CN1546381A - Method for preparing conglobate-free nano alpha-Al2O3 powders - Google Patents
Method for preparing conglobate-free nano alpha-Al2O3 powders Download PDFInfo
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- CN1546381A CN1546381A CNA2003101144558A CN200310114455A CN1546381A CN 1546381 A CN1546381 A CN 1546381A CN A2003101144558 A CNA2003101144558 A CN A2003101144558A CN 200310114455 A CN200310114455 A CN 200310114455A CN 1546381 A CN1546381 A CN 1546381A
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Abstract
The invention provides a process for preparing agglomeration-proof nano alpha-Al2O3 powder which comprises, dispersing nano carbon black completely in inorganic aluminium salt solution whose concentration is 0.5-3.0 mol/L, then charging alkaline liquor with a finite concentration slowly in reaction field with turbulent motion, controlling the pH of the final reaction liquid between 5.0-8.0, depositing 7-12 hours after end of reaction, filtering and scouring, processing the filter cake 1-3 hours in 1000 deg. C to 1200 deg. C inert gas furnace, calcining in 600 deg. C to 800 deg. C air tank for removing the surface coating, thus obtaining alpha-Al2O3 powder.
Description
Technical field
The present invention relates to a kind of no-agglomeration nano α-Al
2O
3The preparation method of powder belongs to field of inorganic material preparing technology.
Background technology
Nano material is the field of new that grows up the beginning of the eighties in last century, because superfine crystal grain and a large amount of atoms that is in crystal boundary and intragranular defect center, make nano material on physical and chemical performance, show the greatest differences with the micron order material, have peculiar performance and wide application prospect, caused the very big concern of scientific circles and business circles.Nanometer Al wherein
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 a kind of most widely used, nano material that demand is the most urgent.Nanometer Al
2O
3Multiple crystal formation is arranged, and in actual applications, mostly need the nanometer Al of high content of alpha phase
2O
3Powder, traditional nanometer Al
2O
3Because the α phase content is few, have a strong impact on its sintering character and application performance in the powder, therefore the nanometer Al of high α phase content
2O
3Powder becomes demand.
Relevant preparation α-Al on the present 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 etc. are arranged, because solid phase and gas phase synthesis method exist cost height, granularity to be difficult to the shortcomings such as control mostly, at present many researchs of the current nano aluminium oxide developing direction of representative are reported, mostly adopt sol-gel process and the sluggish precipitation of liquid phase method.These two kinds of methods are used for preparing the nanometer γ of small particle diameter-Al
2O
3Powder has had the technology of comparative maturity, but wants to prepare the nanometer α of small particle diameter, narrow distribution-Al
2O
3But relatively more difficult, its reason is γ-Al
2O
3Therefore must at high temperature just can change the α phase into, hard aggregation very easily takes place in particle in the phase inversion process, is difficult to obtain the nanometer α of narrowly distributing-Al
2O
3Powder, and the homogeneity of nano particle is the key of applications well performance.How to prepare the nanometer α that small particle diameter, narrow distribution, good dispersion, nothing reunite-Al
2O
3It is the target that researcher is made great efforts in the world wide always.
JP-A-03-080106 has reported a kind of aluminium chloride high-temperature calcination, although can make the nanometer Al of 50nm～200nm
2O
3Powder can only reach 70% but the α phase content is the highest, and the size distribution inequality, does not satisfy application requirements.EP1262457A2 has also reported a kind of method, adopts this method can produce the higher nanometer Al of α phase content of 10～100nm
2O
3Powder.But this method need be selected crystal seed, and presoma need calcine in being full of the HCl medium, can cause corrosion to equipment, in addition, the growing up of crystal grain in the calcination process also needs to add crystal grain accretion inhibitor, and last gained powder also needs further to mill.The people such as Wu Yiquan have introduced a kind of doping and introduce the method for crystal seed in xerogel, but this method needs ball milling 24h, and dry 12h at a certain temperature behind the ball milling, last gained α-Al
2O
3Particle diameter is bigger, skewness, because the introducing of additive, the pattern of part crystal grain is long column shape.
Goal of the invention
The invention solves employing nanometer medium and inorganic aluminate raw material cheap and easy to get in special reacting field, by simple process conditions prepare that particle diameter is little, narrowly distributing, nothing are reunited nanometer α-Al
2O
3Powder.
The present invention realizes by following scheme, no-agglomeration nano α-Al
2O
3The preparation method of powder, 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, wash, filter cake was processed 1～3 hour in 1000～1200 ℃ inert gas retort, in 600～800 ℃ air retort, be fired to surperficial coating and eliminate, the α-Al that need not mill and namely get 30～60nm, be evenly distributed, do not have reunion
2O
3Powder.
Aluminium salt of the present invention is Al (NO
3)
3, Al
2(SO
4)
3, Al
2(NH
4)
2(SO
4)
4, aluminium alcoholates or its mixture, solution concentration is 0.5～3.0mol/L, solvent is ethanol, water, cyclohexane or its mixture.
Reacting field of the present invention is the fluid with turbulence effect, can pass through ultrasonic wave, mechanical agitator or air-flow stirring device and realize.
Alkaline agent of the present invention is urea, ammoniacal liquor, sodium hydroxid, potassium hydroxide, and the mol ratio of alkaline agent add-on and aluminium salt is 2～5: 1.
Rare gas element of the present invention is nitrogen, argon gas.
No-agglomeration nano α-Al
2O
3The preparation method of powder, in the fluid reaction field of turbulence effect, to adopt adsorbing medium porous powdered carbon, network molecule sieve or dextrin class, aluminium salt hydrolysis product is coated or absorption, pass through then suction filtration, washing, alcohol wash, filter cake heats phase inversion in inert gas, the precipitation surface coating is removed in calcining in air, gets the nanometer α of loose shape 30～50nm-Al
2O
3Powder.
The present invention is dispersed in specific adsorbing medium in the special reacting field, thereby form special reaction system, then certain density aluminum saline solution is joined in the above-mentioned reaction system, slow dripping alkali liquid, the pH value of control reactant liquor, nano adsorption medium in hydrolysate and the system is fully coated or adsorb, react and leave standstill after complete, filter then, wash, filter cake is high-temperature process in being full of the retort of inert gas, in air, be fired to then surperficial coating and eliminate, namely get loose shape α-Al
2O
3Powder.
Aluminium salt of the present invention is Al (NO
3)
3, Al
2(SO
4)
3, Al
2(NH
4)
2(SO
4)
4, aluminium alcoholates or its mixture, solution concentration is 0.5～3.0mol/L.
Reacting field of the present invention is the fluid with turbulence effect, can pass through ultrasonic wave, mechanical agitator or air-flow stirring device and realize.
Alkaline agent of the present invention is urea, ammoniacal liquor, sodium hydroxid, potassium hydroxide, and the mol ratio of alkaline agent add-on and aluminium salt is 2～5: 1.
Heat-treatment temperature range of the present invention is 1000～1200 ℃.
Rare gas element of the present invention is nitrogen, argon gas.
Calcining temperature of the present invention is 500～700 ℃.
Beneficial effect of the present invention and advantage:
1, the nanometer medium in the special reaction field is adsorbable or be coated on the hydrolysate surface, weaken the attraction between precipitation particles, the reunion that precipitates in the hydrolytic process and the mass transport process in the postorder high-temperature heat treatment phase inversion have been stoped, crystal grain is reunited and growth thereby reduced, and is not nano-powder so that product need not be milled simultaneously.
2, gained powder α phase content height, particle diameter is little, is evenly distributed.
3, owing to cheap raw materials such as use inorganic salt, and technology is simple and easy to control, suitability for scale production.
Particle size analysis the results are shown in Table 1, from test result as can be seen, the particle size distribution 40.6～41.9mm of product, the prepared powder granule size that goes out is even, and it is very narrow to distribute.
Table 1 is α-Al
2O
3Diameter of particle analytical test result
Description of drawings
Fig. 1 is α-Al
2O
3The powder transmission electron microscope picture
Fig. 2 is that X diffraction analysis result is pure α phasor
Below by embodiment the present invention is further described, present embodiment is to be used for illustrating of the present invention, rather than the present invention is carried out any restriction.
Embodiment 1:
2g is adopted in the aluminum nitrate ethanolic solution of the standby ultrasonic 1.5mol/L of being distributed to of nano carbon black of lamp legal system, be 20kHz in frequency then, power is slowly to add 20% sodium hydrate aqueous solution under the ul-trasonic irradiation of 300W, reaction is 2 hours under the room temperature, controls end reaction liquid pH value about 6.5, precipitation 8 hours, filter then, wash, the gained filter cake was processed 3 hours in 1100 ℃ of retorts that are full of nitrogen, and calcining is 1 hour in 700 ℃ air, can obtain loose shape α-Al
2O
3Powder.
Particle size analysis the results are shown in Figure 1; X diffraction analysis result is pure α phase, as shown in Figure 2; Transmission electron microscope as shown in Figure 3.
Embodiment 2:
Adopt the nano carbon black ultra-sonic dispersion of lamp method preparation in the aluminum nitrate ethanolic soln of 1.5mol/L 2g, the aqueous sodium hydroxide solution of slow adding 20% under the high speed machine stirring action, reaction is 2 hours under the room temperature, control end reaction liquid pH value is about 6.5, heavyization 8 hours, filter then, wash, the gained filter cake was handled 3 hours in 1100 ℃ of retorts that are full of nitrogen, calcining is 1 hour in 700 ℃ air, the gained diameter of particle is 51.2nm, white powder, X diffraction analysis result is pure alpha-phase aluminum oxide.
Embodiment 3:
Adopt the nano carbon black ultra-sonic dispersion of lamp method preparation in the exsiccated ammonium alum alcohol solution of 2.0mol/L 2g, the sodium hydroxide solution of slow adding 30% under the air-flow stirring action, the pH value of control end reaction liquid is about 7.5, reaction is 2 hours under the room temperature, control end reaction liquid pH value is about 6.5, heavyization 8 hours, filter then, wash, the gained filter cake was handled 3 hours in 1100 ℃ of retorts that are full of nitrogen, calcining is 1 hour in 700 ℃ air, the gained diameter of particle is 59.5nm, white powder, and X diffraction analysis result is pure alpha-phase aluminum oxide.
Claims (5)
1, a kind of no-agglomeration nano α-Al
2O
3The preparation method of powder, 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, wash, filter cake was processed 1～3 hour in 1000～1200 ℃ inert gas retort, in 600～800 ℃ air retort, be fired to surperficial coating and eliminate, the α-Al that need not mill and namely get 30～60nm, be evenly distributed, do not have reunion
2O
3Powder.
2, no-agglomeration nano α-Al according to claim 1
2O
3The preparation method of powder is characterized in that described aluminium salt is Al (NO
3)
3, Al
2(SOAl
2(NH
4)
2(SO
4)
4, aluminium alcoholates or its mixture, solvent is ethanol, water, cyclohexane or its mixture.
3, no-agglomeration nano α-Al according to claim 1
2O
3Powder preparation method is characterized in that described reacting field is the fluid with turbulence effect, can pass through ultrasonic wave, mechanical agitator or air-flow stirring device and realize.
4, no-agglomeration nano α-Al according to claim 1
2O
3The preparation method of powder is characterized in that alkaline agent is urea, ammoniacal liquor, sodium hydroxid, potassium hydroxide, and the mol ratio of alkaline agent addition and aluminium salt is 2～5: 1.
5, no-agglomeration nano α-Al according to claim 1
2O
3Powder preparation method is characterized in that inert gas is nitrogen, argon gas.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310114455 CN1288085C (en) | 2003-12-09 | 2003-12-09 | Method for preparing conglobate-free nano alpha-Al2O3 powders |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310114455 CN1288085C (en) | 2003-12-09 | 2003-12-09 | Method for preparing conglobate-free nano alpha-Al2O3 powders |
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|---|---|
| CN1546381A true CN1546381A (en) | 2004-11-17 |
| CN1288085C CN1288085C (en) | 2006-12-06 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107140677A (en) * | 2017-06-05 | 2017-09-08 | 苏州大学 | A kind of preparation method of function element metal oxide nanoparticles |
-
2003
- 2003-12-09 CN CN 200310114455 patent/CN1288085C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107140677A (en) * | 2017-06-05 | 2017-09-08 | 苏州大学 | A kind of preparation method of function element metal oxide nanoparticles |
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