CN1848316A - Method for interal supplying oxygen self-spreading high-temperature synthetizing MnZn ferrite - Google Patents
Method for interal supplying oxygen self-spreading high-temperature synthetizing MnZn ferrite Download PDFInfo
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- CN1848316A CN1848316A CN 200610011648 CN200610011648A CN1848316A CN 1848316 A CN1848316 A CN 1848316A CN 200610011648 CN200610011648 CN 200610011648 CN 200610011648 A CN200610011648 A CN 200610011648A CN 1848316 A CN1848316 A CN 1848316A
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Abstract
The present invention provides a method for preparing manganese-zinc ferrite by utilizing internal oxidation self-spreading high-temperature synthesis process. Said method includes the following steps: according to mixing ratio of Mn0.5 Zn 0.5 Fe2O4 mixing raw materials of MnO2 (Mn3O4), ZnO, Fe2O3 and Fe powder, adding different internal oxygen-supplying agents of NH4No3, KCLO3 and KMnO4, uniformly mixing them, low-temperature drying, placing them into a refractory boat protected by graphite, adding tungsten wire coil, powering on, lighting powder, placing synthetic powder in a ball-grinding tank, wet-grinding to remove residual substances from ferrite, grinding synthetic manganese-zinc ferrite powder, water-washing and drying so as to obtain the invented product.
Description
Technical field
The invention belongs to the self propagating high temperature synthesis technical field, particularly a kind of method of interal supplying oxygen self-spreading high-temperature synthetizing MnZn ferrite
Background technology
The magnetic permeability of manganese-zinc ferrite is higher, and is low at the low-frequency range internal loss, also is best a kind of of present high magnetic permeability.The main method of preparation manganese-zinc ferrite is divided into wet method and dry method at present, and the main distinction of its preparation is the difference of ferrite pioneer powder preparing, and in general, wet method has coprecipitation, hydro thermal method, Sol-Gel; Dry method has the ceramic process method, the SHS high-temperature synthesis.The self propagating high temperature synthesizing of ferrite saves time, energy-conservation, the temperature height that burning is synthetic can purify the impurity of being brought into by raw material and oxygenate, and at the synthetic back of high temperature air Li temper fire, keeps a large amount of high temperature information, has sintering activity preferably.The method of self propagating high temperature synthesizing of ferrite powder has mainly adopted iron replacement partial oxidation iron at present, enclose middle synthetic powder (seeing Chinese publication number CN1328329A) in hyperbaric oxygen atmosphere, but this method is limited to high-tension apparatus, limited efficiency.
Summary of the invention
The object of the invention is to provide a kind of method of interal supplying oxygen self-spreading high-temperature synthetizing MnZn ferrite, has avoided the use high-pressure bottle, has solved in the course of reaction problem of high-velocity combustion oxygen interal supplying oxygen deficiency.
The present invention is by adding different oxygenates, makes in quick high-temp synthesizing of ferrite process by interal supplying oxygen, and enough heat and atmospheres are provided.Concrete steps are as follows:
A, with raw material MnO
2(Mn
3O
4), ZnO (Zn (NO
3)
2), Fe
2O
3, Fe powder Mn in proportion
0.5Zn
0.5Fe
2O
4, Fe: Fe wherein
2O
3=1: 1 (mol ratio), wet-milling mixes 1～2h, and ball, material were than 3: 1 (mass ratio).Ingredient requirement sees attached list 1
Subordinate list 1: raw meal requirement
| Component | Average grain diameter/μ m | Purity % |
| MnO 2(Mn 3O 4) | ≤1 | ≥98 |
| ZnO(Zn(NO 3) 2) | ≤1 | ≥98 |
| Fe 2O 3 | ≤1 | ≥98 |
| Fe | ≤30 | ≥97 |
B, the different interal supplying oxygen agent of adding mix, and oxidant is NH
4NO
3, KClO
3, KMnO
4, addition is a powder dry weight 10%～30%, is formulated as saturated solution, and after mixing, low temperature drying is placed on the fire-resistant boat of graphite protection, inserts tungsten filament coil, and powder is lighted in energising in the air;
C, synthetic powder is placed ball grinder wet-milling 60～120min, use the washed with de-ionized water ferrite powder then, remove the surplus materials that remains in the ferrite.The oven dry after grinding washing of synthetic manganese-zinc ferrite powder.
Advantage of the present invention is as follows:
It is synthetic in the air atmosphere burning to have solved synthesizing of ferrite, and safety saves time, and saves complicated high-tension apparatus or supercharging equipment, has realized that common container is the technology approach of incendivity synthesizing of ferrite.For adopting NH
4NO
3Be the combustion synthesis reaction of oxidant, do not introduce impurity and can omit water-washing process that technology is more simple.And for KMnO
4, the internal solids oxygen supply not only being provided but also can becoming the source of manganese-zinc ferrite manganese, production cost is relatively low.And for KClO
3, at reaction oxygenate MnO
2Under the catalysis, the accelerated combustion aggregate velocity can further improve efficient.By secondary ball milling and washing, can further remove soluble impurity in the ferrite, obtain comparatively pure ferrite.
Description of drawings
Fig. 1 is the XRD figure of the embodiment of the invention 1
Fig. 2 is the XRD figure of the embodiment of the invention 2
Fig. 3 is an XRD figure of the present invention
Fig. 4 is magnetization curve figure of the present invention.
Embodiment:
Embodiment 1:
With raw material MnO proportionally
2: Zn (NO
3)
2: Fe: Fe
2O
3=0.5: 0.5: 1: 0.5, wet-milling mixed 1～2h, and ratio of grinding media to material 3: 1 (mass ratio) adds NH
4NO
3Amount is 30% of raw material weight, mixes to put into drying box and insert crystal vessel light powder after 60～80 ℃ of low temperature dryings, and the dry preparation of ball milling removes manganese-zinc ferrite powder then.The synthetic temperature of high combustion is 1130 ℃, burning aggregate velocity 1.22mm/s, and the ferrite degree is 77.7%.(synthetic manganese-zinc ferrite XRD sees accompanying drawing 1).
Embodiment 2
With raw material Mn proportionally
3O
4: ZnO: Fe: Fe
2O
3=0.25: 0.5: 1: 0.5, wet-milling mixed 1～2h, and ratio of grinding media to material 3: 1 (mass ratio) adds KMnO
4Amount is 20% of raw material, mixes to put into drying box and insert crystal vessel light powder after 60～80 ℃ of low temperature dryings, and ball milling after washing drying is prepared manganese-zinc ferrite powder then.The synthetic temperature of high combustion is 1256 ℃, and burning aggregate velocity is 1.45mm/s, and the ferrite degree is 94.5% (the manganese-zinc ferrite XRD that synthesizes sees accompanying drawing 2)
Embodiment 3
With raw material MnO proportionally
2: ZnO: Fe: Fe
2O
3=0.5: 0.5: 1.2: 0.4, wet-milling mixed 1～2h, and ratio of grinding media to material 3: 1 (mass ratio) adds KClO
3Amount is 10% of raw material, mixes to put into drying box and insert crystal vessel light powder after 60～80 ℃ of low temperature dryings, and the dry preparation of ball milling after washing removes manganese-zinc ferrite powder then.High combustion synthesis temperature is 1332 ℃, burning aggregate velocity 1.85mm/s, and the ferrite degree is 99.5% (synthetic manganese-zinc ferrite XRD sees accompanying drawing 3).It is 1.12 μ m that this ferrite powder particle diameter is measured average grain diameter through laser particle size.Its saturation magnetization is 64.44Am
2Kg
-1, coercive force is 0.4kAm
-1, remanent magnetism is 1.349Am
2Kg
-1(magnetization curve such as accompanying drawing 4).
Claims (2)
1, a kind of interal supplying oxygen, the method for the synthetic manganese-zinc ferrite of self-propagating high-temperature is characterized in that:
A, with raw material MnO
2(Mn
3O
4), ZnO (Zn (NO
3)
2, Fe
2O
3, Fe powder Mn in proportion
0.5Zn
0.5Fe
2O
4Batching, wherein Fe: Fe
2O
3=1: 1 mol ratio, wet-milling mixes 1～2h, ball, material mass ratio 3: 1;
B, the different interal supplying oxygen agent NH of adding
4NO
3, KClO
3, KMnO
4, addition is a powder dry weight 10%～30%, is formulated as saturated solution, and after mixing, low temperature drying is placed on the fire-resistant boat of graphite protection, inserts tungsten filament coil, and powder is lighted in energising in the air;
C, synthetic powder is placed ball grinder wet-milling 60～120min, use the washed with de-ionized water ferrite powder then, remove the surplus materials that remains in the ferrite, synthetic manganese-zinc ferrite powder is through grinding the oven dry of washing back.
2, method according to claim 1 is characterized in that: the average grain diameter of raw material: MnO
2(Mn
3O
4)≤1 μ m, ZnO (Zn (NO
3)
2)≤1 μ m, Fe
2O
3≤ 1 μ m, Fe≤30 μ m; The purity of raw material: MnO
2(Mn
3O
4) 〉=98%, ZnO (Zn (NO
3)
2) 〉=98%, Fe
2O
3〉=98%, Fe 〉=97%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006100116484A CN1848316B (en) | 2006-04-12 | 2006-04-12 | Method for interal supplying oxygen self-spreading high-temperature synthetizing MnZn ferrite |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006100116484A CN1848316B (en) | 2006-04-12 | 2006-04-12 | Method for interal supplying oxygen self-spreading high-temperature synthetizing MnZn ferrite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1848316A true CN1848316A (en) | 2006-10-18 |
| CN1848316B CN1848316B (en) | 2010-06-23 |
Family
ID=37077827
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|---|---|---|---|
| CN2006100116484A Expired - Fee Related CN1848316B (en) | 2006-04-12 | 2006-04-12 | Method for interal supplying oxygen self-spreading high-temperature synthetizing MnZn ferrite |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101376590B (en) * | 2008-10-13 | 2012-06-27 | 北京科技大学 | Method for preparing manganese-zinc ferrite powder by self-propagating high temperature synthesis |
| CN106316378A (en) * | 2015-06-30 | 2017-01-11 | 中国人民解放军军械工程学院 | Y type barium ferrite hollow ceramic microsphere wave-absorbing material |
| CN106316379A (en) * | 2015-06-30 | 2017-01-11 | 中国人民解放军军械工程学院 | W type barium ferrite hollow ceramic microsphere wave-absorbing material |
| CN110511016A (en) * | 2019-08-26 | 2019-11-29 | 严华军 | A kind of production technology of manganese-zinc ferrite magnetic material |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1182549C (en) * | 2002-09-13 | 2004-12-29 | 无锡晶石磁性电子器件有限公司 | Magnanese-zinc ferrite magnetic core |
-
2006
- 2006-04-12 CN CN2006100116484A patent/CN1848316B/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101376590B (en) * | 2008-10-13 | 2012-06-27 | 北京科技大学 | Method for preparing manganese-zinc ferrite powder by self-propagating high temperature synthesis |
| CN106316378A (en) * | 2015-06-30 | 2017-01-11 | 中国人民解放军军械工程学院 | Y type barium ferrite hollow ceramic microsphere wave-absorbing material |
| CN106316379A (en) * | 2015-06-30 | 2017-01-11 | 中国人民解放军军械工程学院 | W type barium ferrite hollow ceramic microsphere wave-absorbing material |
| CN110511016A (en) * | 2019-08-26 | 2019-11-29 | 严华军 | A kind of production technology of manganese-zinc ferrite magnetic material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1848316B (en) | 2010-06-23 |
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Inventor after: Gao Xuexu Inventor after: Yang Ke Inventor after: Sui Yanli Inventor before: Guo Zhimeng Inventor before: Yang Ke Inventor before: Sui Yanli |
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Free format text: CORRECT: INVENTOR; FROM: GUO ZHIMENG YANG KE SUI YANLI TO: GAO XUEXU YANG KE SUI YANLI |
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Granted publication date: 20100623 Termination date: 20130412 |