CN103304230A - Permanent magnetic ferrite low-temperature pre-sintering powder and preparation method thereof - Google Patents
Permanent magnetic ferrite low-temperature pre-sintering powder and preparation method thereof Download PDFInfo
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- CN103304230A CN103304230A CN2013102330340A CN201310233034A CN103304230A CN 103304230 A CN103304230 A CN 103304230A CN 2013102330340 A CN2013102330340 A CN 2013102330340A CN 201310233034 A CN201310233034 A CN 201310233034A CN 103304230 A CN103304230 A CN 103304230A
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Abstract
The invention provides a preparation method of permanent magnetic ferrite low-temperature pre-sintering powder. The ferrite pre-sintering material is a permanent magnetic ferrite material of a hexagonal crystal system taking strontium as one of the major raw materials, and the molecular formula is SrO.mFe2O3, wherein m is greater than 5 and less than 6; and a low-melting sintering aid is a mixture of two or more of CaCO3, SiO2 and ZrO2, wherein the dosage of CaCO3 (z%) accounts for 1-10% of the total material weight, the dosage of SiO2 (y%) accounts for 0.1-10% of the total material weight, and the dosage of ZrO2 (wt%) accounts for 0-5% of the total material weight. The preparation method comprises the following steps of: (1) mixing Fe2O3 and strontium carbonate powder; (2) performing wet-process ball milling on the mixture to obtain slurry; (3) pressing the slurry into a cake and drying and directly pre-sintering; and (4) performing dry-type coarse grinding on the pre-sintered material. By adopting the processes such as optimization of a raw material formula, a superfine powder ball milling technology, addition of a low-melting sintering aid and the like, the preparation method provided by the invention produces high-performance strontium ferrite low-temperature pre-sintering powder, and the pre-sintering temperature is 100 DEG C lower than that of a conventional pre-sintering material; and meanwhile, the preparation method has the advantages of simple production technology and low energy consumption, and brings broad social and economic benefits.
Description
Technical field
The invention belongs to the permanent-magnet ferrite field, specifically a kind of permanent-magnet ferrite low temperature presintering powder and preparation method thereof.
Background technology
China's permanent-magnet ferrite output occupies first place in the world, and is magnetic material product big producing country.The ferrite industry of China in the past few years remains essentially in the speed increment more than 20%, and average per five annual production are doubled.Research and develop high trade mark permanent magnet oxysome becomes the main direction and goal of Chinese scholar and enterprise always.Pre-burning is to produce one of ferritic important procedure of high magnetic characteristics.The production technique of ferrite prefiring material is at present: iron oxide red+Strontium carbonate powder-batch mixing-cake of press-drying-pre-burning-pulverizing-ferrite prefiring material powder.Traditional Preburning material production is with ferro-magnetic (Fe
3O
4Be the byproduct of hot rolling carbon steel), pass through high temperature oxidation, and mix, dry with carbonate through ball milling, add an amount of water, be made into the adobe shape with wooden pattern, then be placed on and carry out the high temperature pre-burning in the kiln, make and tentatively finish solid state reaction between the feed particles, to reach part Ferrite method in the mixed oxide.The shortcoming of this Preburning material in the pre-burning process be that sintering temperature is high, production cost is high, yield poorly, the consistence of Preburning material crystallization is poor, thereby seriously affected ferritic quality.
Although, domestic existing Patents " a kind of rubber ferromagnetic oxide powder and preparation method thereof (patent No. 200810238930.5) " employing iron oxide red and Strontium carbonate powder or barium carbonate are raw material at present, and preferably select to be added with to be beneficial to and improve the low temperature presintering effect and control the additive (SiO that crystal grain is given birth to
2Or CaCO
3), through presintering and pulverization process, obtain having the magnetic than high magnetic characteristics and processing characteristics.But also exist calcined temperature up to 1300 ℃, the problem that Preburning material crystallization consistence is poor.
Summary of the invention
Problem in view of above-mentioned existence, this patent adopts composition of raw materials optimization, ultrafine powder ball-milling technology, and add the method such as eutectic sintering agent, produce a kind of ferrite low temperature presintering powder of Preburning material crystallization high conformity, its calcined temperature is than low 60 ℃ of conventional Preburning material, enhances productivity significantly and reduces cost.
A kind of permanent-magnet ferrite low temperature presintering powder is characterized in that it forms the hexaplanar permanent-magnet ferrite material by strontium as one of main starting material, its molecular formula SrOmFe
2O
3, 5＜m＜6 wherein.
The preparation method of described a kind of permanent-magnet ferrite low temperature presintering powder is characterized in that comprising the steps:
(1) with Fe
2O
3Mix Fe with strontium carbonate powder
2O
3With the mol ratio of Strontium carbonate powder be m:1, m=5～6;
(2) above-mentioned compound is added the eutectic sintering agent, carry out wet ball grinding, Ball-milling Time is 1-5 hour, becomes slip behind the ball milling;
(3) above-mentioned slip is pressed into the Preburning material cake post-drying, then carries out presintering, calcined temperature is 1180 ℃-1250 ℃, and soaking time is controlled at 2-5 hour, generates strontium ferrites;
(4) Preburning material cake is carried out the dry type corase grind, namely obtain the strontium ferrites preburning powdered material.
Described preparation method is characterized in that described eutectic sintering agent is CaCO
3, SiO
2And ZrO
2In two kinds and two or more mixture, wherein CaCO
3Addition accounts for 1%-10% of total material weight, SiO
2Addition accounts for 0.1%-10% of total material weight, ZrO
2Addition accounts for 0-5% of total material weight.
Described preparation method is characterized in that described Fe
2O
3Preferred feedstock is purity greater than 99% iron oxide red.
Described preparation method is characterized in that the mean particle size that described slip is worn into is controlled at 0.5-1 μ m.
The process of preparing of a kind of ferrite low temperature presintering powder of the present invention, by choose reasonable, the ultrafine powder ball-milling technology to composition of raw materials, and add the method such as eutectic sintering agent, calcined temperature is controlled at 1180 ℃-1250 ℃, produces the high magnetic characteristics ferrite low temperature presintering powder of mean particle size 1～5 μ m, powder remanent magnetism Br=410 ± 10mT, powder coercive force (Hcj)=320 ± 15 kA/m.It is simple that this invention has technique, the advantage that production cost is low, energy consumption is low
Embodiment
Embodiment 1
The mol ratio of mixing by iron oxide red and Strontium carbonate powder is the 5:1 weigh batching, adds an amount of eutectic sintering agent, wherein CaCO
3Addition accounts for the 1wt% of total material weight, SiO
2Addition accounts for the 10wt% of total material weight, ZrO
2Addition is 2wt%, and wet mixing ball milling 1 hour makes the batch mixing homogeneous chemical composition behind the ball milling, and Slurry Granularity is controlled at about 0.5 μ m; After slurry is pressed into pre-sesame seed cake, puts into rotary kiln and carry out pre-burning, calcined temperature is 1240 ℃, and soaking time is controlled at 3 hours, generates strontium ferrites after the pre-burning.Preburning material is put into ball mill carry out the dry type corase grind, mean particle size 5 μ m after the dry grinding, and obtain narrower size-grade distribution; At this moment, powder remanent magnetism Br=410 ± 10mT; Powder coercive force (Hcj)=320 ± 15 kA/m.
Embodiment 2
The mol ratio of mixing by iron oxide red and Strontium carbonate powder is the 6:1 weigh batching, adds an amount of eutectic sintering agent, wherein CaCO
3Addition accounts for the 10wt% of total material weight, SiO
2Addition accounts for the 0.1wt% of total material weight, ZrO
2Addition is 5wt%, and wet mixing ball milling 5 hours makes the batch mixing homogeneous chemical composition behind the ball milling, and Slurry Granularity is controlled at about 1 μ m; After slurry is pressed into pre-sesame seed cake, puts into tunnel furnace and carry out pre-burning, calcined temperature is 1200 ℃, and soaking time is controlled at 2 hours, generates strontium ferrites after the pre-burning.Preburning material is put into ball mill carry out the dry type corase grind, mean particle size 2 μ m after the dry grinding, and obtain narrower size-grade distribution; At this moment, powder remanent magnetism Br=410 ± 10mT; Powder coercive force (Hcj)=320 ± 15 kA/m.
Embodiment 3
The mol ratio of mixing by iron oxide red and Strontium carbonate powder is the 5.5:1 weigh batching, adds an amount of eutectic sintering agent, wherein CaCO
3Addition accounts for the 8wt% of total material weight, SiO
2Addition accounts for the 5wt% of total material weight, ZrO
2Addition is 1wt%, and wet mixing ball milling 3 hours makes the batch mixing homogeneous chemical composition behind the ball milling, and Slurry Granularity is controlled at about 0.6 μ m; After slurry is pressed into pre-sesame seed cake, puts into tunnel furnace and carry out pre-burning, calcined temperature is 1240 ℃, and soaking time is controlled at 1.5 hours, generates strontium ferrites after the pre-burning.Preburning material is put into ball mill carry out the dry type corase grind, mean particle size 4 μ m after the dry grinding, and obtain narrower size-grade distribution; At this moment, powder remanent magnetism Br=420 ± 10mT; Powder coercive force (Hcj)=320 ± 15 kA/m.
Embodiment 4
The mol ratio of mixing by iron oxide red and Strontium carbonate powder is the 5.2:1 weigh batching, adds an amount of eutectic sintering agent, wherein CaCO
3Addition accounts for the 4wt% of total material weight, SiO
2Addition accounts for the 8wt% of total material weight, and wet mixing ball milling 2 hours makes the batch mixing homogeneous chemical composition behind the ball milling, and Slurry Granularity is controlled at about 0.8 μ m; After slurry is pressed into pre-sesame seed cake, puts into tunnel furnace and carry out pre-burning, calcined temperature is 1180 ℃, and soaking time is controlled at 2.5 hours, generates strontium ferrites after the pre-burning.Preburning material is put into ball mill carry out the dry type corase grind, mean particle size 1 μ m after the dry grinding, and obtain narrower size-grade distribution; At this moment, powder remanent magnetism Br=415 mT; Powder coercive force (Hcj)=315 kA/m.
The above only is preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces and improvement etc., all is included within protection scope of the present invention.
Claims (5)
1. a permanent-magnet ferrite low temperature presintering powder is characterized in that it forms the hexaplanar permanent-magnet ferrite material by strontium as one of main starting material, its molecular formula SrOmFe
2O
3, 5＜m＜6 wherein.
2. the preparation method of a kind of permanent-magnet ferrite low temperature presintering powder as claimed in claim 1 is characterized in that comprising the steps:
(1) with Fe
2O
3Mix Fe with strontium carbonate powder
2O
3With the mol ratio of Strontium carbonate powder be m:1, m=5～6;
(2) above-mentioned compound is added the eutectic sintering agent, carry out wet ball grinding, Ball-milling Time is 1-5 hour, becomes slip behind the ball milling;
(3) above-mentioned slip is pressed into the Preburning material cake post-drying, then carries out presintering, calcined temperature is 1180 ℃-1250 ℃, and soaking time is controlled at 2-5 hour, generates strontium ferrites;
(4) Preburning material cake is carried out the dry type corase grind, namely obtain the strontium ferrites preburning powdered material.
3. preparation method as claimed in claim 2 is characterized in that described eutectic sintering agent is CaCO
3, SiO
2And ZrO
2In two kinds and two or more mixture, wherein CaCO
3Addition accounts for 1%-10% of total material weight, SiO
2Addition accounts for 0.1%-10% of total material weight, ZrO
2Addition accounts for 0-5% of total material weight.
4. preparation method as claimed in claim 2 is characterized in that described Fe
2O
3Preferred feedstock is purity greater than 99% iron oxide red.
5. preparation method as claimed in claim 2 is characterized in that the mean particle size that described slip is worn into is controlled at 0.5-1 μ m.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103626485A (en) * | 2013-12-13 | 2014-03-12 | 湖南航天磁电有限责任公司 | Production method of permanent magnetic ferrite pre-sintering material |
| CN106145917A (en) * | 2016-06-23 | 2016-11-23 | 南京航空航天大学 | A kind of coercitive secondary of permanently magnetic strontium ferrite that improves is combined adding method |
| CN106673638A (en) * | 2016-12-26 | 2017-05-17 | 浙江中科磁业有限公司 | Method for producing pre-sintering material |
| CN106747390A (en) * | 2016-12-30 | 2017-05-31 | 攀枝花钢城集团有限公司 | Strontium ferrite powder and preparation method thereof |
| CN107721405A (en) * | 2017-11-16 | 2018-02-23 | 安徽鑫磁源磁业有限公司 | A kind of low temperature calcination prepares M-type strontium ferrite SrFe12O19The method of Preburning material |
| CN108101528A (en) * | 2017-12-26 | 2018-06-01 | 攀枝花钢城集团有限公司 | A kind of method for improving Strontium ferrite powder remanent magnetism |
| CN108911731A (en) * | 2018-08-30 | 2018-11-30 | 安徽工业大学 | A kind of preparation method of hexaplanar M-type strontium ferrite powder |
| CN109776088A (en) * | 2019-04-01 | 2019-05-21 | 中钢集团南京新材料研究院有限公司 | A kind of preparation method of Strontium ferrite powder |
| CN113651608A (en) * | 2021-08-25 | 2021-11-16 | 上海宝钢磁业有限公司 | Dry-pressing permanent magnetic ferrite and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101055796A (en) * | 2006-04-16 | 2007-10-17 | 张连墩 | Making method for M type Sr-ferrite magnetic material |
-
2013
- 2013-06-13 CN CN201310233034.0A patent/CN103304230B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101055796A (en) * | 2006-04-16 | 2007-10-17 | 张连墩 | Making method for M type Sr-ferrite magnetic material |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103626485A (en) * | 2013-12-13 | 2014-03-12 | 湖南航天磁电有限责任公司 | Production method of permanent magnetic ferrite pre-sintering material |
| CN103626485B (en) * | 2013-12-13 | 2015-03-04 | 湖南航天磁电有限责任公司 | Production method of permanent magnetic ferrite pre-sintering material |
| CN106145917A (en) * | 2016-06-23 | 2016-11-23 | 南京航空航天大学 | A kind of coercitive secondary of permanently magnetic strontium ferrite that improves is combined adding method |
| CN106673638A (en) * | 2016-12-26 | 2017-05-17 | 浙江中科磁业有限公司 | Method for producing pre-sintering material |
| CN106747390A (en) * | 2016-12-30 | 2017-05-31 | 攀枝花钢城集团有限公司 | Strontium ferrite powder and preparation method thereof |
| CN107721405A (en) * | 2017-11-16 | 2018-02-23 | 安徽鑫磁源磁业有限公司 | A kind of low temperature calcination prepares M-type strontium ferrite SrFe12O19The method of Preburning material |
| CN107721405B (en) * | 2017-11-16 | 2020-08-11 | 安徽鑫磁源磁业有限公司 | Preparation of M-type strontium ferrite SrFe through low-temperature calcination12O19Method for pre-firing materials |
| CN108101528A (en) * | 2017-12-26 | 2018-06-01 | 攀枝花钢城集团有限公司 | A kind of method for improving Strontium ferrite powder remanent magnetism |
| CN108911731A (en) * | 2018-08-30 | 2018-11-30 | 安徽工业大学 | A kind of preparation method of hexaplanar M-type strontium ferrite powder |
| CN109776088A (en) * | 2019-04-01 | 2019-05-21 | 中钢集团南京新材料研究院有限公司 | A kind of preparation method of Strontium ferrite powder |
| CN113651608A (en) * | 2021-08-25 | 2021-11-16 | 上海宝钢磁业有限公司 | Dry-pressing permanent magnetic ferrite and preparation method and application thereof |
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| CN103304230B (en) | 2015-01-28 |
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