CN100406406C - Method for preparing M-type barium ferrite magnetic powder - Google Patents
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- CN100406406C CN100406406C CNB2005100282070A CN200510028207A CN100406406C CN 100406406 C CN100406406 C CN 100406406C CN B2005100282070 A CNB2005100282070 A CN B2005100282070A CN 200510028207 A CN200510028207 A CN 200510028207A CN 100406406 C CN100406406 C CN 100406406C
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- 239000006247 magnetic powder Substances 0.000 title claims abstract description 20
- AJCDFVKYMIUXCR-UHFFFAOYSA-N oxobarium;oxo(oxoferriooxy)iron Chemical compound [Ba]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O AJCDFVKYMIUXCR-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title abstract description 22
- 238000002360 preparation method Methods 0.000 claims abstract description 30
- 239000000243 solution Substances 0.000 claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 150000001720 carbohydrates Chemical class 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 239000012266 salt solution Substances 0.000 claims abstract description 11
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 9
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 8
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- 239000002184 metal Substances 0.000 claims abstract description 7
- 239000008139 complexing agent Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 239000007791 liquid phase Substances 0.000 claims abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 21
- 238000004448 titration Methods 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 11
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 10
- 229930006000 Sucrose Natural products 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 9
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims description 9
- 238000007669 thermal treatment Methods 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 7
- WAAJFQMOZDHLQL-UHFFFAOYSA-N barium;oxoiron Chemical compound [Ba].[Fe]=O WAAJFQMOZDHLQL-UHFFFAOYSA-N 0.000 claims description 7
- 229910052593 corundum Inorganic materials 0.000 claims description 7
- 239000010431 corundum Substances 0.000 claims description 7
- 239000012065 filter cake Substances 0.000 claims description 7
- 238000002203 pretreatment Methods 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000005720 sucrose Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 229910002651 NO3 Inorganic materials 0.000 claims description 5
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims description 5
- 229910001864 baryta Inorganic materials 0.000 claims description 5
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052788 barium Inorganic materials 0.000 claims description 3
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- 108010009736 Protein Hydrolysates Proteins 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- 238000003828 vacuum filtration Methods 0.000 claims description 2
- 239000000696 magnetic material Substances 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- 238000000605 extraction Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 12
- 230000005415 magnetization Effects 0.000 description 12
- 230000005308 ferrimagnetism Effects 0.000 description 7
- 206010013786 Dry skin Diseases 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000036571 hydration Effects 0.000 description 5
- 238000006703 hydration reaction Methods 0.000 description 5
- 229910000608 Fe(NO3)3.9H2O Inorganic materials 0.000 description 4
- 159000000009 barium salts Chemical class 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 3
- 235000014633 carbohydrates Nutrition 0.000 description 3
- 238000000975 co-precipitation Methods 0.000 description 3
- 229960000935 dehydrated alcohol Drugs 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
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- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
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- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
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- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
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- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Landscapes
- Hard Magnetic Materials (AREA)
- Compounds Of Iron (AREA)
Abstract
The present invention relates to a preparation method of M type barium ferrite magnetic powder, which belongs to the technical field of magnetic material preparation. The present invention uses saccharide hydrolysates as a complexing agent, a solvent is eliminated through the extraction by low carbon alcohol, and a metal salt solution is mixed with a saccharide solution; then the salt solution which needs doping with metal ions is added, the mixed solution is heated to evaporate water, a barium ferrite hydrate is generated through liquid phase reaction, the solution after the reaction is cooled, the pH value is regulated, water is extracted and removed, and then the solution is pumped and filtered in a vacuum and is dried to obtain a precursor; finally the heat treatment of the precursor is carried out to obtain the magnetic ferrite powder. The method of the present invention has the advantages of low material cost, short preparation time, easy control of technological process and good repeatability and portability, and prepared powder magnetic materials can be used for the fields of stealth materials, etc.
Description
Technical field
The present invention relates to a kind of preparation method of technical field of magnetic materials, specifically, is a kind of preparation method of M type barium ferrite magnetic powder.
Background technology
Ferrite is an oxidate magnetic material most widely used, that have ferrimagnetism, because of its resistivity far above metallicl magnetic material, thereby at high frequency, pulse, microwave and optical frequency wave band, radio electronics, communication, microwave electronics and information storage and processing, and scientific and technical aspect such as stealthy suction ripple is widely used.Up to the present, the method for preparing ultra thin hexagonal crystal system ferrite mainly contains following several: 1, solid reaction process: this method is with reactant feed, mix by a certain percentage as oxide compound or carbonate, ball milling, pyroprocessing, big with this technology synthetic particles of magnetic material diameter, size-grade distribution is wide, and the ball milling operating process meeting of long period simultaneously causes the loss of stoichiometry material and sneaks into the impurity of nonstoichiometric composition; 2, chemical coprecipitation: this method is that the soluble salt solution of required metallic element is mixed by a certain percentage, adds precipitation agent then, makes its co-precipitation, after filtration, cleans the back sintering.The precipitation difficulty that this method forms is cleaned, easy residual impurity, and the production cycle is long, and owing to the kind of this method to metal ion and precipitation agent, the control of pH value scope requires height during co-precipitation, and then this method applicable surface is narrower; 3, hydro-thermal reaction: this method is to utilize the property of the aqueous solution under the high pressure, reacts in autoclave, and the equipment requirements height of use is difficult for promoting; 4, sol-gel method: exactly raw material is made colloidal sol, dehydration obtains gel, and the thermal treatment gel obtains product again.A lot of at present researchs are to prepare ferrite with citric acid and Padil as complexing agent.
Find through literature search prior art, the Chinese patent title: citric acid complex prepares the method for M-type ferrite nanoparticle, publication number: CN 1472166A, and this patent adopts citric acid to make complexing agent, obtain presoma with sol-gel method, the thermal treatment presoma prepares ferrite then.Because this method of employing exists the conditional request of raw material type and formation gel higher, the citric acid consumption is big, raw materials cost height, deficiencies such as dehydration and heat treatment time length.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of preparation method of M type barium ferrite magnetic powder is provided, make it overcome the raw material costliness that exists in the traditional method, complex process, the problem that dewatering time is long.The present invention adopts the carbohydrate hydrolyzed product to make complexing agent, and the micella with obtaining metal ion after the abundant complexing of metal ion behind this micella of thermal treatment, obtains ferrite powder.
The present invention is achieved by the following technical solutions, the present invention desolvates as complexing agent with the low-carbon alcohol extrct with the carbohydrate hydrolysate, metal salt solution is mixed with saccharide solution, add the salts solution of wanting adulterated metal ion then on demand, heating evaporation moisture content, generate a kind of hydrate of barium iron oxygen through liquid phase reaction, with this reacted solution cooling, regulate the pH value, the extrct branch that anhydrates, vacuum filtration and drying obtain presoma then, and the precursor thermal treatment with forming obtains magnetic ferrite powder.
Below the inventive method is described further, step is as follows:
The a raw material is equipped with: the metal-salt that takes by weighing iron content, barium according to required proportioning, as iron nitrate, nitrate of baryta, barium carbonate, barium acetate, hydrated barta, and the sugar of 1-3 times of metal ion mole number, as sucrose, glucose, starch, and add small amount of deionized water respectively and be mixed with the aqueous solution, the metal salt solution and the saccharide solution of iron, barium are added in the reactor, and stirring at room mixes.
The preparation of b hydrated iron oxysome precursor: reactor is fixed on the device heats, temperature is controlled at 80-120 ℃, continuously stirring after question response is finished, stops heating, above-mentioned reactor is taken out, keep stirring, cooling slowly drips sig water, to the pH value of solution value be 6--7, form dark solution this moment; With 2 times low-carbon alcohol titration extracting, the low-carbon alcohol that extracting is used is preferably ethanol, Virahol, propyl carbinol, stirs 30 minutes after titration finishes, and suction filtration gets filter cake, and is dry in baking oven, obtains presoma.
The preparation of c magnetic powder: place corundum to burn in the boat above-mentioned presoma, pre-treatment in retort furnace is heat-treated then, heat up with 10 ℃ of speed of per minute, and under 1100 ℃, kept 0.5-2.0 hour, cooling can make magnetic ferrite powder again.
Because in the presence of acidic solution and strong oxidizer, carbohydrate is understood hydrolysis and is oxidized to carboxylic acid, and metal ion combines with the dissociative carboxylate radical, forms the equally distributed hydrate of metal ion, handle this hydrate and obtain ferritic precursor, this precursor of thermal treatment forms magnetic ferrite powder.The present invention just is based on this principle proposition.
Compare with prior art, the present invention is reflected in the stoichiometric solution and carries out, and is uniformly dispersed, and has omitted mechanical milling process, shortens the production cycle, cuts down the consumption of energy, and helps suitability for industrialized production; Owing to save traditional ball-milling technology, therefore prescription stoichiometry of the present invention is accurate, and control is easy, good reproducibility, and transplantability is good, particularly the needs trace is added adulterated ferrite technology operation commonly used, and control very accurately can be arranged; Sintering temperature is starkly lower than traditional solid phase reaction process, and heat treatment time shortens greatly.Simultaneously can be by different thermal treatment temps and time control grain-size.
Adopt the ferrite doped calcium magneticsubstance of the inventive method preparation, the variation of its hotchpotch trace all can detect and control the influence of the electromagnetic performance of final sample, and process stabilizing, is easy to repetition, stable performance.The inventive method is not only applicable to the various soluble salt solute dopings of alkaline-earth metal, main metal, transition metal, nonmetal, rare earth element, and can also carry out the mixing and doping of two or more element as required.In addition, the inventive method ferrite doping process of also can be used for the adulterated technology of other ferrite magnetic material and needing atmosphere control.
Embodiment
Further provide detailed embodiment in conjunction with above-mentioned summary of the invention:
Embodiment one:
The a raw material is equipped with: take by weighing analytically pure iron nitrate (Fe (NO
3)
3.9H
2O) 116.2 grams, nitrate of baryta (Ba (NO
3)
2) 6.54 grams, white sugar 213.75 gram, material molar ratio is a sucrose: (Fe+Ba)=2, and add deionized water respectively and be mixed with the aqueous solution, iron, barium salt solution and saccharide solution are joined in the flask of 2000ml, stirring at room mixes.
The preparation of b hydration barium iron oxygen precursor: flask is fixed on the heating unit heats, temperature is controlled at 80 ℃, and continuously stirring is after question response is finished, stop heating, above-mentioned reactor is taken out, keep stirring cooling, slowly drip sig water, to the pH value of solution value be 7, form dark solution this moment; With 2 times dehydrated alcohol titration extracting, after finishing, titration stirred 30 minutes, and suction filtration obtains filter cake, and 80 ℃ of dryings obtain presoma in vacuum drying oven.
The preparation of c magnetic powder: place corundum to burn in the boat above-mentioned presoma, 450 ℃ of pre-treatment are two hours in retort furnace, with 10 ℃ of heat-up rate to 1100 ℃ temperature of per minute, keep 1 hour then, lower the temperature then, can make the ferrimagnetism powder.This ferrimagnetism powder is of a size of the hexagonal plate crystal grain of 200～300nm.Under the foreign field of 5T, saturation magnetization is 42.34emu/g, and residual magnetization is 20.6emu/g, and coercive force is 1624.9Oe.
Embodiment two:
The a raw material is equipped with: take by weighing analytically pure iron nitrate (Fe (NO
3)
3.9H
2O) 116.2 grams, barium acetate (Ba (CH
3COO)
2) 6.39 grams, white sugar 106.89 grams, material molar ratio is a sucrose: (Fe+Ba)=1.And add deionized water respectively and be mixed with the aqueous solution, iron, barium salt solution and sugar soln being joined in the flask of 2000ml, stirring at room mixes.
The preparation of b hydration barium iron oxygen complex: flask is fixed on the heating unit heats, temperature is controlled at 120 ℃, and continuously stirring is after question response is finished, stop heating, above-mentioned reactor is taken out, keep stirring cooling, slowly drip sig water, to the pH value of solution value be 7, form dark solution this moment; With 2 times dehydrated alcohol titration extracting, after finishing, titration stirred 30 minutes, and suction filtration obtains filter cake, and 80 ℃ of dryings obtain presoma in vacuum drying oven.
The preparation of c magnetic powder: place corundum to burn in the boat above-mentioned presoma, 450 ℃ of pre-treatment are two hours in retort furnace, with 10 ℃ of heat-up rate to 1100 ℃ temperature of per minute, keep 2 hours then, cooling can make sheet hexagonal barium ferrite magnetic powder then.Under the foreign field of 5T, saturation magnetization is 60.48emu/g, and residual magnetization is 32.84emu/g, and coercive force is 1788.85Oe.
Embodiment three:
The a raw material is equipped with: with embodiment one.
The preparation of b hydration barium iron oxygen precursor: flask is fixed on the heating unit heats, temperature is controlled at 120 ℃, and continuously stirring is after question response is finished, stop heating, above-mentioned reactor is taken out, keep stirring cooling, slowly drip sig water, to the pH value of solution value be 6, form dark solution this moment; With 2 times dehydrated alcohol titration extracting, after finishing, titration stirred 30 minutes, and suction filtration obtains filter cake, and 80 ℃ of dryings obtain presoma in vacuum drying oven.
The preparation of c magnetic powder: place corundum to burn in the boat above-mentioned presoma, 450 ℃ of pre-treatment are two hours in retort furnace, with 10 ℃ of heat-up rate to 1100 ℃ temperature of per minute, keep 2 hours then, lower the temperature then, can make the ferrimagnetism powder.This ferrimagnetism powder grain-size is 300～400nm.Under the foreign field of 5T, saturation magnetization is 64.48emu/g, and residual magnetization is 33.84emu/g, and coercive force is 1848.9Oe.
Embodiment four:
The a raw material is equipped with: take by weighing analytically pure iron nitrate (Fe (NO
3)
3.9H
2O) 116.2 grams, nitrate of baryta (Ba (NO
3)
2) 6.54 grams, white sugar 320.67 grams, material molar ratio is a sucrose: (Fe+Ba)=3., and add small amount of deionized water respectively and be mixed with the aqueous solution, iron, barium salt solution and saccharide solution being joined in the flask of 2000ml, stirring at room mixes.
The preparation of b hydration barium iron oxygen precursor: flask is fixed on the heating unit heats, temperature is controlled at 100 ℃, and continuously stirring is after question response is finished, stop heating, above-mentioned reactor is taken out, keep stirring cooling, slowly drip sig water, to the pH value of solution value be 6, form dark solution this moment; With 2 times propyl carbinol titration extracting, after finishing, titration stirred 30 minutes, and suction filtration obtains filter cake, and 80 ℃ of dryings obtain presoma in vacuum drying oven.
The preparation of c magnetic powder: place corundum to burn in the boat above-mentioned presoma, 450 ℃ of pre-treatment are two hours in retort furnace, with 10 ℃ of heat-up rate to 1100 ℃ temperature of per minute, keep 0.5 hour then, lower the temperature then, can make the ferrimagnetism powder.Under the foreign field of 3T, saturation magnetization is 38.46emu/g, and residual magnetization is 21.6emu/g, and coercive force is 1823.5Oe.
Embodiment five:
The a raw material is equipped with: take by weighing analytically pure iron nitrate (Fe (NO
3)
3.9H
2O) 116.2 grams, hydrated barta (Ba (OH)
2.8H
2O) 7.89 grams, white sugar 213.75 grams, material molar ratio is a sucrose: (Fe+Ba)=2., and add small amount of deionized water respectively and be mixed with the aqueous solution, iron, barium salt solution and saccharide solution being joined in the flask of 2000ml, stirring at room mixes.
B hydration barium iron oxygen precursor prepares: flask is fixed on the heating unit heats, temperature is controlled at 80 ℃, and continuously stirring is after question response is finished, stop heating, above-mentioned reactor is taken out, keep stirring cooling, slowly drip sig water, to the pH value of solution value be 6.5, form dark solution this moment; With 2 times Virahol titration extracting, after finishing, titration stirred 30 minutes, and suction filtration obtains filter cake, and 80 ℃ of dryings obtain presoma in vacuum drying oven.
The preparation of c magnetic powder: place corundum to burn in the boat above-mentioned presoma, 450 ℃ of pre-treatment are two hours in retort furnace, with 10 ℃ of heat-up rate to 1100 ℃ temperature of per minute, keep 1.5 hours then, lower the temperature then, can make the ferrimagnetism powder.Under the foreign field of 3T, saturation magnetization is 61.12emu/g, and residual magnetization is 43.8emu/g, and coercive force is 1748.6Oe.
Embodiment six:
The preparation method is identical with embodiment one, and different is to be doped with cobalt metal and titanium ion, adopts Xiao Suangu, and tetra-n-butyl titanate is made hotchpotch, and thermal treatment temp is 1100 ℃, and heat treatment time was respectively 1 hour.Under the foreign field of 3T, saturation magnetization is 52.16emu/g, and residual magnetization is 23.8emu/g, and coercive force is 1725.9Oe.
Claims (7)
1. the preparation method of a M type barium ferrite magnetic powder, it is characterized in that, desolvate as complexing agent with the low-carbon alcohol extrct with the carbohydrate hydrolysate, its concrete preparation process is: metal salt solution is mixed with saccharide solution, heating evaporation moisture content, generate a kind of hydrate of barium iron oxygen through liquid phase reaction, with this reacted solution cooling, regulate the pH value, the extrct branch that anhydrates, vacuum filtration and drying obtain presoma then, and the precursor thermal treatment with forming obtains magnetic ferrite powder; Described metal-salt is the combination of iron nitrate and nitrate of baryta, or is the combination of iron nitrate and barium acetate, or is the combination of iron nitrate and hydrated barta.
2. the preparation method of M type barium ferrite magnetic powder according to claim 1 is characterized in that, comprises the steps:
The a raw material is equipped with: take by weighing iron nitrate according to required proportioning, nitrate of baryta or barium acetate or hydrated barta, and the carbohydrate of 1-3 times of metal ion mole number, and add deionized water respectively and be mixed with the aqueous solution, the metal salt solution and the saccharide solution of iron, barium are added in the reactor, and stirring at room mixes;
The preparation of b hydrated iron oxysome precursor: reactor is fixed on the device heats, continuously stirring is after question response is finished, stop heating, above-mentioned reactor is taken out, keep stirring cooling, slowly drip sig water, form dark solution, with the low-carbon alcohol titration extracting of twice, suction filtration gets filter cake, dry in baking oven, obtain presoma;
The preparation of c magnetic powder: place corundum to burn in the boat above-mentioned presoma, pre-treatment in retort furnace is heat-treated then, and cooling promptly makes magnetic ferrite powder again.
3. according to the preparation method of claim 1 or 2 described M type barium ferrite magnetic powders, it is characterized in that described carbohydrate is meant: a kind of in sucrose, the glucose.
4. the preparation method of M type barium ferrite magnetic powder according to claim 2 is characterized in that, among the step b, described reactor is fixed on the device and heats, and heating and temperature control is at 80-120 ℃.
5. the preparation method of M type barium ferrite magnetic powder according to claim 2 is characterized in that, among the step b, described slow dropping sig water, to the pH value of solution value be 6-7.
6. the preparation method of M type barium ferrite magnetic powder according to claim 2 is characterized in that, among the step b, and described low-carbon alcohol titration extracting, low-carbon alcohol is a kind of in ethanol, Virahol, the propyl carbinol, stirred 30 minutes the titration back that finishes.
7. the preparation method of M type barium ferrite magnetic powder according to claim 2 is characterized in that, among the step c, described thermal treatment is specially: with 10 ℃ of heat-up rate to 1100 ℃ temperature of per minute, be incubated 0.5-2.0 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100282070A CN100406406C (en) | 2005-07-28 | 2005-07-28 | Method for preparing M-type barium ferrite magnetic powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100282070A CN100406406C (en) | 2005-07-28 | 2005-07-28 | Method for preparing M-type barium ferrite magnetic powder |
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| CN102260071B (en) * | 2011-05-23 | 2012-12-05 | 哈尔滨工业大学 | Method for preparing high-dispersion quasi-spherical M type barium ferrite |
| CN103102867B (en) * | 2013-01-24 | 2014-12-17 | 浙江大学 | Metal ion doped barium ferrite wave absorbing powder and preparation method thereof |
| CN112349508B (en) * | 2020-12-08 | 2022-05-03 | 安徽泰龙锌业有限责任公司 | Method for preparing magnetic material by using zinc-containing waste material |
| CN112442334A (en) * | 2020-12-18 | 2021-03-05 | 中钢集团南京新材料研究院有限公司 | Barium ferrite carbon sphere composite wave-absorbing material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4778734A (en) * | 1987-02-03 | 1988-10-18 | Ube Industries, Ltd. | Barium ferrite magnetic powder and magnetic recording medium containing the same |
| US5078984A (en) * | 1988-06-01 | 1992-01-07 | Sakai Chemical Industry Co., Ltd. | Process for producing microcrystalline barium ferrite platelets |
| CN1202707A (en) * | 1997-06-14 | 1998-12-23 | 中国科学院山西煤炭化学研究所 | Method for preparing super fine barium ferrite powder |
| CN1427166A (en) * | 2001-12-18 | 2003-07-02 | 乐金电子(天津)电器有限公司 | Antifriction device of compressor |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4778734A (en) * | 1987-02-03 | 1988-10-18 | Ube Industries, Ltd. | Barium ferrite magnetic powder and magnetic recording medium containing the same |
| US5078984A (en) * | 1988-06-01 | 1992-01-07 | Sakai Chemical Industry Co., Ltd. | Process for producing microcrystalline barium ferrite platelets |
| CN1202707A (en) * | 1997-06-14 | 1998-12-23 | 中国科学院山西煤炭化学研究所 | Method for preparing super fine barium ferrite powder |
| CN1427166A (en) * | 2001-12-18 | 2003-07-02 | 乐金电子(天津)电器有限公司 | Antifriction device of compressor |
Non-Patent Citations (2)
| Title |
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| 纳米钡铁氧体制备技术的研究进展. 王琦洁，黄英，熊佳.硅酸盐通报，第24卷第3期. 2005 |
| 纳米钡铁氧体制备技术的研究进展. 王琦洁，黄英，熊佳.硅酸盐通报，第24卷第3期. 2005 * |
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