CN101264913B - Fast preparation method for coralloid nano alpha-Al2O3 - Google Patents
Fast preparation method for coralloid nano alpha-Al2O3 Download PDFInfo
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- CN101264913B CN101264913B CN2008100235232A CN200810023523A CN101264913B CN 101264913 B CN101264913 B CN 101264913B CN 2008100235232 A CN2008100235232 A CN 2008100235232A CN 200810023523 A CN200810023523 A CN 200810023523A CN 101264913 B CN101264913 B CN 101264913B
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Abstract
The invention discloses a rapid preparation method for a coralliform nanometer Alpha-Al<SUB>2</SUB>O<SUB>3</SUB>, belonging to inorganic nanometer preparation field. The technical proposal adopted by the invention comprises: preparing aluminum salt solution between zero point five and two mol/L by utilizing soluble inorganic aluminum salt, adding fuel to water solution with the mass ratio betweenzero point two and zero point five parts of fuel to one part of aluminum salt, then adding surface-active material accounting for zero point five to one point five percent of the aluminum salt mass, adopting high-speed mechanical agitation or grinding craft to make into viscous paste shape liquid, putting the paste-shape liquid to a muffle preheated to seven hundred to nine hundred DEG C, collecting the combusted product after the combustion is completed, obtaining the vivid coralliform nanometer Alpha-Al<SUB>2</SUB>O<SUB>3</SUB> powder.The rapid preparation method for a coralliform nanometerhas the advantages of easily available raw material, low cost, simple techonoly, rapid reaction, washing-free and grinding-free products, and industrial polularization value.
Description
Technical field
The present invention relates to a kind of coralloid nano alpha-Al
2O
3Fast preparation method, belong to field of inorganic nano-material preparation.
Background technology
Nanometer α-Al
2O
3Owing to have good wearability, corrosion resistance, optical stability, electrical property, ultraviolet absorbability, catalytic and good biocompatibility, have special purposes in fields such as wear-resisting, insulation, fire-retardant, sound insulation, catalysis, fine ceramics, microelectronic elements, become that a kind of application is wide, the urgent nano material of demand.
Size and morphology control are the focuses that field of nano material preparation is paid close attention to always, and when how finishing size control by the improvement of processing condition, giving the special pattern of nano material of seeing size that is situated between is the target that investigation of materials person chases all the time.
Exist crystal formation, size and pattern in the nano aluminium oxide preparation process at present and be difficult to the problems such as control, restricting application and development, the especially α-Al of nano aluminium oxide
20
3Size and pattern control because α-Al
2O
3Formation generally will be at 1200 ℃ high temperature, more difficult controlling dimension grows up and special pattern under this temperature.Although relevant preparation α-Al on the document
2O
3Method a lot, alum pyrolysismethod, chlorethanol method, improvement Bayer process, induced with laser vapour deposition process, plasma (orifice) gas phase synthesi, alkoxide hydrolysis, spray drying process, sol-gel process, template intervention method etc. are arranged, and general what generate is the microscopic pattern of spherical and class sphere but adopt these methods.Various microscopic pattern nanometer α-Al in recent years
2O
3Preparation caused researcher's concern, bibliographical information is existing about cellular, fibrous, flake nano α-Al
2O
3Synthetic, adopt the two-step anodization method to prepare apparent pore diameter such as document [Materials Science and Engineering journal, 2005,24 (3)] and increase to the regular porous alumina formwork of 70nm from 30nm; Document [Chinese Journal of Inorganic Chemistry, 2006,22 (1)] prepares the Technology for Heating Processing of hydrated alumina by controlling sol-gel method, obtain the fibrous or globular α-Al of Nano grade
2O
3Document [Chinese powder technology, 2005,6] adopts on the standby basis of alumina technology of aluminium carbonate ammonium legal system, by adding the methods such as crystal growth promoters and change thermal decomposition process, has effectively controlled a-Al
2O
3The size of particle and pattern obtain hexagonal plate particle and round pie particle; Document [Acta PhySico-Chimica Sinica, 2005,21 (11)] adopts the secondary anode oxidation technology, and the aluminium anode oxide film (from the O template) of preparation high-sequential is put template in people's corrosive liquid, can obtain the alumina nanowires of a large amount of impalpable structures.Document [Journal of Inorganic Materials, 2006,21 (4)] report utilizes phosphoric acid solution dipping to have unique hexagonal structure and the porous type anodised aluminium (PAAO) of composition, has obtained the nano-alumina fiber of the different-shape such as banded, bar-shaped, tubulose; Document [Rare Metals Materials and engineering, 2006,35 (9)] adopts organogel one thermal decomposition method to prepare fine magnesia, α-Al take citric acid, lactic acid and slaine as raw material
2O
3With spinel structure magnesium aluminate fiber, the densification of gained fibre structure, crystal grain are tiny, and diameter can be less than 1 μ m, and draw ratio is big.But up to now, preparation coralloid nano alpha-Al is not arranged on the document
2O
3Report, only mention the coralliform aluminium oxide during source of document [Shandong metallurgy, 2004,6] field trash in discussing casting process, infer that it may derive from original dendroid or point bunch shape alumina inclusion and act on by " Ostwald-ripening " and forming.
Summary of the invention
The object of the present invention is to provide that a kind of technology is simple, preparation fast, the coralloid nano alpha-Al of product good dispersion
2O
3The preparation method.
The technical solution adopted in the present invention is: a kind of coralloid nano alpha-Al is provided
2O
3Fast preparation method:
(1) the solubility inorganic aluminate is mixed with the aluminum saline solution of 0.5～2.0mol/L;
(2) fuel is joined in the above-mentioned aqueous solution, the mass ratio of fuel and aluminium salt is 0.2～0.5: 1, adds the tensio-active agent of aluminium salt quality 0.5～1.5% again, adopts high speed machine to stir or grinding technics, makes heavy-gravity paste liquid;
(3) above-mentioned paste liquid is put into the Muffle furnace that is heated in advance 700～900 ℃ of temperature, burning is namely collected combustion product after finishing, and obtains coralloid nano alpha-Al
2O
3Powder.
Described inorganic aluminate is a kind of in aluminum nitrate, aluminum chloride and the Tai-Ace S 150 or their arbitrary combination.Described fuel is the ammonium class, comprises a kind of in urea, ammonium sulfate, volatile salt, bicarbonate of ammonia, ammoniumper chlorate and the ammonium nitrate or their arbitrary combination.Described surfactant is anion and the non-ionic surface active agent with foaming and thickening power.
Outstanding advantage of the present invention is: utilize combustion reactions to synthesize coralloid nano alpha-Al2O3 powder, technology is simple, and it is quick to be swift in response, and need not washing in the process, and the waste gas of generation adopts alkali lye to absorb, and is pollution-free.The process and the product pattern of combustion reactions can be effectively controlled in the adjusting of fuel element and tensio-active agent in the combustion processes, make combustion reactions steadily orderly, the product easily collecting.The product of preparation has fluffy, purity advantages of higher, need not to grind, and is dispersed good.
Description of drawings
Fig. 1 is the prepared coralloid nano alpha-Al of the embodiment of the invention 1
2O
3The X diffraction pattern of powder;
Fig. 2 is the prepared coralloid nano alpha-Al of the embodiment of the invention 1
2O
3The sem photograph of powder;
Fig. 3 is the prepared coralloid nano alpha-Al of the embodiment of the invention 1
2O
3The transmission electron microscope picture of powder.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is further described:
Embodiment 1:
With 10gAlCl
36H
2O is dissolved in the 50ml deionized water, be made into settled solution, in solution, add 2g urea, the fuel that 1g ammonium nitrate and 1g ammonium perchlorate form, adding 1ml contains the aqueous solution of 0.1g neopelex, becomes the paste liquid of thickness behind the agitation grinding, the paste mixing material is put into be heated in advance 800 ℃ Muffle furnace, collect combustion product after combustion process (approximately about 40s) finishes, need not grinding and namely get 1.8g coralloid nano alpha-Al
2O
3Powder (theoretical value is 2.1g) does not almost have smog to produce in the combustion process.
Referring to accompanying drawing 1: it is to show by the nanometer alumina powder X diffraction analysis result that the described preparation method of present embodiment makes: [012], [104] and [113], [116] etc. diffraction maximum is more sharp-pointed by force, [110], [024], the weak diffraction maximum such as [214] and [300] is also all very obvious, with α-Al
2O
3(JCPDF 46-1212) is in full accord for the material phase analysis normal data.
Referring to accompanying drawing 2: it is the α-Al that makes by the described preparation method of present embodiment
2O
3The sem photograph of nano-powder, as seen from the figure, prepared aluminium oxide is coralliform true to nature, there are many tiny projections on the surface.
Referring to accompanying drawing 3: it is the α-Al that makes by the described preparation method of present embodiment
2O
3The transmission electron microscope image of nano-powder, as seen from the figure, prepared aluminium oxide is the porous coralliform.
Embodiment 2:
With 10gAl (NO
3)
39H
2O is dissolved in the 50ml deionized water, be made into settled solution, in solution, add 3g urea, fuel with 2g ammonium perchlorate composition, adding 1ml contains the aqueous solution of 0.1g AEO, becomes the paste liquid of thickness behind the agitation grinding, the paste mixing material is put into be heated in advance 700 ℃ Muffle furnace, collect combustion product after combustion process (approximately about 30s) finishes, need not grinding and namely get 1.1g coralloid nano alpha-Al
2O
3Powder (theoretical value is 1.3g) only discharges minute quantity smog nearly when burning finishes in the combustion process.
Embodiment 3:
With 10g Al
2(SO
4)
318H
2O is dissolved in the 50ml deionized water, be made into settled solution, in solution, add 3g urea and 2g ammonium nitrate, adding 1ml contains the aqueous solution of 0.15g APES, become the paste liquid of thickness behind the agitation grinding, the paste mixing material put into be heated in advance 850 ℃ Muffle furnace, collect combustion product after combustion process (approximately about 50s) finishes, need not to grind and namely get 1.2g coralloid nano alpha-Al
2O
3Powder (theoretical value is 1.5g) discharges a small amount of smog in the combustion process, absorb with sig water to get final product.
Claims (1)
1. coralloid nano alpha-Al
2O
3Fast preparation method, it is characterized in that:
(1) the solubility inorganic aluminate is mixed with the aluminum saline solution of 0.5～2.0mol/L;
(2) fuel is joined in the above-mentioned aqueous solution, the mass ratio of fuel and aluminium salt is 0.2～0.5: 1, adds the tensio-active agent of aluminium salt quality 0.5～1.5% again, adopts high speed machine to stir or grinding technics, makes heavy-gravity paste liquid;
(3) above-mentioned paste liquid is put into the Muffle furnace that is heated in advance 700～900 ℃ of temperature, burning is namely collected combustion product after finishing, and obtains coralloid nano alpha-Al
2O
3Powder;
Described inorganic aluminate is a kind of in aluminum nitrate, aluminum chloride and the Tai-Ace S 150 or their arbitrary combination;
Described fuel comprises a kind of in urea, ammonium sulfate, volatile salt, bicarbonate of ammonia, ammoniumper chlorate and the ammonium nitrate or their arbitrary combination;
Described surfactant is anion and the non-ionic surface active agent with foaming and thickening power.
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| CN2008100235232A CN101264913B (en) | 2008-04-03 | 2008-04-03 | Fast preparation method for coralloid nano alpha-Al2O3 |
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| CN101264913B true CN101264913B (en) | 2010-10-06 |
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| KR101913990B1 (en) | 2014-12-17 | 2018-10-31 | 스미또모 가가꾸 가부시끼가이샤 | Inorganic oxide powder, slurry containing same, nonaqueous electrolyte secondary battery, and method for manufacturing nonaqueous electrolyte secondary battery |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1439603A (en) * | 2003-01-24 | 2003-09-03 | 东北大学 | Preparation for alpha-type nanometer aluminium oxide powder by combustion synthetic method |
| DE102004027633A1 (en) * | 2004-06-05 | 2006-01-05 | Robert Bosch Gmbh | Sensor for determining the oxygen concentration in the exhaust gas of internal combustion engines |
| CN1919737A (en) * | 2005-08-26 | 2007-02-28 | 大连路明纳米材料有限公司 | Method of preparing good dispersion and high-purity ultra-fine alpha-Al2O3 |
| CN1986408A (en) * | 2006-12-22 | 2007-06-27 | 武汉大学 | Preparing process fibrous nano alumina powder |
-
2008
- 2008-04-03 CN CN2008100235232A patent/CN101264913B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1439603A (en) * | 2003-01-24 | 2003-09-03 | 东北大学 | Preparation for alpha-type nanometer aluminium oxide powder by combustion synthetic method |
| DE102004027633A1 (en) * | 2004-06-05 | 2006-01-05 | Robert Bosch Gmbh | Sensor for determining the oxygen concentration in the exhaust gas of internal combustion engines |
| CN1919737A (en) * | 2005-08-26 | 2007-02-28 | 大连路明纳米材料有限公司 | Method of preparing good dispersion and high-purity ultra-fine alpha-Al2O3 |
| CN1986408A (en) * | 2006-12-22 | 2007-06-27 | 武汉大学 | Preparing process fibrous nano alumina powder |
Non-Patent Citations (5)
| Title |
|---|
| DE 102004027633 A1,说明书第[0003]-[0008]段. |
| 朱顺官 等.溶液燃烧法制备纳米Al2O3.中国粉体技术 2.2005,(2),21-23. |
| 朱顺官等.溶液燃烧法制备纳米Al2O3.中国粉体技术 2.2005,(2),21-23. * |
| 邢存章 等.燃烧法制备铝酸锌超细粉体的研究.现代化工27 4.2007,27(4),44-45. |
| 邢存章等.燃烧法制备铝酸锌超细粉体的研究.现代化工27 4.2007,27(4),44-45. * |
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