CN103204676A - Method for microwave-assisted low-temperature rapid synthesis of ferrite ultrafine powder - Google Patents
Method for microwave-assisted low-temperature rapid synthesis of ferrite ultrafine powder Download PDFInfo
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- CN103204676A CN103204676A CN2013101429753A CN201310142975A CN103204676A CN 103204676 A CN103204676 A CN 103204676A CN 2013101429753 A CN2013101429753 A CN 2013101429753A CN 201310142975 A CN201310142975 A CN 201310142975A CN 103204676 A CN103204676 A CN 103204676A
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Abstract
The invention discloses a method for microwave-assisted low-temperature rapid synthesis of ferrite ultrafine powder. The method comprises the steps of respectively weighing metallic oxide of Me, ZnO and Fe2O3 depending on chemical dosage of ferrite Me(1-x)ZnxFe2O4, mixing and wet-ball milling, drying and filtering by a 100-mesh sieve to obtain a mixture; and adding the mixture in a microwave reaction furnace, carrying out microwave-assisted solid synthesis for 10-30min in an air atmosphere at 600-950 DEG C, and cooling to obtain the ferrite ultrafine powder, wherein the Me is Ni, Mn or Co, and x is not greater than 1.0 and not less than 0. The process for microwave-assisted low-temperature rapid synthesis of the ferrite ultrafine powder is simple, high in temperature raising speed, short in heat preservation duration, low in synthesis temperature and excellent in performance, and is capable of effectively reducing production cost and energy consumption, and improving the production efficiency. And the method is applicable to mass production.
Description
One, technical field
The present invention relates to a kind of preparation method of magneticsubstance, specifically the method for the quick synthesizing of ferrite micro mist of a kind of microwave-assisted low temperature.
Two, background technology
Characteristics such as ferrite magnetic material has that resistivity height, loss are little, dielectric properties and frequency response characteristic are good are the important magnetic functional materials of a class, all have in fields such as modern communication, military affairs, electronics, information, chemical industry, biology, medical science widely and use.At present, industrial production mainly adopts the metal oxide solid reaction process to prepare with ferrite powder, and its technology is simple, prescription is accurate, is easy to large-scale commercial production.But traditional solid reaction process synthesizing of ferrite powder, its solid state reaction temperature height (thousands of degree) (Liu Shuxin, China's powder technology, 2011,17(1): 29), synthesis cycle long (a few hours), each component High temperature diffusion and speed of response differ, cause synthesizing of ferrite material material solute segregation, thereby worsen the electromagnetic property of Ferrite Material, and production cost is higher, energy consumption is bigger, therefore must manage to reduce its synthesis temperature and time, improves microtexture, composition homogeneity and the performance of ferrite micropowder.
In recent years, for character and the electromagnetic performance that improves ferrite powder, adopt synthesizing of ferrite powders such as low-heat solid state reaction method, self propagating high temperature synthesis method, Hydrothermal Preparation, sol-gel method, coprecipitation method.Though these methods can overcome the defective of high temperature solid-state synthesizing of ferrite powder effectively, obtain ultra-fine ultrapure ferrite powder under the low temperature, but shortcomings such as these method ubiquity processing steps are many, synthesis cycle is relatively grown, yield poorly, cost height are unfavorable for large-scale industrial production.
Three, summary of the invention
The present invention is for fear of above-mentioned the deficiencies in the prior art part, and the method for the quick synthesizing of ferrite micro mist of a kind of microwave-assisted low temperature is provided.Technical problem to be solved by this invention is to reduce the temperature of metal oxide solid state reaction synthesizing of ferrite micro mist, shortening generated time, makes preparation process be easy to suitability for industrialized production, improves the electromagnetic performance of ferrite micropowder simultaneously.
Technical solution problem of the present invention adopts following technical scheme:
The method of the quick synthesizing of ferrite micro mist of microwave-assisted low temperature of the present invention, difference with the prior art is:
According to ferrite Me
(1-x)Zn
xFe
2O
4Stoichiometric ratio take by weighing metal oxide, ZnO and the Fe of Me respectively
2O
3Each raw material, each raw material is analytical pure, mixes the back wet ball mill, and wet ball mill medium (being solvent) is dehydrated alcohol, 5 hours wet ball mill time, ball material mass ratio (5～10): 1, dry back is crossed 100 mesh sieves and is obtained compound; With described compound place the microwave reaction stove at air atmosphere in 600-950 ℃ of microwave-assisted solid phase synthesis 10-30 minute, microwave frequency is 2.45GHz, temperature rise rate is 20-40 ℃/min, namely gets ferrite micropowder after the cooling;
Described Me is Ni, Mn or Co, 0≤x≤1.0.
The metal oxide of described Me is selected from NiO, Mn
2O
3Or Co
2O
3
The metal oxide of described Me, ZnO and Fe
2O
3Particle diameter be 10-30 μ m.
Microwave-assisted is synthetic to be a kind of technology with high energy efficiency ratio, because its fast rate of heating and unique heating mechanism, is conducive to promote under the low temperature nucleation and growth speed of material, and the powder of obtained performance excellence just is being subjected to people and is more and more paying close attention to.Especially for the raw iron oxide material that has good electromagnetic absorption performance in the prescription etc., can improve problems such as synthesis temperature height, powder nucleation inequality, solute segregation in traditional solid phase synthesis ferrite powder process, the quick synthesized high-performance ferrite micropowder of low temperature.
Compare with technology with the preparation technology of traditional solid phase pyroreaction synthesizing of ferrite micro mist, advantage applies of the present invention exists: preparation technology is simple, reduces its synthesis temperature effectively; shorten the production cycle; reduce production costs and energy consumption, enhance productivity, be suitable for large-scale production.Simultaneously, the crystal grain of the quick synthesizing of ferrite micro mist of microwave-assisted low temperature is tiny, component is even, and the sintering activity height has excellent performance.
Four, description of drawings
Fig. 1 is for adopting traditional solid state reaction and microwave-assisted low temperature synthetic Ni fast
0.5Zn
0.5Fe
2O
4(CS: traditional solid state reaction is synthetic for the XRD figure spectrum of ferrite micropowder; MS: the microwave-assisted solid phase synthesis).As can be seen from Figure 1,600 ℃ of synthetic 30min of microwave-assisted can obtain pure Ni
0.5Zn
0.5Fe
2O
4Ferrite micropowder; And adopt 900 ℃ of calcinings of traditional solid reaction process 120min, also exist in the sample and fully do not react dephasign (NiO, Fe as yet
2O
3).
Fig. 2 is the synthetic 30min Ni of 680 ℃ of microwave-assisted
0.5Zn
0.5Fe
2O
4The FESEM photo of ferrite micropowder.As can be seen from Figure 2, microwave-assisted synthetic sample particle diameter is～1.0 μ m.
Fig. 3 is the synthetic 30min Ni of 680 ℃ of microwave-assisted
0.5Zn
0.5Fe
2O
4The magnetic hysteresis loop of ferrite micropowder.As can be seen from Figure 3, the microwave-assisted synthetic sample demonstrates typical soft magnetic property, its saturation magnetization Ms and coercive force H
cBe respectively 70.4Am
2Kg
-1, 2.5kAm
-1
Five, embodiment
Following embodiment further specifies the present invention, but embodiment can not be construed as limiting the invention.In the technical solution of the present invention cited to spinel type, carbuncle type and three types of Ferrite Materials of Magnetoplumbate-type can both realize the present invention, and the bound value of spinel type, carbuncle type and three types of Ferrite Material different componentss of Magnetoplumbate-type can both realize the present invention; Be that example is enumerated the embodiment of the invention with spinel type Ni-Zn Ferrite Material only at this.
Embodiment 1:
According to Ni
0.5Zn
0.5Fe
2O
4Ferritic stoichiometric ratio takes by weighing analytical pure metal oxide NiO3.479g, ZnO3.423g and Fe respectively
2O
313.433g, in the stainless steel jar mill of packing into, be solvent with the dehydrated alcohol, wet ball mill 5 hours, ratio of grinding media to material is 6:1, the slurry that ball milling is obtained is crossed 100 mesh sieves after drying and is got compound.With the compound alumina-ceramic crucible of packing into, and cover with the auxilliary backing of SiC, be incubated 30min after placing microwave agglomerating furnace to be warming up to 680 ℃ with the temperature rise rate of 20 ℃/min then, microwave frequency is 2.45GHz, namely gets ferrite micropowder after the cooling.
Embodiment 2:
Present embodiment is the contrast experiment of embodiment 1.
Take by weighing analytical pure metal oxide NiO, ZnO and Fe respectively
2O
3Each is 3.479,3.423 and 13.433g years old.Raw material is packed in the stainless steel jar mill, is solvent with the dehydrated alcohol, wet ball mill 5 hours, and ratio of grinding media to material is 6:1, the slurry that ball milling is obtained is crossed 100 mesh sieves after drying and is got compound.With the ball milling compound alumina-ceramic crucible of packing into, place the box-type furnace sintering oven then, be incubated 120min after being warming up to 900 ℃ with the temperature rise rate of 10 ℃/min, namely get ferrite micropowder after the cooling.
Fig. 1 adopts traditional solid state reaction and microwave-assisted solid phase synthesis Ni
0.5Zn
0.5Fe
2O
4The XRD figure spectrum of ferrite micropowder.As can be seen from Figure 1, embodiment 1 adopts the microwave-assisted low temperature synthetic Ni that obtains fast
0.5Zn
0.5Fe
2O
4Ferrite micropowder.
Fig. 2 is 680 ℃ of microwave-assisted solid phase synthesis 30min Ni
0.5Zn
0.5Fe
2O
4The FESEM photo of ferrite micropowder, sample particle diameter are～1.0 μ m.
Adopt U.S. Lakeshore7307-9309 vibrating sample magnetometer to measure microwave-assisted solid phase synthesis Ni
0.5Zn
0.5Fe
2O
4The agnetic property at room temperature m of ferrite micropowder.Fig. 3 is the magnetic hysteresis loop of sample, its saturation magnetization Ms and coercive force H
cBe respectively 70.4Am
2Kg
-1, 2.5kAm
-1
Embodiment 3:
According to Ni
0.7Zn
0.3Fe
2O
4Ferritic stoichiometric ratio takes by weighing analytical pure metal oxide NiO4.871g, ZnO0.104g and Fe respectively
2O
313.51g, in the stainless steel jar mill of packing into, be solvent with the dehydrated alcohol, wet ball mill 5 hours, ratio of grinding media to material is 6:1, the slurry that ball milling is obtained is crossed 100 mesh sieves after drying and is got compound.With the compound alumina-ceramic crucible of packing into, and cover with the auxilliary backing of SiC, be incubated 20min after placing microwave agglomerating furnace to be warming up to 950 ℃ with the temperature rise rate of 30 ℃/min then, microwave frequency is 2.45GHz, namely gets ferrite micropowder after the cooling.
Embodiment 4:
According to Ni
0.3Zn
0.7Fe
2O
4Ferritic stoichiometric ratio takes by weighing analytical pure metal oxide NiO3.459g, ZnO3.403g and Fe respectively
2O
313.359g, in the stainless steel jar mill of packing into, be solvent with the dehydrated alcohol, wet ball mill 5 hours, ratio of grinding media to material is 6:1, the slurry that ball milling is obtained is crossed 100 mesh sieves after drying and is got compound.With the compound alumina-ceramic crucible of packing into, and cover with the auxilliary backing of SiC, be incubated 30min after placing microwave agglomerating furnace to be warming up to 900 ℃ with the temperature rise rate of 20 ℃/min then, microwave frequency is 2.45GHz, namely gets ferrite micropowder after the cooling.
Claims (6)
1. the method for the quick synthesizing of ferrite micro mist of microwave-assisted low temperature is characterized in that:
According to ferrite Me
(1-x)Zn
xFe
2O
4Stoichiometric ratio take by weighing metal oxide, ZnO and the Fe of Me respectively
2O
3, mix the back wet ball mill, dry back is crossed 100 mesh sieves and is obtained compound; With described compound place the microwave reaction stove at air atmosphere in 600-950 ℃ of microwave-assisted solid phase synthesis 10-30 minute, namely get ferrite micropowder after the cooling;
Described Me is Ni, Mn or Co, 0≤x≤1.0.
2. synthetic method according to claim 1 is characterized in that:
The metal oxide of described Me is selected from NiO, Mn
2O
3Or Co
2O
3
3. synthetic method according to claim 1 and 2 is characterized in that:
The metal oxide of described Me, ZnO and Fe
2O
3Particle diameter be 10-30 μ m.
4. synthetic method according to claim 1 is characterized in that:
The solvent of described wet ball mill is dehydrated alcohol, 5 hours wet ball mill time, ball material mass ratio (5～10): 1.
5. synthetic method according to claim 1 is characterized in that:
Microwave frequency is 2.45GHz in the microwave-assisted solid phase synthesis.
6. synthetic method according to claim 1 or 5 is characterized in that:
Temperature rise rate is 20-40 ℃/min in the microwave-assisted solid phase synthesis.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105048020A (en) * | 2015-06-12 | 2015-11-11 | 安徽理工大学 | Method for preparing lithium-doped cobalt ferrite material by employing waste lithium battery as raw material |
| CN107790193A (en) * | 2017-10-30 | 2018-03-13 | 贵州理工学院 | A kind of high frequency magnetic field auxiliary ball-milling preparation method of sewage disposal catalyst |
| CN110772911A (en) * | 2018-07-30 | 2020-02-11 | 天津大学 | Microwave reaction device and reaction system for removing bioaerosol and application thereof |
| CN113862719A (en) * | 2021-11-05 | 2021-12-31 | 上海交通大学 | Transition metal oxide catalyst and preparation method and application thereof |
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| CN101913850A (en) * | 2010-07-06 | 2010-12-15 | 电子科技大学 | Preparation method of high-magnetic-conductivity low-temperature-sintering Z-shaped hexagonal ferrite material |
| CN102584198A (en) * | 2012-02-24 | 2012-07-18 | 湖南阳东微波科技有限公司 | Method for pre-sintering soft magnetic manganese-zinc high-permeability powder in microwave kiln and preparation method of soft magnetic manganese-zinc high-permeability powder |
| CN103011793A (en) * | 2012-12-27 | 2013-04-03 | 中南大学 | Method for preparing nickel-zinc ferrite by using microwave technology |
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2013
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Patent Citations (3)
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| CN101913850A (en) * | 2010-07-06 | 2010-12-15 | 电子科技大学 | Preparation method of high-magnetic-conductivity low-temperature-sintering Z-shaped hexagonal ferrite material |
| CN102584198A (en) * | 2012-02-24 | 2012-07-18 | 湖南阳东微波科技有限公司 | Method for pre-sintering soft magnetic manganese-zinc high-permeability powder in microwave kiln and preparation method of soft magnetic manganese-zinc high-permeability powder |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105048020A (en) * | 2015-06-12 | 2015-11-11 | 安徽理工大学 | Method for preparing lithium-doped cobalt ferrite material by employing waste lithium battery as raw material |
| CN107790193A (en) * | 2017-10-30 | 2018-03-13 | 贵州理工学院 | A kind of high frequency magnetic field auxiliary ball-milling preparation method of sewage disposal catalyst |
| CN107790193B (en) * | 2017-10-30 | 2020-07-14 | 贵州理工学院 | High-frequency magnetic field assisted ball milling preparation method of catalyst for sewage treatment |
| CN110772911A (en) * | 2018-07-30 | 2020-02-11 | 天津大学 | Microwave reaction device and reaction system for removing bioaerosol and application thereof |
| CN110772911B (en) * | 2018-07-30 | 2021-11-09 | 天津大学 | Microwave reaction device and reaction system for removing bioaerosol and application thereof |
| CN113862719A (en) * | 2021-11-05 | 2021-12-31 | 上海交通大学 | Transition metal oxide catalyst and preparation method and application thereof |
| CN113862719B (en) * | 2021-11-05 | 2023-07-11 | 上海交通大学 | Transition metal oxide catalyst and preparation method and application thereof |
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Application publication date: 20130717 |