon carbide+common strontium carbonate in Examples 1 to 3
The magnetic property for obtaining permanent-magnet ferrite is held essentially constant, and still, the cost of silicon carbide is 10,000 yuan/ton, the cost of common strontium carbonate
It is 0.6 ten thousand yuan/ton, and the cost of active carbonic acid strontium is 100,000 yuan/ton, therefore, according to the dosage of formulation material in the method for the present invention,
The formulation material cost for preparing permanent-magnet ferrite can at least decline 300 yuan/ton.
In conclusion the method for the present invention passes through the mixture replacing active carbonic acid strontium with silicon carbide and common strontium carbonate, drop
Low production cost, maintains preferable permanent-magnet ferrite comprehensive magnetic energy.
Claims (8)
1. a kind of preparation method of high-performance permanent-magnet ferrite, it is characterised in that: by permanent ferrite prefiring material, silicon carbide and general
The mixture and other formulation materials of logical strontium carbonate are placed in ball mill, add water, ball milling, filtering；By the slurry note after filtering precipitating
Enter mold, under magnetic field condition, is press-formed into molding green compact；Molding green compact are sintered, are polished,；The carbonization
The additive amount of silicon and common strontium carbonate mixture is the 0.4~0.8% of permanent ferrite prefiring material quality；The silicon carbide and general
In the mixture of logical strontium carbonate, the mass ratio of silicon carbide and common strontium carbonate is 1:2.5~3.5；Other formulation materials add
Enter 2~3% that amount is permanent ferrite prefiring material quality；Other formulation materials are made of following components and parts by weight: calcium carbonate
3~5 parts, 1~2 part of quartz sand, 2~4 parts of chromium oxide, 1~3 part of cobalt sesquioxide.
2. the preparation method of high-performance permanent-magnet ferrite according to claim 1, it is characterised in that: described plus water amount is forever
1.5~2.5 times of magnetic ferrites Preburning material quality.
3. the preparation method of high-performance permanent-magnet ferrite according to claim 1 or claim 2, it is characterised in that: be milled to slurry
Average particle size is 0.6~1.0 μm；The moisture content of filtering to precipitating is 32~35wt%.
4. the preparation method of high-performance permanent-magnet ferrite according to claim 1 or claim 2, it is characterised in that: the magnetic field it is strong
Degree is 500~600kA/m；The pressure of pressurization is 13~18MPa, and the time is 60~80s.
5. the preparation method of high-performance permanent-magnet ferrite according to claim 3, it is characterised in that: the intensity in the magnetic field is
500~600kA/m；The pressure of pressurization is 13~18MPa, and the time is 60~80s.
6. the preparation method of high-performance permanent-magnet ferrite according to claim 1 or claim 2, it is characterised in that: the temperature of the sintering
Degree is 1170~1190 DEG C, and the time of sintering is 100~150min, and the rate of heating is 2~4 DEG C/min.
7. the preparation method of high-performance permanent-magnet ferrite according to claim 3, it is characterised in that: the temperature of the sintering is
1170~1190 DEG C, the time of sintering is 100~150min, and the rate of heating is 2~4 DEG C/min.
8. the preparation method of high-performance permanent-magnet ferrite according to claim 4, it is characterised in that: the temperature of the sintering is
1170~1190 DEG C, the time of sintering is 100~150min, and the rate of heating is 2~4 DEG C/min.
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| CN106673637A (en) * | 2016-12-14 | 2017-05-17 | 湖南航天磁电有限责任公司 | Permanent magnetic ferrite preparation method with improved formula materials |
| CN107954705A (en) * | 2017-12-05 | 2018-04-24 | 湖南航天磁电有限责任公司 | A kind of manufacturing technique method of high-performance permanent-magnet ferrite Preburning material |
| CN111960816B (en) * | 2020-08-27 | 2022-04-19 | 安徽万磁电子有限公司 | Preparation process of permanent magnetic ferrite |
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