CN104649234A - Preparation method of oxide hollow microspheres - Google Patents
Preparation method of oxide hollow microspheres Download PDFInfo
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- CN104649234A CN104649234A CN201310613226.4A CN201310613226A CN104649234A CN 104649234 A CN104649234 A CN 104649234A CN 201310613226 A CN201310613226 A CN 201310613226A CN 104649234 A CN104649234 A CN 104649234A
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- powder
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- oxide
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- 239000004005 microsphere Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 71
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 27
- 239000001301 oxygen Substances 0.000 claims abstract description 27
- QFXZANXYUCUTQH-UHFFFAOYSA-N ethynol Chemical group OC#C QFXZANXYUCUTQH-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002245 particle Substances 0.000 claims abstract description 20
- 239000007789 gas Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 229910052755 nonmetal Inorganic materials 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 5
- 239000000853 adhesive Substances 0.000 claims abstract description 4
- 230000001070 adhesive effect Effects 0.000 claims abstract description 4
- 230000001590 oxidative effect Effects 0.000 claims abstract 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- 239000008187 granular material Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000000498 ball milling Methods 0.000 claims description 12
- 239000007921 spray Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 7
- 210000003934 vacuole Anatomy 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000839 emulsion Substances 0.000 claims description 5
- 239000003822 epoxy resin Substances 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 229920000647 polyepoxide Polymers 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 4
- 238000005187 foaming Methods 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 229920001187 thermosetting polymer Polymers 0.000 claims description 4
- 238000007711 solidification Methods 0.000 claims description 3
- 230000008023 solidification Effects 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 18
- 239000007788 liquid Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 239000004088 foaming agent Substances 0.000 abstract 2
- 230000002277 temperature effect Effects 0.000 abstract 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 238000001311 chemical methods and process Methods 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 238000000053 physical method Methods 0.000 description 3
- -1 polyoxyethylene Polymers 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 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
- 238000009776 industrial production Methods 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/32—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process
- C01B13/322—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process of elements or compounds in the solid state
- C01B13/324—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process of elements or compounds in the solid state by solid combustion synthesis
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
- C01G9/03—Processes of production using dry methods, e.g. vapour phase processes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Glanulating (AREA)
Abstract
The invention relates to a preparation method of oxide hollow microspheres. The preparation method is characterized in that ball-milled and refined metal powder (or nonmetal) is mixed with a foaming agent, an adhesive is added, the mixture is ground into fine agglomerated particles after being dried and solidified, agglomerated particles are jetted into strong oxidative oxyacetylene torch to generate strong oxidation reaction on substances in the particles and oxygen under the high temperature effect of flame so as to generate molten oxide drops, the foaming agent is simultaneously decomposed to release gas, partial gas cannot overflow and is remained in the molten oxide drops to generate hollow liquid bubbles, and the hollow liquid bubbles are rapidly solidified to generate oxide hollow microspheres. The oxide hollow microspheres prepared by virtue of the preparation method have the advantages that the process is controllable, furthermore, microspheres with various specifications of metal and nonmetal oxide components and hollow structures can be generated, and the application is wide.
Description
Technical field
The present invention relates to a kind of preparation method of hollow oxide microsphere.
Background technology
Tiny balloon is the multi-functional powder material of a kind of novel-section that the seventies grows up, and has the features such as light weight, good fluidity, stable chemical performance, cost be low, is described as Space Age material.Ferric oxide hollow particle has special physicochemical property, has been widely used in the fields such as magnetic liquid, catalysis, optical filtering, electromagnetic wave absorbing material, magnetic recording material, coating, function ceramics.
The preparation method of oxidate microspheres mainly contains physical method and chemical process.Physical method prepares microballoon can adopt vacuum condensation method, physical pulverization method, mechanical attrition method etc.But the sample common product purity prepared with physical method is low, size distribution is uneven, so seldom adopted in industrial production and test.Chemical process mainly contains coprecipitation method, sol-gel method, microemulsion method, hydrolysis method, hydrothermal method etc.The particle run-of-the-mill of the particulate adopting chemical process to obtain is better, and granularity is less, but chemical process all exists certain deficiency, as low in productive rate, cost is high, equipment is complicated, powder collection is difficult.Become by Preparation cenosphere also to need expensive production unit, its complex process, cost is higher, should not promote.The preparation method of a kind of iron oxide hollow microsphere involved in the present invention, its production unit is simple, and cost is low, and balling ratio is high, has very large application and promotion prospect.
Summary of the invention
The object of this invention is to provide a kind of preparation method of hollow oxide microsphere.
Its main contents are after mixing with whipping agent with metal (or nonmetal) powder, add adhesive solidification, reunion powder granule is broken for after drying, then oxy-acetylene flame spray gun is adopted, purity oxygen is adopted to be that the dispersion of reunion powder granule is spurted in the oxyacetylene torch after lighting by powder feeding gas, material in powder reacts with pure oxygen generation vigorous oxidation under the effect of oxyacetylene torch high temperature, release a large amount of thermosetting liquid oxygen compound molten drops, molten drop foaming is formed hollow ball by thermogenetic gas by whipping agent simultaneously, hollow drop falls into deionized water and cools fast afterwards, obtain hollow oxide microsphere.
Principal feature of the present invention
1, the present invention can be used for hollow oxide microsphere preparation.
2, present device is simple, and lightly, easy to operate, be widely used, cost is low.
3, the tiny balloon balling ratio obtained of the present invention is high, can reach more than 95%.
4, generating period of the present invention is short, within 2-3 days, just can obtain a collection of finished product.
Embodiment
The present invention relates to a kind of preparation method of hollow oxide microsphere, concrete implementation step is:
(1) agglomerating particles powder is prepared: metal powder (or nonmetal) and quantitative whipping agent raw material are put into ball mill, ball milling more than 12 hours, makes material particles be less than 10 microns; After ball milling completes, then the solution containing tackiness agent (as epoxy resin) is become emulsion form with the powder stirring after ball milling, mix, put into oven for drying, temperature remains on 100-150 DEG C; After oven dry completes, the material of block will be become to take out, pulverize, cross 325 mesh sieves in pulverizer, obtaining particle diameter, to be less than the reunion powder particles of 45 microns stand-by.
(2) reunion powder granule above-mentioned steps prepared, loads in the barrel of oxy-acetylene flame spray gun, adopts purity oxygen to be powder feeding gas.Light oxyacetylene torch, adjustment flame is neutral flame, opens powder feeding oxygen, and powder feeding oxygen pressure remains on 0.6MPa, opens blanking barrel control valve, and reunion powder granule is penetrated and sucked spray gun pipeline by powder feeding oxygen, and the oxyacetylene torch after lighting is spurted in dispersion; Material in powder reacts with pure oxygen generation vigorous oxidation under the effect of oxyacetylene torch high temperature, release a large amount of thermosetting liquid oxygen compound molten drops, molten drop foaming is formed hollow vacuole by thermogenetic gas by whipping agent simultaneously, the hollow vacuole of melting afterwards falls into deionized water and cools fast, after supercentrifuge is separated, dehydrate, obtain hollow oxide microsphere.
Concrete embodiment
Embodiment 1
(1) take the Fe powder that 200 grams of median sizes are 5 microns, polyoxyethylene glycol whipping agent 20 grams, puts into high energy ball mill after mixing, ball milling 16 hours;
(2), after ball milling completes, add epoxy resin 20 grams and a certain amount of alcohol, stir;
(3) pour in drying basin by uniform emulsion form mixture, put into air dry oven and dry, temperature remains on about 120 DEG C;
(4), after having dried, by becoming the material of block to take out, pulverizing in agitation type pulverizer, crossing 350 mesh sieves, obtain reunion powder particles stand-by;
(5) the reunion powder granule prepared by above-mentioned steps, load in the barrel of oxy-acetylene flame spray gun, adopt purity oxygen to be powder feeding gas, powder feeding oxygen pressure remains on 0.6MPa;
(6) light oxyacetylene torch, adjustment flame is neutral flame, opens powder feeding oxygen, opens blanking barrel control valve, and reunion powder granule is penetrated and sucked spray gun pipeline by powder feeding oxygen, and the oxyacetylene torch after lighting is spurted in dispersion; Below flame, place deionized water, the hollow vacuole of reacted melting falls into deionized water and cools fast, receives reacted powder.
(7) particle will collected in deionized water, after supercentrifuge is separated, dehydrates, and obtains ferric oxide tiny balloon.
Embodiment 2
(1) take the Zn powder that 200 grams of median sizes are 5 microns, polyoxyethylene glycol whipping agent 20 grams, puts into high energy ball mill after mixing, ball milling 16 hours;
(2), after ball milling completes, add epoxy resin 20 grams and a certain amount of alcohol, stir;
(3) pour in drying basin by uniform emulsion form mixture, put into air dry oven and dry, temperature remains on about 120 DEG C;
(4), after having dried, by becoming the material of block to take out, pulverizing in agitation type pulverizer, crossing 350 mesh sieves, obtain reunion powder particles stand-by;
(5) the reunion powder granule prepared by above-mentioned steps, load in the barrel of oxy-acetylene flame spray gun, adopt purity oxygen to be powder feeding gas, powder feeding oxygen pressure remains on 0.6MPa;
(6) light oxyacetylene torch, adjustment flame is neutral flame, opens powder feeding oxygen, opens blanking barrel control valve, and reunion powder granule is penetrated and sucked spray gun pipeline by powder feeding oxygen, and the oxyacetylene torch after lighting is spurted in dispersion; Below flame, place deionized water, the hollow vacuole of reacted melting falls into deionized water and cools fast, receives reacted powder.
(7) particle will collected in deionized water, after supercentrifuge is separated, dehydrates, and obtains Zinc oxide hollow microsphere.
Embodiment 3
(1) take the Si powder that 200 grams of median sizes are 5 microns, polyoxyethylene glycol whipping agent 20 grams, puts into high energy ball mill after mixing, ball milling 16 hours;
(2), after ball milling completes, add epoxy resin 20 grams and a certain amount of alcohol, stir;
(3) pour in drying basin by uniform emulsion form mixture, put into air dry oven and dry, temperature remains on about 120 DEG C;
(4), after having dried, by becoming the material of block to take out, pulverizing in agitation type pulverizer, crossing 350 mesh sieves, obtain reunion powder particles stand-by;
(5) the reunion powder granule prepared by above-mentioned steps, load in the barrel of oxy-acetylene flame spray gun, adopt purity oxygen to be powder feeding gas, powder feeding oxygen pressure remains on 0.6MPa;
(6) light oxyacetylene torch, adjustment flame is neutral flame, opens powder feeding oxygen, opens blanking barrel control valve, and reunion powder granule is penetrated and sucked spray gun pipeline by powder feeding oxygen, and the oxyacetylene torch after lighting is spurted in dispersion; Below flame, place deionized water, the hollow vacuole of reacted melting falls into deionized water and cools fast, receives reacted powder.
(7) particle will collected in deionized water, after supercentrifuge is separated, dehydrates, and obtains silicon oxide tiny balloon.
Claims (4)
1. the preparation method of a hollow oxide microsphere, after it is characterized in that mixing with whipping agent with metal powder (or non-metal powder), add adhesive solidification, agglomerating particles powder is broken for after drying, then oxy-acetylene flame spray gun is adopted, purity oxygen is adopted to be that the dispersion of reunion powder granule is spurted in the oxyacetylene torch after lighting by powder feeding gas, material in powder reacts with pure oxygen generation vigorous oxidation under the effect of oxyacetylene torch high temperature, release a large amount of thermosetting liquid oxygen compound molten drops, molten drop foaming is formed hollow ball shape drop by thermogenetic gas by whipping agent simultaneously, hollow drop falls into deionized water and cools fast afterwards, obtain hollow oxide microsphere.
2. the method preparing hollow oxide microsphere according to claim 1, is characterized in that hollow oxide microsphere following steps obtain:
(1) form metal powder (or non-metal powder) and mix rear reunion powder granule with whipping agent: metal fine powder (or non-metal powder) and quantitative whipping agent raw material are put into ball mill, ball milling more than 12 hours, makes material particles be less than 10 microns; After ball milling completes, then the solution containing tackiness agent (as epoxy resin) is become emulsion form with the powder stirring after ball milling, mix, put into oven for drying, temperature remains on 100-150 DEG C; After oven dry completes, the material of block will be become to take out, pulverize, cross 325 mesh sieves in pulverizer, obtaining particle diameter, to be less than the reunion powder particles of 45 microns stand-by.
(2) reunion powder granule above-mentioned steps prepared, loads in the barrel of oxy-acetylene flame spray gun, adopts purity oxygen to be powder feeding gas.Light oxyacetylene torch, adjustment flame is neutral flame, opens powder feeding oxygen, and powder feeding oxygen pressure remains on 0.6MPa, opens blanking barrel control valve, and reunion powder granule is penetrated and sucked spray gun pipeline by powder feeding oxygen, and oxyacetylene torch is spurted in dispersion; Material composition in reunion powder reacts with oxygen generation vigorous oxidation under the effect of oxyacetylene torch high temperature, release a large amount of thermosetting liquid oxygen compound molten drops, molten drop foaming is formed hollow vacuole by thermogenetic gas by whipping agent simultaneously, the hollow vacuole of melting afterwards falls into deionized water and cools fast, after supercentrifuge is separated, dehydrate, obtain hollow oxide microsphere.
3. the method preparing hollow oxide microsphere according to claim 2, is characterized in that: after mixing with whipping agent with metal powder (or non-metal powder), add adhesive solidification, is broken for particle diameter and is less than 45 microns of reunion powder granules after drying.
4. the method preparing hollow oxide microsphere according to claim 2, it is characterized in that: adopt purity oxygen to be powder feeding gas, forming oxygen enrichment hot environment, at high temperature there is violent oxidizing reaction in metal fine powder (or non-metal powder) and oxygen, generates oxide compound.
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CN201310613226.4A CN104649234A (en) | 2013-11-25 | 2013-11-25 | Preparation method of oxide hollow microspheres |
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CN201310613226.4A CN104649234A (en) | 2013-11-25 | 2013-11-25 | Preparation method of oxide hollow microspheres |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106830982A (en) * | 2017-03-21 | 2017-06-13 | 兰州理工大学 | A kind of method for preparing hollow ceramic microspheres |
Citations (2)
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CN101870588A (en) * | 2009-04-21 | 2010-10-27 | 河北勇龙邦大新材料有限公司 | Method and device for preparing hollow ceramic microspheres |
CN104658732A (en) * | 2013-11-25 | 2015-05-27 | 中国人民解放军军械工程学院 | New Al-Ni-Co hollow magnetic microsphere microwave absorbing material |
-
2013
- 2013-11-25 CN CN201310613226.4A patent/CN104649234A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101870588A (en) * | 2009-04-21 | 2010-10-27 | 河北勇龙邦大新材料有限公司 | Method and device for preparing hollow ceramic microspheres |
CN104658732A (en) * | 2013-11-25 | 2015-05-27 | 中国人民解放军军械工程学院 | New Al-Ni-Co hollow magnetic microsphere microwave absorbing material |
Non-Patent Citations (2)
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106830982A (en) * | 2017-03-21 | 2017-06-13 | 兰州理工大学 | A kind of method for preparing hollow ceramic microspheres |
CN106830982B (en) * | 2017-03-21 | 2020-04-17 | 兰州理工大学 | Method for preparing hollow ceramic microspheres |
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Application publication date: 20150527 |