CN101712556A - Method for synthesizing presintering hard ferrite material - Google Patents
Method for synthesizing presintering hard ferrite material Download PDFInfo
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- CN101712556A CN101712556A CN200910197783A CN200910197783A CN101712556A CN 101712556 A CN101712556 A CN 101712556A CN 200910197783 A CN200910197783 A CN 200910197783A CN 200910197783 A CN200910197783 A CN 200910197783A CN 101712556 A CN101712556 A CN 101712556A
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- presintering
- hard ferrite
- ball milling
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- ferrite material
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Abstract
The invention discloses a method for synthesizing a presintering hard ferrite material, which takes one or more of oxide or carbonate of ferrite cations and other additives such as CaO, Al2O3 and the like as raw materials, and comprises the following steps: ball milling and tempering, drying, heating by a microwave physical field with the frequency of 300-3,000MHz, raising the temperature to 1,150-1,350 DEG C at the heating-warming speed of 20-80 DEG C/min, and preserving the temperature for 30-180min to obtain the single-phase presintering hard ferrite material with the grain size being about 0.2-2 mu m. Compared with the traditional method for synthesizing presintering materials, the method in the invention has the advantages of short presintering time, low energy consumption, fine and uniform grains of the presintering materials, good moldability and stable magnetic performance, and can be used for preparing sintering bodies by wet compression moulding and dry compression moulding.
Description
Technical field
The present invention relates to a kind of synthetic method of presintering hard ferrite material.The new technical field that belongs to the magneticsubstance preparation.
Background technology
Ferrite is a kind of ferromagnetic metal oxide that has, and the raw material that production technique is produced permanent-magnet ferrite mainly is the oxide compound (Fe of Powdered iron
2O
3Deng), MO (M:Ba, Sr etc.) or to adding the M salts substances that heat energy is easy to form oxide compound.Dusty raw materials is mixed, and pre-burning in oxidizing atmosphere makes it that solid state reaction take place, and generates MO6Fe
2O
3The magnetic phase, Here it is, and ferrimagnet is produced used material, is called pre-imitation frosted glass.
The raw material that ferrite prefiring material is produced as permanent-magnet ferrite after pre-imitation frosted glass is pulverized, through dry method or wet method extrusion forming, then carries out double sintering, could obtain ferrimagnet at last after carrying out precision work on the grinding machine.The height of therefore pre-imitation frosted glass performance has significant effects to ferritic preparation.Pre-imitation frosted glass normally adopts Fe
2O
3, SrCO
3And other additive (CaO, Al
2O
3, Nd
2O
3, La
2O
3, Co
2O
3Deng) through the high-temperature roasting synthetic, synthesis conditions such as calcined temperature, soaking time and content of additive have very big influence to the structure and the performance of pre-imitation frosted glass.
Method for preparing permanent magnetic ferrite is divided into solid reaction process and chemical synthesis substantially.The ferrite chemical synthesis process has coprecipitation method, amorphous crystallization method, self propagating high temperature synthesis method, hydrothermal synthesis method, mechanical alloying method and sol-gel method etc.But use maximum still solid reaction processes in the actual industrial production, can obtain high performance pre-imitation frosted glass by lower cost.
At present, the pre-common rotary kiln of imitation frosted glass carries out the pre-burning process, finishes the solid state reaction of ferriteization; reaction process not only temperature can be up to 1300 ℃ about; reaction times also reached about 4 hours, and it is bigger to add in the reaction process heat radiation of rotary kiln body, made reaction process energy consumption height.
The present invention is by introducing the mode of microwave heating, make the interaction that utilizes powder and microwave in the powder building-up process, the quick heating of powder self, improve the combined coefficient of powder, reduced cost, simultaneously since microwave to apply and remove speed fast, and then help controlling the length of the duration of heat, thereby can effectively control the grain-size of synthetic powder.
Summary of the invention
The objective of the invention is to propose a kind of presintering hard ferrite material synthetic method.Compare with the pre-imitation frosted glass synthetic method of tradition, this method pre-burning generated time is short, and synthetic energy consumption is low, the pre-tiny homogeneous of imitation frosted glass crystal grain, and good moldability, magnetic property is stable, can be used for Wet-pressing molding, dry-pressing formed preparation sintered compact.
Technical scheme of the present invention
A kind of presintering hard ferrite material synthetic method, its building-up process comprises the following steps:
(1), proportion of raw materials is calculated
With the cationic, oxidized thing of ferrite, carbonate and additive by the cationic, oxidized thing of ferrite: carbonate: the mol ratio of additive is 5.6～6: 1: 0.005～0.05 prepares burden;
Wherein the oxide compound of iron is Fe
2O
3
Wherein carbonate is Pb (CO
3)
2, Fe (CO
3)
2Or Sr (CO
3)
2
Wherein additive is CaO, Al
2O
3, Nd
2O
3, La
2O
3Or Co
2O
3In one or more;
(2), the mixing of raw material
With the raw material of step (1) gained by water: the raw material gross weight: ball milling with ball by mass ratio 1: 1.5～2.5: 1.5～3 ball grinder batch mixing of packing into, rotational speed of ball-mill 150～250r/min, ball milling 1～4h, the ball milling slurry;
(3), drying is anhydrated
The ball milling slurry of step (2) gained is staticly settled anhydrate branch or Electric heat oven drying 12～24h;
(4), material is handled
To be pressed into piece or clay into power through the dried material of step (3), pack into anti-more than 1400 ℃ container or be placed on the refractory slab;
The caked material of dry-pressing formed preparation wherein also can adopt Wet-pressing molding;
(5), microwave calcination
The one-tenth piece of step (4) or the material of claying into power are put into microwave oven, adopting frequency is the microwave physical field heating of 300～3000MHz, heat temperature raising speed with 20～80 ℃/min is warmed up to 1150～1350 ℃, be incubated 30～180min then, can obtain the presintering hard ferrite material runic that particle diameter is about 0.2～2 μ m;
(6), pre-burning pellet abrasive dust is broken
After the presintering hard ferrite material runic cooling with step (5) gained, take out secondary ball milling, control rotational speed of ball-mill 150～250r/min, ball milling 5～10h promptly gets the presintering hard ferrite material that particle diameter of the present invention is about 0.2～2 μ m.
Beneficial effect of the present invention
A kind of presintering hard ferrite material synthetic method of the present invention, with respect to existing ferrite prefiring preparation method for material, this method has short, synthetic low, the characteristics such as synthetic powder crystal grain is evenly distributed, stable performance of energy consumption of generated time, and the synthetic powder compacting is good, is suitable for mass production.A kind of presintering hard ferrite material synthetic method of the present invention also can be used for the synthetic of soft magnetic ferrite and the pre-imitation frosted glass powder of other pottery.
Description of drawings
The XRD figure spectrum of Fig. 1, ferrite prefiring material
The SEM collection of illustrative plates of Fig. 2, ferrite prefiring material
The magnetic hysteresis loop of Fig. 3, ferrite prefiring material
Embodiment
Also in conjunction with the accompanying drawings the present invention is further set forth below by embodiment, but do not limit the present invention.
Embodiment 1
With the pre-imitation frosted glass of strontium ferrites is example, a kind of synthetic method of presintering hard ferrite material.
(1), calculates Fe by 5.8: 1: 0.01 mol ratios
2O
3, SrCO
3And Nd
2O
3Proportioning, weighing then;
(2), with load weighted material with water, material, the ball mass ratio ball grinder batch mixing of packing at 1: 2: 2, rotational speed of ball-mill 200r/min, ball milling 2h;
(3), the ball milling slurry is staticly settled the dry 20h of the branch Electric heat oven that anhydrates;
(4), dried material is put into alumina crucible;
(5), the alumina crucible that material will be housed is put into microwave oven, adopting frequency is the microwave physical field heating of 2450MHz, heat temperature raising speed with 50 ℃/min is warmed up to 1215 ℃, is incubated 60min then, can obtain the single-phase ferrite prefiring material that particle diameter is about 0.8 μ m;
(6), after the cooling of the pre-imitation frosted glass of synthetic, take out secondary ball milling, control rotational speed of ball-mill 220r/min, ball milling 5h promptly gets the presintering hard ferrite material that particle diameter of the present invention is about 0.8 μ m.
Utilize XRD that sample is carried out structured testing, see accompanying drawing 1, the thing of its diffraction peak correspondence is SrFe mutually
12O
19
Utilize SEM etc. that sample is carried out the pattern test, see accompanying drawing 2, uniform crystal particles, the about 0.8 μ m of median size;
Utilize VSM etc. that sample is carried out performance test, see accompanying drawing 3, its saturation magnetization is 40emu/g.
Embodiment 2
With the barium ferrite pre-sintered material is example, a kind of synthetic method of presintering hard ferrite material.
(1), calculates Fe by 5.6: 1: 0.02 mol ratios
2O
3, BaCO
3And La
2O
3Proportioning, weighing then;
(2), with load weighted material with water, material, the ball mass ratio ball grinder batch mixing of packing at 1: 2: 2, rotational speed of ball-mill 200r/min, ball milling 2h;
(3), the ball milling slurry is staticly settled the dry 20h of the branch Electric heat oven that anhydrates;
(4), dried material is put into alumina crucible;
(5), the alumina crucible that material will be housed is put into microwave oven, adopting frequency is the microwave physical field heating of 3000MHz, heat temperature raising speed with 70 ℃/min is warmed up to 1150 ℃, is incubated 80min then, can obtain the single-phase ferrite prefiring material that particle diameter is about 0.9 μ m;
(6), after the cooling of the pre-imitation frosted glass of synthetic, take out secondary ball milling, control rotational speed of ball-mill 200r/min, ball milling 5h promptly gets the presintering hard ferrite material that particle diameter of the present invention is about 0.9 μ m.
Embodiment 3
With the pre-imitation frosted glass of lead ferrite is example, a kind of synthetic method of presintering hard ferrite material.
(1), calculates Fe by 1: 5.8: 0.025 mol ratio
2O
3, PbCO
3With the proportioning of CaO, weighing then;
(2), with load weighted material with water, material, the ball mass ratio ball grinder batch mixing of packing at 1: 2: 2, rotational speed of ball-mill 200r/min, ball milling 2h;
(3), the ball milling slurry is staticly settled the dry 2h of the branch Electric heat oven that anhydrates;
(4), dried material is put into alumina crucible;
(5), the alumina crucible that material will be housed is put into microwave oven, adopting frequency is the microwave physical field heating of 300MHz, heat temperature raising speed with 30 ℃/min is warmed up to 1300 ℃, is incubated 60min then, can obtain the single-phase ferrite prefiring material that particle diameter is about 1.5 μ m;
(6), after the cooling of the pre-imitation frosted glass of synthetic, take out secondary ball milling, control rotational speed of ball-mill 180r/min, ball milling 8h promptly gets the presintering hard ferrite material that particle diameter of the present invention is about 1.5 μ m.
Claims (3)
1. a presintering hard ferrite material synthetic method is characterized in that its building-up process comprises the following steps:
(1), proportion of raw materials is calculated
With the cationic, oxidized thing of ferrite, carbonate and additive by the cationic, oxidized thing of ferrite: carbonate: the mass ratio of additive is 5.6～6: 1: 0.005～0.05 prepares burden;
Wherein the cationic, oxidized thing of ferrite is Fe
2O
3
Wherein carbonate is SrCO
3, BaCO
3Or PbCO
3
Wherein additive is CaO, Al
2O
3, Nd
2O
3, La
2O
3Or Co
2O
3In one or more;
(2), the mixing of raw material
Raw material is by water: the raw material gross weight: ball milling with ball by mass ratio 1: 1.5～2.5: 1.5～3 ball grinder batch mixing of packing into, rotational speed of ball-mill 150～250r/min, ball milling 1～4h, the ball milling slurry;
(3), drying is anhydrated
The ball milling slurry of step (2) gained is staticly settled anhydrate branch or Electric heat oven drying 12～24h;
(4), material is handled
To be pressed into piece or clay into power through the dried material of step (3), pack into anti-more than 1400 ℃ container or be placed on the refractory slab;
(5), microwave calcination
The one-tenth piece of step (4) or the material of claying into power are put into microwave oven, adopting frequency is the microwave physical field heating of 300～3000MHz, heat temperature raising speed with 20～80 ℃/min is warmed up to 1150～1350 ℃, is incubated 30～180min then, can obtain the presintering hard ferrite material runic;
(6), pre-burning pellet abrasive dust is broken
After the presintering hard ferrite material runic cooling with step (5) gained, take out secondary ball milling, control rotational speed of ball-mill 150～250r/min, ball milling 5～10h promptly gets presintering hard ferrite material of the present invention.
2. a kind of presintering hard ferrite material synthetic method as claimed in claim 1 is characterized in that the material briquetting in the processing of its synthesis step (4) material adopts dry-pressing formed or the Wet-pressing molding preparation.
3. a kind of presintering hard ferrite material synthetic method as claimed in claim 1 is characterized in that the presintering hard ferrite material particle diameter of gained is about 0.2～2 μ m.
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| CN2009101977836A CN101712556B (en) | 2009-10-28 | 2009-10-28 | Method for synthesizing presintering hard ferrite material |
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| CN101712556B CN101712556B (en) | 2012-06-06 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102503392A (en) * | 2011-10-21 | 2012-06-20 | 武汉理工大学 | Single-phase multi-ferreous strontium-ferrite ceramic material and preparation method thereof |
| CN103408296A (en) * | 2013-08-15 | 2013-11-27 | 上海应用技术学院 | Characterization analysis method for migration of lanthanum and cobalt ions in lanthanum-cobalt substituted strontium ferrite permanent magnet material |
| CN104230325A (en) * | 2013-06-24 | 2014-12-24 | 广东江粉磁材股份有限公司 | Preparation method of permanent magnetic ferrite pre-sintering material and preparation method of permanent magnetic ferrite |
| CN104230326A (en) * | 2013-06-24 | 2014-12-24 | 广东江粉磁材股份有限公司 | Preparation method of M-type calcium permanent magnetic ferrite |
| CN105292990A (en) * | 2015-12-09 | 2016-02-03 | 攀枝花钢城集团有限公司 | Strontium ferrite pre-sintering ball material cooling and storing system and process |
| CN105565793A (en) * | 2015-12-29 | 2016-05-11 | 海安南京大学高新技术研究院 | Method for molten salt assisted sintering of strontium ferrite |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101206941A (en) * | 2006-12-21 | 2008-06-25 | 横店集团东磁股份有限公司 | Method of preparing high magnetoconductivity low temperature co-baking NiCuZn ferrite |
| CN101492286A (en) * | 2009-01-13 | 2009-07-29 | 沈阳选矿机械研究所 | Process for producing permanent ferrite with high-fracture toughness property |
| CN101462872B (en) * | 2009-01-21 | 2011-09-14 | 电子科技大学 | Low frequency microstrip aerial substrate material and preparation thereof |
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2009
- 2009-10-28 CN CN2009101977836A patent/CN101712556B/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102503392A (en) * | 2011-10-21 | 2012-06-20 | 武汉理工大学 | Single-phase multi-ferreous strontium-ferrite ceramic material and preparation method thereof |
| CN102503392B (en) * | 2011-10-21 | 2013-10-02 | 武汉理工大学 | Single-phase multi-ferreous strontium-ferrite ceramic material and preparation method thereof |
| CN104230325A (en) * | 2013-06-24 | 2014-12-24 | 广东江粉磁材股份有限公司 | Preparation method of permanent magnetic ferrite pre-sintering material and preparation method of permanent magnetic ferrite |
| CN104230326A (en) * | 2013-06-24 | 2014-12-24 | 广东江粉磁材股份有限公司 | Preparation method of M-type calcium permanent magnetic ferrite |
| CN104230326B (en) * | 2013-06-24 | 2016-02-10 | 广东江粉磁材股份有限公司 | The preparation method of M type calcium permanent ferrite |
| CN103408296A (en) * | 2013-08-15 | 2013-11-27 | 上海应用技术学院 | Characterization analysis method for migration of lanthanum and cobalt ions in lanthanum-cobalt substituted strontium ferrite permanent magnet material |
| CN103408296B (en) * | 2013-08-15 | 2014-10-29 | 上海应用技术学院 | Characterization analysis method for migration of lanthanum and cobalt ions in lanthanum-cobalt substituted strontium ferrite permanent magnet material |
| CN105292990A (en) * | 2015-12-09 | 2016-02-03 | 攀枝花钢城集团有限公司 | Strontium ferrite pre-sintering ball material cooling and storing system and process |
| CN105565793A (en) * | 2015-12-29 | 2016-05-11 | 海安南京大学高新技术研究院 | Method for molten salt assisted sintering of strontium ferrite |
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