CN103755336B - Preparation method of nanometer ferrite particles - Google Patents
Preparation method of nanometer ferrite particles Download PDFInfo
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Abstract
The invention discloses a preparation method of nanometer ferrite particles. On the basis of the existing sol-gel technique, the method adopts an organic template to absorb sol to overcome the defects that segregation of microelements is easily generated during the drying process of common sol, so that the impurity phase is produced in the final product. The cracking and carbonizing of phenolic resin which is wrapped on the non-shaped ferrite particle surface and the crystal form conversion of the ferrite are simultaneously carried out, so the agglomeration and growth of the ferrite particles in the calcination process are prevented, and the nanometer ferrite particles with uniform particle size, large specific area and good magnetic performance can be obtained. The method has the advantages that the defects of multiple impurity phases, difficult control of particle size, poor magnetic performance and smaller specific area of the solid phase method are overcome, and the defects of easy agglomeration, nonuniform particle size and the like of the chemical precipitation method are also overcome.
Description
Technical field
The invention belongs to technical field of inorganic nonmetallic materials, be specifically related to a kind of preparation method of Nano-Ferrite Particle.
Background technology
Nano material refers to have small-size effect, surface effects, quantum size effect and macro quanta tunnel effect etc. by the material that characteristic dimension forms in the nano sized particles of nano level (being often referred to 1-100nm).Ferrite is the widely used nonmetal magnetic material of a class.Nano-Ferrite Particle not only has specific physical and the chemical property of nano material imparting, also there is special magnetic property, the material of the variforms such as nanometer magnetic film, nanometer magnet-wire, nano-magnetic powder and magnetic fluid can be made, have a wide range of applications in traditional industries and high-technology field such as high voltage power transmission and transforming, communication, biomedicine, national defence etc.The purity of Nano-Ferrite Particle, specific surface area and magnetic property be its be widely used in magnetic recording media, magnetic fluid, absorbing material and in medical applications as the key of magnetic target pharmaceutical carrier, cellular segregation and magnetic control contrast medium etc.
Nanometer ferrite raw powder's production technology directly determines the performance of nanometer ferrite.The preparation method of current nanometer ferrite is a lot, mainly contains: solid phase method, chemical coprecipitation, hydrothermal synthesis method and colloidal sol is solidifying-glue method etc.Wherein, solid phase method output is high, and technique is simple, is the main method of suitability for industrialized production ferrite particle, but exist particle size comparatively large and uneven, easily produce the shortcomings such as impurity, beads magnetic energy and specific surface area are lower.Chemical coprecipitation due to its technique simple, not high to equipment, technical requirements, the advantages such as products therefrom purity is higher, particle size is less, are widely used in recent years and prepare Nano-Ferrite Particle.But the standby magnetic-particle size distribution of this legal system is wider, reunite serious, magnetic property is lower.Hydrothermal synthesis method gained Nano-Ferrite Particle have better crystallinity degree, particle diameter little, reunite low, without the need to advantages such as pyroprocessing, but high to equipment requirements, the higher and more difficult batch production of cost.Nano-Ferrite Particle purity prepared by sol-gel method is higher, and chemical constitution is evenly accurate.But dispersed for improving, usually add tensio-active agent, adopt the methods such as supercritical drying.Thus there is cost higher, the shortcomings such as operational difficulty.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art, provides a kind of preparation method of Nano-Ferrite Particle.
In order to achieve the above object, technical scheme provided by the invention is:
The preparation method of described Nano-Ferrite Particle comprises the steps:
(1) hybrid metal nitrate is dissolved in dehydrated alcohol, is mixed with hybrid metal nitrate-ethanolic soln; Citric acid is dissolved in dehydrated alcohol, is mixed with citric acid-ethanolic soln; Hybrid metal nitrate-ethanolic soln is mixed with the volume ratio of citric acid-ethanolic soln by 1:1, obtained hybrid metal nitrate-citric acid ethanolic soln; Wherein, described hybrid metal nitrate is Fe (NO
3)
39H
2the mixture that the transition metal nitrate that O is different from one or both mixes according to the molar ratio forming spinel type ferrite, consisting of of described spinel type ferrite: M
xn
1-xfe
2o
4, M and N represents the transition-metal cation that different metal nitrates provides, 0≤x≤1; The add-on that described hybrid metal nitrate is dissolved in hybrid metal in dehydrated alcohol is: every 10g hybrid metal nitrate is dissolved in 50-300mL dehydrated alcohol; The add-on that described citric acid is dissolved in citric acid in dehydrated alcohol is: every 10g citric acid is dissolved in 50-300mL dehydrated alcohol;
(2) regulate the pH value of hybrid metal nitrate-citric acid ethanolic soln to be 0.5-6 with ammoniacal liquor, be preferably 1-4, this solution concentrated obtains the colloidal sol that viscosity is 0.005-0.03Pas;
(3) in colloidal sol, add absorbent cotton, after colloidal sol adsorbs by absorbent cotton completely, absorbent cotton is dried, obtains xerogel-absorbent cotton;
(4) by xerogel-absorbent cotton in oxidizing atmosphere, temperature≤600 DEG C, are preferably insulation 0.5-6h under DEG C condition of temperature≤500, are preferably 2-4h, obtain amorphous iron ferrite powder;
(5) cross 600-900 mesh sieves by after the grinding of amorphous iron ferrite powder, obtain the amorphous iron ferrite powder after grinding; Add in dehydrated alcohol by the amorphous iron ferrite powder after grinding, ultrasonic disperse (general supersound process 1-3h) is obtained ferrite particle-alcohol suspension afterwards; In ferrite particle-alcohol suspension, add resol, stir under 40-80 DEG C of conditions, after ethanol evaporation and phenolic resin curing, obtain the amorphous Nano-Ferrite Particle that resol is coated; Wherein, the add-on that the amorphous iron ferrite powder after described grinding adds amorphous iron ferrite powder in dehydrated alcohol is: the amorphous iron ferrite powder after every 1g grinding adds 30-350mL, is preferably in 50-300mL dehydrated alcohol; The add-on that described resol adds resol in ferrite particle-alcohol suspension is: add 5-140mL in every 100mL ferrite particle-alcohol suspension, be preferably 10-120mL resol;
(6) amorphous Nano-Ferrite Particle coated for resol is carbonized in inert atmosphere, carbonization temperature is 500-1100 DEG C, and be preferably 600-1000 DEG C, carbonization time is 0.5-6h, be preferably 1-4h, obtain the nanometer spinel type ferrite particle that charcoal is coated;
(7) cross 600-900 mesh sieves by after nanometer spinel type ferrite particulate abrasive coated for charcoal, obtain the Nano-Ferrite Particle after grinding; After Nano-Ferrite Particle after grinding is carried out carbon removal process in acid, obtain Nano-Ferrite Particle.
In addition, step (1) described transition metal is copper, nickel, cobalt or zinc etc.
Ammonia concn described in step (2) is 1-12mol/L, is preferably 2-10mol/L.
The add-on of step (3) described absorbent cotton is: add 1-10g in every 100mL colloidal sol, be preferably 2-8g absorbent cotton; After colloidal sol adsorbs by absorbent cotton completely, absorbent cotton is dried under 60-100 DEG C of conditions.
Oxidizing atmosphere described in step (4) refers to air atmosphere.
Inert atmosphere described in step (6) is nitrogen atmosphere or argon atmospher.
Acid described in step (7) is concentration of volume percent is 40-100%, the preferably perchloric acid of 60-100%, and the temperature of carbon removal process is 40-100 DEG C, preferably 50-90 DEG C.
The present invention, on the basis of existing sol-gel technique, prepares high purity by organic formwork absorption-charcoal covered composite yarn technique, high-ratio surface sum high magnetic characteristics Nano-Ferrite Particle.Organic formwork absorption overcomes the microcomponent segregation easily occurred in conventional sol drying process, occurs the shortcoming of a small amount of impurity phase in the finished product; Synchronously carrying out of the Phenolic resin pyrolysis Carbonization being coated on amorphous iron oxysome particle surface and ferrite crystal conversion, the reunion of ferrite particle in calcination process is prevented to grow up, be conducive to obtaining uniform particle sizes, specific surface area is high, the Nano-Ferrite Particle of magnetic property excellence.
It is more that preparation method of the present invention overcomes the impurity phase that solid phase method easily occurs, size controlling difficulty, magnetic property and the less deficiency of specific surface area, also overcomes the particle that chemical precipitation method exists and easily reunite, the shortcomings such as granularity is uneven.The advantages such as the nano magnetic particle prepared by present method has that purity is high, uniform particle sizes, and the large and magnetic property of specific surface area is excellent, and abundant raw material source, cheap, technique is simply, low for equipment requirements, is easy to mass production.The Nano-Ferrite Particle adopting present method to prepare is expected to obtain in high-end fields such as high-density magnetic storage, photomagnetism, magnetic fluid, magnetic electric compound material, catalyzer to apply widely.
Accompanying drawing explanation
Fig. 1 is the TEM figure of gained Nano-Ferrite Particle in embodiment 1;
Fig. 2 is the magnetic hysteresis loop of gained Nano-Ferrite Particle in embodiment 1; Wherein, X-coordinate is magneticstrength H, and ordinate zou is magnetic induction density B.
Embodiment
Embodiment 1
Described Nano-Ferrite Particle CoFe
2o
4preparation method comprise the steps:
(1) by 30.9947g Fe (NO
3)
39H
2o and 11.1638g Co (NO
3)
26H
2o is dissolved in 300ml dehydrated alcohol, prepares hybrid metal nitrate-ethanolic soln; 24.1828g citric acid is dissolved in 300ml ethanol, prepares citric acid-ethanolic soln.With vigorous stirring, under agitation added by citric acid-ethanolic soln in hybrid metal nitrate-ethanolic soln, Keep agitation 4h, prepares the ethanolic soln of hybrid metal nitrate-citric acid;
(2) under agitation, with the NH of 8mol/L
3h
2the pH value of O regulating step (1) gained solution is to 3.5, and then this solution concentrated forms the colloidal sol with certain viscosity, should be positioned at about 0.025Pas under the viscosity room temperature of gained colloidal sol;
(3) in step (2) gained colloidal sol, add about 20g absorbent cotton to adsorb this colloidal sol, after waiting absorbent cotton to be adsorbed by colloidal sol completely, move into 80 DEG C of oven dry in baking oven and, to constant weight, obtain xerogel-absorbent cotton;
(4) step (3) gained xerogel-absorbent cotton is put into box-type furnace, at 400 DEG C, be incubated in air atmosphere and burn completely (sample constant weight) to absorbent cotton, obtain amorphous CoFe
2o
4powder;
(5) by the amorphous CoFe of step (4) gained
2o
4powder porphyrize, crosses 800 mesh sieves.Get 3g sieve after amorphous CoFe
2o
4particle, adds 300ml dehydrated alcohol, and ultrasonic disperse 2h makes amorphous CoFe
2o
4even particulate dispersion, in dehydrated alcohol, prepares ferrite particle-alcohol suspension.Get the resol of about 90ml, add in aforementioned suspension, ultrasonic disperse 2h, ferrite powder is dispersed in the ethanolic soln of resol.Then make ethanol evaporation 60 DEG C of mechanical stirring and make phenolic resin curing, obtaining the amorphous nano Co Fe that resol is coated
2o
4particle;
(6) by amorphous nano Co Fe coated for step (5) gained resol
2o
4particle is placed in tube-type atmosphere furnace, under rare gas element (nitrogen or argon gas) protection, is incubated 2h charing, obtains the nanometer spinel type CoFe that charcoal is coated at 800 DEG C
2o
4particle;
(7) by nanometer spinel type CoFe coated for step (6) gained charcoal
2o
4particle porphyrize crosses 800 mesh sieves, and by gained particle at 80 DEG C, volume percent is carry out carbon removal process in the perchloric acid solution of 80%, can obtain high purity, high-specific surface area, high magnetic characteristics nano Co Fe
2o
4particle.
Gained nano Co Fe
2o
4xRD test result inclusion-free phase, particle diameter is 30 ± 10nm, and specific surface area is 68.5m
2/ g; Saturation magnetization is 86.8emu/g, and residual magnetization is 41.1emu/g, and coercive force is 1176G, and squareness ratio is 0.47.Gained nano Co Fe
2o
4the TEM figure of particle is shown in Fig. 1, and magnetic hysteresis loop is shown in Fig. 2.
Embodiment 2
Described Nano-Ferrite Particle Ni
0.5zn
0.5fe
2o
4preparation method comprise the steps:
(1) by 10.1964g Fe (NO
3)
39H
2o, 1.8349g Ni (NO
3)
26H
2o and 1.8771g Zn (NO
3)
26H
2o is dissolved in 200ml dehydrated alcohol, prepares hybrid metal nitrate-ethanolic soln; 7.9555g citric acid is dissolved in 200ml ethanol, prepares citric acid-ethanolic soln; With vigorous stirring, citric acid-ethanolic soln is added in hybrid metal nitrate-ethanolic soln, Keep agitation 4h, form the ethanolic soln of hybrid metal nitrate-citric acid;
(2) under agitation, with the NH of 6mol/L
3h
2the pH value of O regulating step (1) gained solution is to 3.5, and then this solution concentrated forms viscosity is the colloidal sol of 0.015Pas;
(3) in step (2) gained colloidal sol, add about 15g absorbent cotton to adsorb this colloidal sol, after waiting absorbent cotton to be adsorbed by colloidal sol completely, move into 80 DEG C of oven dry in baking oven and, to constant weight, obtain xerogel-absorbent cotton;
(4) step (3) gained xerogel-absorbent cotton sample is put into box-type furnace, at 400 DEG C, be incubated in air atmosphere and burn completely (sample constant weight) to absorbent cotton, obtain amorphous Ni
0.5zn
0.5fe
2o
4powder;
(5) by the amorphous Ni of step (4) gained
0.5zn
0.5fe
2o
4powder porphyrize, crosses 800 mesh sieves.Get 2g sieve after Ni
0.5zn
0.5fe
2o
4particle, add the dehydrated alcohol dilution of 200ml, ultrasonic disperse 2h, makes ferrite particle be dispersed in ethanolic soln, prepares ferrite particle-alcohol suspension.Get the resol of about 60ml, add in aforementioned suspension, ultrasonic disperse 2h, ferrite powder is dispersed in resol ethanolic soln.Then make ethanol evaporation 60 DEG C of stirrings and make phenolic resin curing, obtaining the amorphous Ni nanoparticle that resol is coated
0.5zn
0.5fe
2o
4particle;
(6) by amorphous Ni nanoparticle coated for step (5) gained resol
0.5zn
0.5fe
2o
4particle product is placed in tube-type atmosphere furnace, under rare gas element (nitrogen or argon gas) protection, is incubated 2h charing, obtains the nanometer spinel type Ni that charcoal is coated at 900 DEG C
0.5zn
0.5fe
2o
4particle;
(7) by nanometer spinel type Ni coated for step (6) gained charcoal
0.5zn
0.5fe
2o
4particle porphyrize crosses 800 mesh sieves, and by gained particle at 70 DEG C, volume percent is carry out carbon removal process in the perchloric acid solution of 70%, can obtain high purity, high-specific surface area, high magnetic characteristics Ni nanoparticle
0.5zn
0.5fe
2o
4particle.
Gained Ni nanoparticle
0.5zn
0.5fe
2o
4xRD test result inclusion-free phase, particle diameter is 50 ± 10nm, and specific surface area can reach 95.8m
2/ g; Saturation magnetization is 66.8emu/g, residual magnetization 4.85emu/g, and coercive force is 56G, and squareness ratio is 0.07.
Embodiment 3
Described Nano-Ferrite Particle NiFe
2o
4preparation method comprise the steps:
(1) by 31.0265g Fe (NO
3)
39H
2o and 11.1665g Ni (NO
3)
36H
2o is dissolved in 600ml dehydrated alcohol, prepares hybrid metal nitrate-ethanolic soln; 24.2076g citric acid is dissolved in 600ml dehydrated alcohol, prepares citric acid ethanol-solution; With vigorous stirring, citric acid-ethanolic soln is added in hybrid metal nitrate-ethanolic soln, Keep agitation 3h, obtain the ethanolic soln of hybrid metal nitrate-citric acid;
(2) under agitation, with the NH of 6mol/L
3h
2the pH value of O regulating step (1) gained solution is to 3.5, and then this solution concentrated forms viscosity is the colloidal sol of 0.03Pas;
(3) in step (2) gained colloidal sol, add about 12g absorbent cotton to adsorb this colloidal sol, after waiting absorbent cotton to be adsorbed by colloidal sol completely, move into 80 DEG C of oven dry in baking oven and, to constant weight, obtain xerogel-absorbent cotton;
(4) step (3) gained xerogel-absorbent cotton sample is put into box-type furnace, at 500 DEG C, be incubated in air atmosphere and burn completely (sample constant weight) to absorbent cotton, obtain amorphous NiFe
2o
4powder;
(5) by the amorphous NiFe of step (4) gained
2o
4powder porphyrize, crosses 900 mesh sieves.Get 4g sieve after NiFe
2o
4particle, adds the dehydrated alcohol of 400ml, ultrasonic disperse 2h, makes ferrite particle be dispersed in dehydrated alcohol, prepares ferrite particle-alcohol suspension.Get the resol of about 150ml, add in aforementioned suspension, ultrasonic disperse 2h, ferrite powder is dispersed in resol ethanolic soln.Then make ethanol evaporation 60 DEG C of mechanical stirring and make phenolic resin curing, obtaining the amorphous nano-Ni/Fe that resol is coated
2o
4particle;
(6) by amorphous nano-Ni/Fe coated for step (5) gained resol
2o
4particle product is placed in tube-type atmosphere furnace, under rare gas element (nitrogen or argon gas) protection, is incubated 2h charing, obtains the nanometer spinel type NiFe that charcoal is coated at 900 DEG C
2o
4particle;
(7) by nanometer spinel type NiFe coated for step (6) gained charcoal
2o
4particle porphyrize crosses 800 mesh sieves, and by gained particle at 90 DEG C, volume percent is carry out carbon removal process in the perchloric acid solution of 90%, can obtain high purity, high-specific surface area, high magnetic characteristics nano-Ni/Fe
2o
4particle.
Gained nano-Ni/Fe
2o
4xRD test result inclusion-free phase, particle diameter is 40 ± 5nm, and specific surface area can reach 85.3m
2/ g; Saturation magnetization is 75.3emu/g, residual magnetization 7.85emu/g, and coercive force is 50G, and squareness ratio is 0.10.
Claims (7)
1. a preparation method for Nano-Ferrite Particle, is characterized in that, described method comprises the steps:
(1) hybrid metal nitrate is dissolved in dehydrated alcohol, is mixed with hybrid metal nitrate-ethanolic soln; Citric acid is dissolved in dehydrated alcohol, is mixed with citric acid-ethanolic soln; Hybrid metal nitrate-ethanolic soln is mixed with the volume ratio of citric acid-ethanolic soln by 1:1, obtained hybrid metal nitrate-citric acid ethanolic soln; Wherein, described hybrid metal nitrate is Fe (NO
3)
39H
2the mixture that the transition metal nitrate that O is different from one or both mixes according to the molar ratio forming spinel type ferrite, consisting of of described spinel type ferrite: M
xn
1-xfe
2o
4, M and N represents the transition-metal cation that different transition metal nitrate provides, 0≤x≤1; The add-on that described hybrid metal nitrate is dissolved in hybrid metal in dehydrated alcohol is: every 10g hybrid metal nitrate is dissolved in 50-300mL dehydrated alcohol; The add-on that described citric acid is dissolved in citric acid in dehydrated alcohol is: every 10g citric acid is dissolved in 50-300mL dehydrated alcohol;
(2) regulate the pH value of hybrid metal nitrate-citric acid ethanolic soln to be 0.5-6 with ammoniacal liquor, this solution concentrated obtains the colloidal sol that viscosity is 0.005-0.03Pas;
(3) in colloidal sol, add absorbent cotton, after colloidal sol adsorbs by absorbent cotton completely, absorbent cotton is dried, obtains xerogel-absorbent cotton;
(4) by xerogel-absorbent cotton in oxidizing atmosphere, under DEG C condition of temperature≤600 be incubated 0.5-6h, obtain amorphous iron ferrite powder;
(5) cross 600-900 mesh sieves by after the grinding of amorphous iron ferrite powder, obtain the amorphous iron ferrite powder after grinding; Amorphous iron ferrite powder after grinding is added in dehydrated alcohol, obtained ferrite particle-alcohol suspension after ultrasonic disperse; In ferrite particle-alcohol suspension, add resol, stir under 40-80 DEG C of conditions, after ethanol evaporation and phenolic resin curing, obtain the amorphous Nano-Ferrite Particle that resol is coated; Wherein, the add-on that the amorphous iron ferrite powder after described grinding adds amorphous iron ferrite powder in dehydrated alcohol is: the amorphous iron ferrite powder after every 1g grinding adds in 30-350mL dehydrated alcohol; The add-on that described resol adds resol in ferrite particle-alcohol suspension is: add 5-140mL resol in every 100mL ferrite particle-alcohol suspension;
(6) carbonized in inert atmosphere by amorphous Nano-Ferrite Particle coated for resol, carbonization temperature is 500-1100 DEG C, and carbonization time is 0.5-6h, obtains the nanometer spinel type ferrite particle that charcoal is coated;
(7) cross 600-900 mesh sieves by after nanometer spinel type ferrite particulate abrasive coated for charcoal, obtain the Nano-Ferrite Particle after grinding; After Nano-Ferrite Particle after grinding is carried out carbon removal process in acid, obtain Nano-Ferrite Particle.
2. the method for claim 1, is characterized in that, step (1) described transition metal is copper, nickel, cobalt or zinc.
3. the method for claim 1, is characterized in that, the ammonia concn described in step (2) is 1-12mol/L.
4. the method for claim 1, is characterized in that, the add-on of step (3) described absorbent cotton is: add 1-10g absorbent cotton in every 100mL colloidal sol; After colloidal sol adsorbs by absorbent cotton completely, absorbent cotton is dried under 60-100 DEG C of conditions.
5. the method for claim 1, is characterized in that, the oxidizing atmosphere described in step (4) refers to air atmosphere.
6. the method for claim 1, is characterized in that, the inert atmosphere described in step (6) is nitrogen atmosphere or argon atmospher.
7. the method for claim 1, is characterized in that, the acid described in step (7) to be concentration of volume percent be 40-100% perchloric acid, the temperature of carbon removal process is 40-100 DEG C.
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| CN104016414B (en) * | 2014-06-23 | 2015-11-18 | 湖南大学 | A kind of preparation method of ferrite nano line |
| CN104496454B (en) * | 2015-01-19 | 2016-02-03 | 陈吉美 | A kind of preparation method of Nano-Ferrite Particle |
| CN105753057A (en) * | 2016-01-21 | 2016-07-13 | 中国计量学院 | Soft magnetic nickel and zinc ferrite nanometer powder and method for preparing same |
| CN106145919A (en) * | 2016-07-05 | 2016-11-23 | 陕西科技大学 | A kind of preparation method of three-dimensional netted ferrite microwave absorbing material |
| CN108101114B (en) * | 2017-12-21 | 2020-05-01 | 湖南大学 | Nano ferrite composite material with double-shell structure and preparation method thereof |
| CN108417821B (en) * | 2018-03-07 | 2020-04-24 | 浙江大学 | Aluminum ion-seawater/aluminum composite battery and use method thereof |
| CN108617154B (en) * | 2018-04-16 | 2019-10-15 | 晋中学院 | A kind of porous carbon load nano nickel absorbing material and preparation method thereof |
| CN109295490A (en) * | 2018-11-26 | 2019-02-01 | 镇江市高等专科学校 | A kind of Ni ferrite electrophoresis suspensioning liquid and its preparation method and application |
| CN114014642A (en) * | 2021-10-09 | 2022-02-08 | 国家能源集团科学技术研究院有限公司 | Manganese-cobalt ferrite nano material and preparation method and application thereof |
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|---|---|---|---|---|
| US5585084A (en) * | 1994-06-20 | 1996-12-17 | Ube Industries, Ltd. | Silicon nitride powder |
| CN101531502A (en) * | 2009-04-03 | 2009-09-16 | 陕西科技大学 | Preparation method for barium ferrite magnetic powder |
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2014
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5585084A (en) * | 1994-06-20 | 1996-12-17 | Ube Industries, Ltd. | Silicon nitride powder |
| CN101531502A (en) * | 2009-04-03 | 2009-09-16 | 陕西科技大学 | Preparation method for barium ferrite magnetic powder |
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