CN105984891A - Method for preparing nano aluminum oxide at low temperature - Google Patents
Method for preparing nano aluminum oxide at low temperature Download PDFInfo
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- CN105984891A CN105984891A CN201510054602.XA CN201510054602A CN105984891A CN 105984891 A CN105984891 A CN 105984891A CN 201510054602 A CN201510054602 A CN 201510054602A CN 105984891 A CN105984891 A CN 105984891A
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Abstract
The invention discloses a method for preparing nano aluminum oxide at a low temperature. The method comprises the steps of: adding a seed crystal, adopting a two-step hydrolysis method, and adding glucose and polyvinylpyrrolidone respectively as a dispersant before and after hydrolysis, wherein the mass fraction of the seed crystal is 2-5%, the molar concentration of aluminum isopropoxide is 0.5-1.5mol/L, the concentration of the glucose is 0.5-1.5g/ml, and the concentration of the polyvinylpyrrolidone is 0.05-0.1g/ml; performing solvent evaporation on the obtained solution in a draught cupboard, and performing drying for 2-5h at a temperature of 100-200 DEG C after all the solvent in the solution is evaporated so as to form a loose precursor; and in an air atmosphere, performing high-temperature calcination on the dried precursor to obtain high-purity nano aluminum oxide powder. The method disclosed by the invention has the advantages of simple operation, short required period, and good repeatability, thereby facilitating implementation of industrialization. A crystal form transformation temperature (1000 DEG C) required by [alpha]-Al2O3 is relatively low, and the prepared aluminum oxide is small in particle size (smaller than 50nm) and good in dispersity.
Description
Technical field
The present invention relates to a kind of low temperature and prepare nano alumina powder jointed method, belong to field of material preparation.
Background technology
Nano aluminium oxide makes it show due to skin effect, quantum size effect, small-size effect and macro quanta tunnel effect
Optical, electrical, magnetic, heat not available for conventional material and mechanical performance are shown, be widely used in space flight and aviation, metallurgy,
The high-tech areas such as chemical industry, pottery, electronics, national defence and nuclear technology thereof.Prepare nano alumina powder jointed method master at present
Solid phase method to be divided into, liquid phase method and vapor phase method.Solid phase method includes: mechanical attrition method, high-temperature solid phase reaction method, salt divide
Solution and combustion method etc.；Vapor phase method includes: vapor condensation method, chemical vapour deposition technique etc.；Liquid phase method includes: the sedimentation method,
Sol-gel process, hydro-thermal method, phase transfer separation process, nebulization and solvent volatile matter solution etc..Solid phase method is readily incorporated
Impurity, and obtained diameter of particle is difficult to reach Nano grade；Vapor phase method is huge due to equipment, and apparatus expensive etc. lacks
Point limits it and uses；So far, the research that liquid phase method is prepared nano aluminium oxide is the most, obtained powder body
There is particle diameter little, the advantage such as good dispersion.
Jiang Li et al. (Ceramics International.2006,32,587 591) is with Al (NO3)3With citric acid as former
Material, uses sol-gel process to prepare citric acid presoma, can be prepared by α-Al at 1000 DEG C2O3But, the method
α-the Al obtained2O3Diameter of particle is relatively big, about 200nm, and dispersibility is not fine.Fu Gao feng et al.
(ceramics international, 2010,36,1253-1257) is by adding AlF in alumina precursor3Crystal seed,
Both α-Al can have been prepared at 900 DEG C2O3, in the method, α-Al2O3Crystal conversion temperature decreases, but, experiment
During do not add any dispersant, obtained sample particle diameter is relatively big, about 500nm, and poor dispersion.Upper
State in two kinds of methods, α-Al2O3Crystal conversion temperature decreases, but α is-Al2O3Particle diameter is the biggest, not up to receives
Meter level is other.
Summary of the invention
It is an object of the invention to provide a kind of method that low temperature prepares nano aluminium oxide.
The technical scheme is that a kind of method that low temperature prepares nano aluminium oxide, use following steps to prepare:
1. configuration aluminum isopropylate. solution, adds α-Al2O3Powder body crystal seed, is uniformly mixed, wherein, and α-Al2O3Powder body is brilliant
Plant the 2%-5% that quality is aluminum isopropylate. quality；
2. two-step hydrolysis, adds the glucose solution of 1/3 in above-mentioned solution, stirs 0.5-1h at a temperature of 80-82 DEG C,
Adding remaining glucose solution, stir 3-5h the temperature of 80-82 DEG C, wherein, glucose concentration is
0.5-1.5g/ml, solvent is water, and wherein water is 3:1 with the ratio of the amount of the material of aluminum isopropylate.；
3. in above-mentioned solution, add polyvinylpyrrolidonesolution solution, stir 4-8h, wherein, polyethylene the temperature of 80-82 DEG C
Pyrrolidone solution concentration is 0.05-0.1g/ml, and solvent is the quality of isopropanol, polyvinylpyrrolidone and aluminum isopropylate.
Ratio be 1:15；
4. by the evaporation of gained solution at room temperature solvent completely, it is dried at a temperature of 100-200 DEG C to moisture and evaporates completely, shape
Become loose presoma；
5. calcining heat treatment after being ground by presoma in atmosphere, calcining heat treatment cools to room temperature with the furnace after completing, obtains
α-Al2O3Powder body.
Step 1. in, the molar concentration of aluminum isopropylate. solution is 0.5-1.5mol/L, and its solvent is the mixed of toluene and isopropanol
Closing solution, wherein, the volume ratio of toluene and isopropanol is 3:1, α-Al2O3Particle diameter < the 100nm of powder body crystal seed.
Step 4. described in drying time be 2h-5h.
Step 5. described in time of heat treatment be 2h-5h, heat treatment temperature is 1000-1200 DEG C, and heating rate is 5 DEG C
/min。
This method is prepared with other compared with method of nano aluminium oxide, has the advantages that
1. the present invention uses two step hydrolysis method, by adding crystal seed, and is separately added into different dispersion before and after metal alkoxide hydrolyzes
Agent obtains uniform particle sizes, the nano aluminium oxide of good dispersion；
2. the present invention is simple to operate, and the described cycle is short, and repeatability is high, it is simple to realize industrialized production；
3. aluminium oxide crystal conversion temperature is relatively low, is 1000 DEG C；
4. the diameter of particle prepared is little, less than 50nm, good dispersion；
5. preparation process is not introduced into other inorganic impurities, prepares powder purity high.
Accompanying drawing explanation
Fig. 1 is the experiment flow figure of the present invention.
Fig. 2 is α-Al in the embodiment of the present invention 12O3The X-ray diffractogram of powder body.
Fig. 3 is α-Al in the embodiment of the present invention 12O3The scanning electron microscope diagram sheet of powder body.
Fig. 4 is α-Al in the embodiment of the present invention 12O3The transmission electron micrograph of powder body.
Fig. 5 is α-Al in the embodiment of the present invention 22O3The scanning electron microscope diagram sheet of powder body.
Fig. 6 is α-Al in the embodiment of the present invention 32O3The X-ray diffractogram of powder body.
Fig. 7 is α-Al in the embodiment of the present invention 32O3The scanning electron microscope diagram sheet of powder body.
Fig. 8 is α-Al in the embodiment of the present invention 32O3The transmission electron micrograph of powder body.
Detailed description of the invention
Embodiment 1: α-Al2O3The preparation of powder body
The toluene of 54ml and the isopropanol of 18ml are stirred at 80-82 DEG C, weighs 15g aluminum isopropylate. and 0.75g
α-Al2O3Powder body, joins in above-mentioned mixed solvent, and stirring treats that aluminum isopropylate. is completely dissolved, and forms solution A, weighs
4.5g glucose, joins in the middle of 4.5ml deionized water, and at 80-82 DEG C, stirring makes it dissolve, and forms B solution,
The B solution taking 1/3 joins in the middle of above-mentioned solution A, after stirring reaction 30min, is slowly added to remaining B solution,
Continue stirring 4h, form C solution, weigh 1g polyvinylpyrrolidone, join in the isopropanol of 20ml, at 80-82 DEG C
Lower stirring, to dissolving, forms solution D, solution D is added slowly in the middle of C solution, continues stirring 4h.By institute
Obtain solution to be placed in fume hood, after its solvent evaporates completely, at 110 DEG C, be dried 2h so that it is moisture evaporates completely,
Obtain the presoma loosened.To be dried during presoma is put in corundum crucible completely and corundum crucible is put in
In KSL-1400X-A4 type Muffle furnace, heating rate is set as 5 DEG C/min.It is warming up to 1000 DEG C, protects at such a temperature
Temperature 2h, Muffle furnace starts cooling subsequently, and in the temperature range of 1000 DEG C to 500 DEG C, it is 10 that rate of temperature fall controls
K/min.When temperature reduces to less than 500 DEG C, rate of temperature fall is about 5 DEG C/min.When temperature reduces to room temperature, close Muffle furnace,
Take out product.The result of X-ray diffraction analysis (Fig. 2) shows, the diffraction maximum of obtained sample and α-Al2O3Mark
Quasi-card fits like a glove, without other miscellaneous peak.Scanning electron microscope (Fig. 3) and transmission electron microscope (Fig. 4) show
Made α-the Al obtained2O3Diameter of particle is less, < 50nm, and dispersibility is preferable, and hard aggregation is inconspicuous.
Changing the reaction temperature in embodiment 1, other parameters keep constant, when reaction temperature is less than 80 DEG C, and isopropanol
Aluminum dissolves not exclusively, the α-Al prepared2O3Particle diameter is uneven, when reaction temperature is higher than 82 DEG C, can cause solvent
Evaporation, in course of reaction pressed powder separate out, the α-Al prepared2O3Particle diameter is relatively big and uneven.
Embodiment 2: α-Al2O3The preparation of powder body
The toluene of 54ml and the isopropanol of 18ml are stirred at 80-82 DEG C, weighs 15g aluminum isopropylate. and 0.50g
α-Al2O3Powder body, joins in above-mentioned mixed solvent, and stirring treats that aluminum isopropylate. is completely dissolved, and forms solution A, weighs
4.5g glucose, joins in the middle of 4.5ml deionized water, and at 80-82 DEG C, stirring makes it dissolve, and forms B solution, takes
The B solution of 1/3 joins in the middle of above-mentioned solution A, after stirring reaction 30min, is slowly added to remaining B solution, continues
Continuous stirring 4h, forms C solution, weighs 1g polyvinylpyrrolidone, join in the isopropanol of 20ml, at 80-82 DEG C
Lower stirring, to dissolving, forms solution D, solution D is added slowly in the middle of C solution, continues stirring 4h. by gained
Solution is placed in fume hood, after its solvent evaporates completely, is dried 2h so that it is moisture evaporates completely at 110 DEG C,
To loose presoma.To be dried during presoma is put in corundum crucible completely and corundum crucible is put in
In KSL-1400X-A4 type Muffle furnace, heating rate is set as 5 DEG C/min.It is warming up to 1000 DEG C, protects at such a temperature
Temperature 2h, Muffle furnace starts cooling subsequently, and in the temperature range of 1000 DEG C to 500 DEG C, it is 10 DEG C that rate of temperature fall controls
/min.When temperature reduces to less than 500 DEG C, rate of temperature fall is about 5 DEG C/min.When temperature reduces to room temperature, close Muffle furnace,
Take out product.Scanning electron microscope (Fig. 5) can be seen that made α-Al2O3Particle diameter is less, < 50nm, hard aggregation
Inconspicuous.
The toluene of 54ml and the isopropanol of 18ml are stirred at 80-82 DEG C, weighs 15g aluminum isopropylate. and 0.50g
α-Al2O3Powder body, joins in above-mentioned mixed solvent, and stirring treats that aluminum isopropylate. is completely dissolved, and forms solution A, by 1g
Polyvinylpyrrolidone and 4.5g glucose first mix, and are configured to aqueous solution, are designated as B solution, by the B solution of 1/3
Join in solution A, stirring reaction 0.5h, remaining B solution is joined in above-mentioned solution, continue stirring reaction
8h.2h it is dried so that it is moisture evaporates completely, obtains the presoma loosened at 110 DEG C.Other experiment parameter and enforcement
Example 2 is identical.α-the Al that the method obtains2O3Powder body is with α-Al obtained in embodiment 22O3Powder body is compared, particle diameter
Relatively big, reunite more serious.
Embodiment 3: α-Al2O3The preparation of powder body
The toluene of 54ml and the isopropanol of 18ml are stirred at 80-82 DEG C, weighs 15g aluminum isopropylate. and 0.35g
α-Al2O3Powder body, joins in above-mentioned mixed solvent, and stirring treats that aluminum isopropylate. is completely dissolved, and forms solution A, weighs
4.5g glucose, joins in the middle of 4.5ml deionized water, and at 80-82 DEG C, stirring makes it dissolve, and forms B solution, takes
The B solution of 1/3 joins in the middle of above-mentioned solution A, after stirring reaction 30min, is slowly added to remaining B solution, continues
Continuous stirring 4h, forms C solution, weighs 1g polyvinylpyrrolidone, join in the isopropanol of 20ml, at 80-82 DEG C
Lower stirring, to dissolving, forms solution D, solution D is added slowly in the middle of C solution, continues stirring 4h. by gained
Solution is placed in fume hood, after its solvent evaporates completely, is dried 2h so that it is moisture evaporates completely at 110 DEG C,
To loose presoma.To be dried during presoma is put in corundum crucible completely and corundum crucible is put in
In KSL-1400X-A4 type Muffle furnace, heating rate is set as 5 DEG C/min.It is warming up to 1000 DEG C, protects at such a temperature
Temperature 2h, Muffle furnace starts cooling subsequently, and in the temperature range of 1000 DEG C to 500 DEG C, it is 10 DEG C that rate of temperature fall controls
/min.When temperature reduces to less than 500 DEG C, rate of temperature fall is about 5 DEG C/min.When temperature reduces to room temperature, close Muffle furnace,
Take out product.The result of X-ray diffraction analysis (Fig. 6) shows, all diffraction maximums of obtained sample and α-Al2O3
Standard card fits like a glove, without other miscellaneous peak.Scanning electron microscope (Fig. 7) and transmission electron microscope (Fig. 8) table
The bright made α-Al obtained2O3Particle diameter is less, for < 50nm, and dispersibility is preferable, and hard aggregation is inconspicuous.
Claims (4)
1. the method that a low temperature prepares nano aluminium oxide, it is characterised in that comprise the steps:
1. configuration aluminum isopropylate. solution, adds α-Al2O3Powder body crystal seed, is uniformly mixed, wherein, and α-Al2O3Powder body is brilliant
Plant the 2%-5% that quality is aluminum isopropylate. quality；
2. two-step hydrolysis, adds the glucose solution of 1/3 in above-mentioned solution, stirs 0.5-1h at a temperature of 80-82 DEG C,
Adding remaining glucose solution, stir 3-5h the temperature of 80-82 DEG C, wherein, the concentration of glucose solution is
0.5-1.5g/ml, solvent is water, and wherein water is 3:1 with the ratio of the amount of the material of aluminum isopropylate.；
3. in above-mentioned solution, add polyvinylpyrrolidonesolution solution, stir 4-8h, wherein, polyethylene the temperature of 80-82 DEG C
The concentration of pyrrolidone solution is 0.05-0.1g/ml, and solvent is the matter of isopropanol, polyvinylpyrrolidone and aluminum isopropylate.
The ratio of amount is 1:15；
4. by the evaporation of gained solution at room temperature solvent completely, it is dried at a temperature of 100-200 DEG C to moisture and evaporates completely, shape
Become loose presoma；
5. calcining heat treatment after being ground by presoma in atmosphere, calcining heat treatment cools to room temperature with the furnace after completing, obtains
α-Al2O3Powder body.
2. the method that low temperature as claimed in claim 1 prepares nano aluminium oxide, it is characterised in that step 1. in,
α-Al2O3< 100nm, the molar concentration of aluminum isopropylate. solution is 0.5-1.5mol/L to the particle diameter of powder body crystal seed, and its solvent is first
Benzene and the mixed solution of isopropanol, wherein, the volume ratio of toluene and isopropanol is 3:1.
3. the method that low temperature as claimed in claim 1 prepares nano aluminium oxide, it is characterised in that step 4. described in
Drying time is 2h-5h.
4. the method that low temperature as claimed in claim 1 prepares nano aluminium oxide, it is characterised in that step 5. described in
The time of heat treatment is 2h-5h, and heat treatment temperature is 1000-1200 DEG C, and heating rate is 5 DEG C/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110564418A (en) * | 2019-09-18 | 2019-12-13 | 陕西科技大学 | Method for preparing amorphous aluminum-based nano fluorescent powder by sol-gel method and application thereof |
| CN112295516A (en) * | 2019-07-31 | 2021-02-02 | 中国石油化工股份有限公司 | Phase-change microcapsule and preparation method thereof |
-
2015
- 2015-02-02 CN CN201510054602.XA patent/CN105984891A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 李志平: ""高比表面积有序介孔氧化铝的制备及表征"", 《北京化工大学硕士学位论文》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112295516A (en) * | 2019-07-31 | 2021-02-02 | 中国石油化工股份有限公司 | Phase-change microcapsule and preparation method thereof |
| CN110564418A (en) * | 2019-09-18 | 2019-12-13 | 陕西科技大学 | Method for preparing amorphous aluminum-based nano fluorescent powder by sol-gel method and application thereof |
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Application publication date: 20161005 |