CN1948155A - Preparation method of mono dispersion nano-alpha aluminium oxide particle powder - Google Patents
Preparation method of mono dispersion nano-alpha aluminium oxide particle powder Download PDFInfo
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- CN1948155A CN1948155A CN 200610104871 CN200610104871A CN1948155A CN 1948155 A CN1948155 A CN 1948155A CN 200610104871 CN200610104871 CN 200610104871 CN 200610104871 A CN200610104871 A CN 200610104871A CN 1948155 A CN1948155 A CN 1948155A
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Abstract
The present invention discloses a preparation method of monodisperse agglomeration-free alpha-alumina granule powder body. Said preparation method includes the following steps: adding auxiliary isolation phase of water-soluble salt in aluminium salt solution, then adding alpha-alumina crystal seed and hydrophilic surfactant into said system, stirring to make the hydrophilic surfactant be fully dissolved, then slowly drop-adding alkaline aqueous solution into said reaction liquor, after the reaction is completed, making said reaction system undergo the process of homogenization treatment, drying, grinding, mixing and calcining at 950-1100 deg.C so as to obtain the invented monodisperse alpha-alumina nano granule powder body whose grain size is 10-30 nm.
Description
Technical field
Single preparation method who disperses the no-agglomeration nano alpha aluminium oxide particle powder that use in the fields such as a kind of pottery, catalyzer, electronic industry, coated material, biomedicine and optical material that the present invention relates to.
Background technology
Do not have the requisite raw material that the nano-alpha aluminium oxide particle powder of reuniting is preparation high-compactness, fine grain nano-alpha aluminium oxide pottery single the dispersion.Because the chemical stability of nano-alpha aluminium oxide uniqueness and heat, electricity, optical property have important using value in a lot of fields.Alpha-alumina is the stable structure of aluminum oxide thermodynamics, generally is to adopt aluminium hydroxide or transition aluminas to make through the high-temperature calcination more than 1100 ℃, but can produces hard aggregation inevitably when high-temperature calcination.At present, technologies such as chemical vapour deposition, liquid phase sol-gel method, chemical precipitation method and solid phase decomposition by combustion are adopted in the preparation of Alpha-alumina more.Wherein reaction condition can be accurately controlled in chemical vapour deposition (CVD), under the different operating condition, obtain different grain size and pattern, disperse preferably nano-powder, but cost height, productive rate low, be difficult to realize industrial scale production.Sol-gel method can make the high pure and ultra-fine powder, but the cost of material height, organic solvent is poisonous and can form hard aggregation during pyroprocessing.Solid phase method is easy to suitability for industrialized production, but pyrolytic process easily causes the hard aggregation of powder.The chemical precipitation preparation method of commonly using at present, its technology is simple, cost is low, be fit to suitability for industrialized production, but has serious hard aggregation problem.
Chinese invention patent application 200310114455.8 discloses a kind of no-agglomeration nano α-Al
2O
3The preparation method of powder, it is that nano carbon black is well dispersed in the inorganic aluminum salting liquid that concentration is 0.5～3.0mol/L, then in the reacting field with turbulence effect, slowly add certain density alkali lye, the pH value of control end reaction liquid is 5.0～8.0, reacted complete rear precipitation 7～12 hours, filter then, washing, filter cake was processed 1～3 hour in 1000～1200 ℃ inert gas retort, be fired to surperficial coating and eliminate in 600～800 ℃ air retort, obtaining need not mill is 30～60nm, be evenly distributed, there is not the α-Al that reunites
2O
3Powder.Therefore this patent will guarantee its action effect owing to be that the undissolvable nano carbon black of employing is dispersant, and the dispersion in reaction solution requires just especially high to carbon black in preparation process.The preparation cost of this technology is also with higher on the other hand.
Summary of the invention
The invention provides and a kind ofly can overcome the prior art deficiency, by at lower cost and comparatively simple technology obtain the method for mono dispersion nano-alpha aluminium oxide particle powder material.
Method of the present invention is to be the auxiliary isolation phase of adding water-soluble salt in 0.005～0.1mol/l aluminum salt solution in the aluminum ion volumetric molar concentration, the mol ratio of water-soluble salt and aluminium salt is 10≤m≤80, make the auxiliary fully dissolving in aluminum salt solution of isolating through stirring, in system, add the hydrophilic surfactant active again by 0.5～1.0g/100ml (aluminum salt solution), after fully dissolving the hydrophilic surfactant active, stirring in reaction liquid, slowly splashes into the aqueous solution of alkali again, the final pH value that makes system is 8.5～10, after reaction is finished to the reaction system processing that homogenizes, carry out drying treatment again, the gained powder is carried out ground and mixed again, powder after ground and mixed is calcined at 950～1100 ℃, obtained single Alpha-alumina nano particle powder that disperses not have reunion 10～30nm.
The concept of method of the present invention is to be converted into α-Al for fear of aluminium oxide in calcination process from transitional face
2O
3Phase time forms hard aggregation, and aluminium oxide is converted into the process of α phase from transitional face when calcining, utilizes the auxiliary isolation of water soluble salt that aluminum oxide nanoparticle is kept apart mutually, thereby has avoided Al
2O
3Hot polymerization took place or forms the sintering neck and the hard aggregation problem that causes in when calcining in nano particle, had guaranteed the α-Al that obtains
2O
3No reunion monodispersity.
Among the present invention, as in reaction system, adding again α-Al of 1～3% that its amount of substance is aluminium salt amount of substance after fully dissolving at auxiliary isolation decentralized photo
2O
3Crystal seed.α-Al
2O
3Crystal seed is provided as epipole, has reduced transition state of alumina to α-Al
2O
3The conversion potential barrier, thereby reduce α-Al
2O
3Formation temperature.
Method optimum controling range of the present invention is: aluminum ions volumetric molar concentration is 0.01～0.05mol/l in the reaction system, the water-soluble salt that adds and the mol ratio of aluminium salt are 20～60, the crystal seed amount of substance that is added is 1.5～2.5% of an inorganic aluminate amount of substance, and the tensio-active agent that is added can be PEG200 and PEG100 (polyoxyethylene glycol, Polyethylene Glycol, HO (CH
2CH
2O)
nH) with the mixture that is combined to form of arbitrary proportion.Aluminium salt used in the present invention is preferably Al (NO
3)
3, the water soluble salt that adds is sodium chloride or potassium chloride, and used aqueous alkali is ammoniacal liquor, and the final pH value of reaction system is 9.
Test shows that the auxiliary isolation adopted in the method for the present invention and the ratio of the amount of substance of aluminium oxide are necessary conditions, because the auxiliary isolation phase of mixing does not have good isolation effect very little, to such an extent as to can not obtain monodispersed alpha-alumina nano powder; The auxiliary isolation of mixing can take place too much mutually serious two and be separated when high temperature, being separated to cause the alligatoring of part nano particle, to cause the product granularity inhomogeneous.When if aluminium ion concentration is excessive among the present invention in addition, cause reunion in the easy collision of the aluminum hydroxide particles of precipitation process high density; But aluminium ion concentration is crossed the young pathbreaker and is unfavorable for producing in batches.The auxiliary isolation of dry run general easier separating out mutually, so that auxiliary isolation is not even the mixing with alumina precursor two solid phases, so want ground and mixed to make after the drying to assist to isolate to mix with alumina precursor is full and uniform.
Advantage of the present invention is:
(1) in the chemical precipitation process owing to introduce chemically stable auxiliary isolation phase, and because isolation is water soluble salt mutually, in water, be easy to dissolving, therefore can be so that the precursor of preparing---the hydroxide particles of aluminium is assisted isolation to keep apart admirably mutually, the contact of the aluminum oxide nanoparticle that has generated when having avoided calcining has suppressed Al
2O
3Hot polymerization took place or forms the sintering neck and the agglomeration traits that causes in when calcining in nano particle, thereby had guaranteed the α-Al that obtains
2O
3Monodispersity.
(2) and the used auxiliary degree of scatter of isolating in reaction system of the present invention to be far superior to the degree of scatter of nano carbon black powder in reaction system of available technology adopting, when the while does not need to react system is not carried out special dispersion treatment.
(3) whole technological process is simple, and cost is low, and is pollution-free, and equipment is not had particular requirement, can large-scale production.
(4) whole technological process is easy to regulate control condition, also is easy to control granularity, dispersiveness and the thing phase of product.
(5) obtained nano particle is spherical in shape, single dispersion, narrow diameter distribution
Description of drawings
Accompanying drawing 1 is the X diffraction spectra by the embodiment final product of the inventive method preparation.
Accompanying drawing 2 is the selected area electron diffraction by the embodiment final product of the inventive method preparation.
Accompanying drawing 3 is the shape appearance figure by the transmission electron microscope of the embodiment final product of the inventive method preparation.
Embodiment
One embodiment of the present of invention below are provided:
1. weigh the Al (NO that gets 11.2539g in the balance
3)
39H
2The NaCl of O and 70.128g dissolves in it in 300ml deionized water, and aluminum ions molar concentration is 0.01mol/l in the solution, NaCl and Al (NO
3)
3The ratio of amount of substance is 40, constantly stirs, and after the dissolving, removes by filter exogenous impurity fully;
2. α-the Al that adds 0.0765g in the mentioned solution
2O
3Crystal seed is used magnetic stirrer 30 minutes, and broken 10 minutes of ultrasonic echography makes α-Al
2O
3Crystal seed is dispersed in the mixed liquor;
3. add Surfactant PEG 200 and each 0.75g of PEG1000, continue to be stirred to PEG and dissolve fully;
4. with the quick above-mentioned mixed solution that stirs of strong aqua titration, it is muddy to oyster white that the about 2ml/min of its titration speed, mixed solution become, and the final pH value of system is 9;
5. system homogenizes: magnetic agitation, ageing;
6. dry, grinding;
7. at 1000 ℃ of calcining 5h;
8. burnt sample is used deionized water eccentric cleaning 5 times and dehydrated alcohol eccentric cleaning 3 times, and used AgNO
3Whether the auxiliary phase ion in the solution check sample cleans up.
Through the X-ray diffraction spectrum of above processing gained sample, see Fig. 1, its diffraction spectra turns out to be product α-Al
2O
3Referring to Fig. 2, show that the product that obtains is α-Al through the SEAD (SAED) of above processing gained sample
2O
3Monocrystalline; Referring to Fig. 3, showing does not have the α-Al that reunites resultant the dispersion for 10nm is single through the shape appearance figure of above processing gained sample transmission electron microscope (TEM)
2O
3Nano particle.
Claims (4)
1, a kind of preparation method of mono dispersion nano-alpha aluminium oxide particle powder, the aqueous solution liquid that splashes into alkali in the inorganic aluminate aqueous solution is reacted, after finishing, reaction carries out drying treatment, the gained solid is calcined, again the solid after calcination processing is cleaned, obtain the mono-dispersed nano Alpha-alumina, it is characterized in that aluminum ions volumetric molar concentration is 0.005～0.1mol/l in the aluminum salt solution, the auxiliary isolation phase that in aluminum saline solution, adds water-soluble salt, the mol ratio of water-soluble salt and aluminium salt is 10≤m≤80, make the auxiliary fully dissolving in aluminum salt solution of isolating through stirring, in system, add the hydrophilic surfactant active again by 0.5～1.0g/100ml (aluminum salt solution), after fully dissolving the hydrophilic surfactant active, stirring in reaction liquid, slowly splashes into the aqueous solution of alkali again, the final pH value that makes system is 8.5～10, to the reaction system processing that homogenizes, carry out drying treatment again, the gained powder is carried out ground and mixed again, powder after powder floods is calcined at 950～1100 ℃, obtained single nano particle that disperses Alpha-alumina.
2, the preparation method of mono dispersion nano-alpha aluminium oxide particle powder according to claim 1 is characterized in that adding α-Al in reaction system after auxiliary isolation decentralized photo fully dissolves again
2O
3Crystal seed, the crystal seed amount that adds are 1～3% of aluminium salt amount of substance.
3, the preparation method of mono dispersion nano-alpha aluminium oxide particle powder according to claim 2, it is characterized in that aluminum ions volumetric molar concentration is 0.01～0.05mol/l in the reaction system, the water-soluble salt that adds and the mol ratio of aluminium salt are 20～60, the crystal seed amount that is added is 1.5～2.5% of an inorganic aluminate molecular weight, and the tensio-active agent that is added is PEG200 and the PEG1000 mixture with the combination of arbitrary proportion.
4, according to the preparation method of the described mono dispersion nano-alpha aluminium oxide particle powder of claims 1 to 3, it is characterized in that used aluminium salt is Al (NO
3)
3, the water soluble salt that adds is sodium chloride or potassium chloride, and used aqueous alkali is ammoniacal liquor, and the final pH value of reaction system is 9.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101456568B (en) * | 2008-12-25 | 2010-12-15 | 中国计量学院 | Method for synthesizing nano alumina powder |
| CN103570049A (en) * | 2013-11-12 | 2014-02-12 | 兰州大学 | Method for preparing completely dispersed alpha aluminum oxide nano particles |
| CN106044816A (en) * | 2016-05-26 | 2016-10-26 | 东南大学 | Method for preparing monodispersion nanometer alpha aluminum oxide |
| CN106044810A (en) * | 2016-05-26 | 2016-10-26 | 东南大学 | Salt-shelled nano compound particles and preparation method thereof |
| CN109772289A (en) * | 2019-02-28 | 2019-05-21 | 江苏国盛新材料有限公司 | A kind of preparation method of lanthanum modified aluminas |
| CN110282644A (en) * | 2019-04-25 | 2019-09-27 | 中南大学 | A kind of preparation method of ultra-fine aluminum oxide |
| RU2770921C1 (en) * | 2021-12-24 | 2022-04-25 | Федеральное государственное автономное образовательное учреждение высшего образования "Белгородский государственный национальный исследовательский университет" (НИУ "БелГУ") | Method for producing finely dispersed activated alpha-aluminum oxide |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6027706A (en) * | 1998-05-05 | 2000-02-22 | Board Of Trustees Operating Michigan State University | Porous aluminum oxide materials prepared by non-ionic surfactant assembly route |
| US7090824B2 (en) * | 2001-07-27 | 2006-08-15 | Board Of Trustees Of Michigan State University | Mesostructured transition aluminas |
| US7211238B2 (en) * | 2003-03-12 | 2007-05-01 | Abb Lummus Global Inc. | Mesoporous aluminum oxide, preparation and use thereof |
| CN1250455C (en) * | 2003-09-26 | 2006-04-12 | 华东理工大学 | Method for preparing light temperature-resistance high surface area alumina and aluminiferous composite oxide |
| TWI304395B (en) * | 2004-11-26 | 2008-12-21 | Ind Tech Res Inst | A method for fabricating a high specific surface area mesoporous alumina |
-
2006
- 2006-11-02 CN CNB2006101048713A patent/CN100427395C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101456568B (en) * | 2008-12-25 | 2010-12-15 | 中国计量学院 | Method for synthesizing nano alumina powder |
| CN103570049A (en) * | 2013-11-12 | 2014-02-12 | 兰州大学 | Method for preparing completely dispersed alpha aluminum oxide nano particles |
| CN103570049B (en) * | 2013-11-12 | 2015-07-15 | 兰州大学 | Method for preparing completely dispersed alpha aluminum oxide nano particles |
| CN106044816A (en) * | 2016-05-26 | 2016-10-26 | 东南大学 | Method for preparing monodispersion nanometer alpha aluminum oxide |
| CN106044810A (en) * | 2016-05-26 | 2016-10-26 | 东南大学 | Salt-shelled nano compound particles and preparation method thereof |
| CN109772289A (en) * | 2019-02-28 | 2019-05-21 | 江苏国盛新材料有限公司 | A kind of preparation method of lanthanum modified aluminas |
| CN110282644A (en) * | 2019-04-25 | 2019-09-27 | 中南大学 | A kind of preparation method of ultra-fine aluminum oxide |
| RU2770921C1 (en) * | 2021-12-24 | 2022-04-25 | Федеральное государственное автономное образовательное учреждение высшего образования "Белгородский государственный национальный исследовательский университет" (НИУ "БелГУ") | Method for producing finely dispersed activated alpha-aluminum oxide |
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| CN100427395C (en) | 2008-10-22 |
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