CN106495194A - A kind of method of low temperature preparation alpha-type aluminum oxide superfine powder - Google Patents
A kind of method of low temperature preparation alpha-type aluminum oxide superfine powder Download PDFInfo
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- CN106495194A CN106495194A CN201510557854.4A CN201510557854A CN106495194A CN 106495194 A CN106495194 A CN 106495194A CN 201510557854 A CN201510557854 A CN 201510557854A CN 106495194 A CN106495194 A CN 106495194A
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- aluminum oxide
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Abstract
The invention discloses a kind of method of low temperature preparation alpha-type aluminum oxide superfine powder.By cross-linking agent resorcinol and dispersant PVP is added in aluminum nitrate, gained reaction solution is dried at 80-90 DEG C, remove solvent, form loose alumina precursor；Then, in air atmosphere, high-temperature calcination is carried out to dried presoma and obtains high-purity superfine alumina powder.The present invention has simple to operate, required cycle is short, reproducible, facilitates implementation industrialization, and α-Al2O3Required crystal conversion temperature is relatively low, and the alumina particle for preparing is little, less than 200nm, good dispersion.
Description
Technical field
The present invention relates to a kind of method of low temperature preparation alpha-type aluminum oxide superfine powder, belongs to chemical materialss preparation field.
Background technology
Alpha-alumina (α-Al2O3) have high rigidity, high intensity, wear-resistant, corrosion-resistant, high temperature resistant, antioxidation,
Good insulating, surface area are big, thermal coefficient of expansion is little, thermal shock resistance is good, the low excellent characteristic of dielectric loss,
So its aspects such as metallurgy, chemical industry, catalysis, fire-retardant, sound insulation, insulation, electronics, fine ceramics have special
Purposes, the therefore preparation of alumina ultrafine powder body has great importance.Current conventional method presses reaction medium can
To be divided into solid phase method, liquid phase method, vapor phase method.Solid phase method is by metallic aluminium or aluminium salt directly grinding or heating point
Xie Hou, then through calcination processing, after there is solid state reaction, directly obtain a kind of method of aluminium oxide.Vapor phase method is straight
Connect using gas or material is become by modes such as plasma, laser evaporation, electron beam heating, electric arc heateds
Into gas, it is allowed to issue biological reason or chemical reaction in gaseous state, finally in cooling procedure, cohesion grows up to be formed
Super fine.Liquid phase method is current laboratory and the industrial widely used method for preparing superfine powder.It basic
Principle is：A kind of suitable aluminum soluble salt is selected, by prepared material composition the configuration of metering into solution, is made each
Element is in ionic state, a kind of suitable precipitant of reselection (or with evaporation, distillation, hydrolyze etc.), makes metal ion
Homogeneous precipitation, will finally precipitate or crystal dehydration (or heating) obtains ultrafine powder.Solid phase method is readily incorporated miscellaneous
Matter, and obtained diameter of particle is difficult to reach Nano grade；Vapor phase method is due to equipping huge, apparatus expensive etc.
Shortcoming limits which and uses；So far, the research for preparing nano aluminium oxide to liquid phase method is relatively more, obtained
Powder body have particle diameter little, the advantages of good dispersion.
Xinghua Su et al. (J.Mater.Sci.Technol, 2011,11,1011-1015) are with Al (NO3)3·9H2O、
NH3H2O, PEG-2000 and K2SO4For raw material, alumina precursor is obtained using sol-gel process, at 900 DEG C
Monocrystalline α-Al are obtained after calcining2O3But, the α-Al that the method is obtained2O3Diameter of particle is larger, about a diameter of
0.5-1.5 μm of lamellar, and step is complicated, raw materials used more, cost is big, and dispersibility is not fine.In addition,
K2SO4It is very difficult to remove so that aluminium oxide purity is substantially reduced.Xuelian Du et al. (Appl.Phys.
A, 2014,116,1963-1969) with Al (NO3)3·9H2O、NH3H2O, PEG-2000, NaCl and α-Al2O3Crystal seed
For raw material, alumina precursor is obtained using sol-gel process, α-Al are obtained after 1000 DEG C of calcinings2O3, this method
Step is numerous and diverse, raw materials used many, and cost is big, and finally cleaning causes aluminium oxide purity to reduce except unnet NaCl.?
In above two method, α-Al2O3Crystal conversion temperature decreases, but α is-Al2O3Particle diameter is still larger, and oxygen
It is not fine to change aluminum purity, is doped with inorganic matters.
Content of the invention
The present invention is intended to provide a kind of method of low temperature preparation alpha-type aluminum oxide superfine powder.
The technical scheme is that：A kind of method of low temperature preparation alpha-type aluminum oxide superfine powder, using following step
Rapid preparation：
1. aluminum nitrate is added in resorcinol solution, be stirred into mixed solution；
2. PVP, and stirring reaction at a temperature of 55-65 DEG C are added in above-mentioned mixed solution；
3. by step, 2. resulting solution is dried to solvent evaporating completely at 80-90 DEG C, forms loose presoma；
4. presoma is calcined heat treatment in atmosphere, room temperature is cooled to the furnace after the completion of calcining heat treatment, is obtained after grinding
α-Al2O3Powder body.
Step 1. in, the molar concentration of resorcinol solution is 0.1-0.2mol/L；Aluminum nitrate is dense in mixed solution
Spend for 0.1-0.2mol/L.
Step 2. in, concentration of the PVP in mixed solution be 0.02-0.05mol/L, the stirring reaction time be 2-4h.
Step 3. in, drying time is 4-6h.
Step 4. in, time of heat treatment is 2-3h, and heat treatment temperature is 1000-1200 DEG C, and heating rate is 5 DEG C
/min.
This method is had the advantages that compared with other prepare the method for aluminium oxide：
1. the present invention carrys out Borolon using resorcinol for cross-linking agent first, does not add formaldehyde and catalyst；
2. aluminium oxide crystal conversion temperature is relatively low, is 1000 DEG C；
3. of the invention simple to operate, the cycle is short, repeatability are high, facilitate implementation industrialized production；
4. the diameter of particle for preparing is little, less than 200nm, good dispersion；
5. other inorganic impurities are not introduced in preparation process, powder purity is obtained high.
Description of the drawings
Fig. 1 is α-Al in the embodiment of the present invention 12O3The X-ray diffractogram of powder body.
Fig. 2 is α-Al in the embodiment of the present invention 12O3The scanning electron microscope diagram piece of powder body.
Fig. 3 is α-Al in the embodiment of the present invention 12O3The transmission electron micrograph of powder body.
Fig. 4 is α-Al in the embodiment of the present invention 22O3The scanning electron microscope diagram piece of powder body.
Fig. 5 is α-Al in the embodiment of the present invention 32O3The X-ray diffractogram of powder body.
Fig. 6 is α-Al in the embodiment of the present invention 32O3The scanning electron microscope diagram piece of powder body.
Specific embodiment
Embodiment 1：α-Al2O3The preparation of powder body
1.1g resorcinol is weighed, 3.75g aluminum nitrates and 0.555gPVP are standby, and resorcinol is dissolved in 100ml
Deionized water in, add aluminum nitrate and PVP, ceaselessly stir to being completely dissolved, there-necked flask is placed in 55-65 DEG C
Water-bath in continue stirring reaction 4h, resulting solution taken out to be placed in 80 DEG C of baking oven dry 4h, remove molten
Agent, forms loose alumina precursor.Completely alumina precursor will be dried to be put in corundum crucible and by just
Beautiful crucible is put in KSL-1400X-A4 type Muffle furnaces, and heating rate is set as 5 DEG C/min.1000 DEG C are warming up to,
2h is incubated at such a temperature, subsequent Muffle furnace starts to lower the temperature, in 1000 DEG C to 400 DEG C of temperature range, cooling
Rate controlled is 10 DEG C/min.When temperature is reduced to less than 400 DEG C, rate of temperature fall is about 5 DEG C/min.Temperature is reduced to
During room temperature, Muffle furnace is closed, take out product.The result of X-ray diffraction analysis (Fig. 1) shows, obtained sample
The diffraction maximum of product and α-Al2O3Standard card fits like a glove, without other miscellaneous peaks.Scanning electron microscope (Fig. 2) and thoroughly
Penetrate ultramicroscope (Fig. 3) and show the made α-Al for obtaining2O3Diameter of particle is less,<200nm, and dispersibility
Preferably, hard aggregation is not obvious.
Embodiment 2：α-Al2O3The preparation of powder body
2.2g resorcinol is weighed, 3.75g aluminum nitrates and 0.555gPVP are standby, and resorcinol is dissolved in 100ml
Deionized water in, add aluminum nitrate and PVP, ceaselessly stir to being completely dissolved, there-necked flask is placed in 55-65 DEG C
Water-bath in continue stirring reaction 4h, resulting solution taken out to be placed in 80 DEG C of baking oven dry 4h, remove molten
Agent, forms loose alumina precursor.Completely alumina precursor will be dried to be put in corundum crucible and by just
Beautiful crucible is put in KSL-1400X-A4 type Muffle furnaces, and heating rate is set as 5 DEG C/min.1000 DEG C are warming up to,
2h is incubated at such a temperature, subsequent Muffle furnace starts to lower the temperature, in 1000 DEG C to 400 DEG C of temperature range, cooling
Rate controlled is 10 DEG C/min.When temperature is reduced to less than 400 DEG C, rate of temperature fall is about 5 DEG C/min.Temperature is reduced to
During room temperature, Muffle furnace is closed, take out product.Scanning electron microscope (Fig. 4) shows the made α-Al for obtaining2O3
Diameter of particle is less,<200nm, and dispersibility is preferably, and hard aggregation is not obvious.
Change the reaction temperature in embodiment 2, other specification keeps constant, when reaction temperature is less than 55 DEG C, hands over
Connection reaction is slow, the α-Al for preparing2O3Particle diameter is uneven, when reaction temperature is higher than 65 DEG C, can cause solvent
Evaporation, in course of reaction, pressed powder is separated out, the α-Al for preparing2O3Particle diameter is larger, and uneven.
Embodiment 3：α-Al2O3The preparation of powder body
1.1g resorcinol is weighed, 3.75g aluminum nitrates and 0.555gPVP are standby, and resorcinol is dissolved in 100ml
Deionized water in, add aluminum nitrate and PVP, ceaselessly stir to being completely dissolved, there-necked flask is placed in 55-65 DEG C
Water-bath in continue stirring reaction 4h, resulting solution taken out to be placed in 80 DEG C of baking oven dry 4h, remove molten
Agent, forms loose alumina precursor.Completely alumina precursor will be dried to be put in corundum crucible and by just
Beautiful crucible is put in KSL-1400X-A4 type Muffle furnaces, and heating rate is set as 5 DEG C/min.1100 DEG C are warming up to,
2h is incubated at such a temperature, subsequent Muffle furnace starts to lower the temperature, in 1100 DEG C to 600 DEG C of temperature range, cooling
Rate controlled is 10 DEG C/min.When temperature is reduced to less than 600 DEG C, rate of temperature fall is about 5 DEG C/min.Temperature is reduced to
During room temperature, Muffle furnace is closed, take out product.The result of X-ray diffraction analysis (Fig. 5) shows, obtained sample
The diffraction maximum of product and α-Al2O3Standard card fits like a glove, without other miscellaneous peaks.Scanning electron microscope (Fig. 6) shows
Made α-the Al for obtaining2O3Diameter of particle is less,<200nm, and dispersibility is preferably, and hard aggregation is not obvious.
Claims (5)
1. a kind of method of low temperature preparation alpha-type aluminum oxide superfine powder, it is characterised in that comprise the steps：
1. aluminum nitrate is added in resorcinol solution, be stirred into mixed solution；
2. PVP, and stirring reaction at a temperature of 55-65 DEG C are added in above-mentioned mixed solution；
3. by step, 2. resulting solution is dried to solvent evaporating completely at 80-90 DEG C, forms loose presoma；
4. presoma is calcined heat treatment in atmosphere, room temperature is cooled to the furnace after the completion of calcining heat treatment, after grinding
Obtain α-Al2O3Powder body.
2. the method for low temperature preparation alpha-type aluminum oxide superfine powder as claimed in claim 1, it is characterised in that
Step 1. in, the molar concentration of resorcinol solution is 0.1-0.2mol/L；Aluminum nitrate is dense in mixed solution
Spend for 0.1-0.2mol/L.
3. the method for low temperature preparation alpha-type aluminum oxide superfine powder as claimed in claim 1, it is characterised in that
Step 2. in, concentration of the PVP in mixed solution be 0.02-0.05mol/L, the stirring reaction time be 2-4h.
4. the method for low temperature preparation alpha-type aluminum oxide superfine powder as claimed in claim 1, it is characterised in that
Step 3. in, drying time is 4-6h.
5. the method for low temperature preparation alpha-type aluminum oxide superfine powder as claimed in claim 1, it is characterised in that
Step 4. in, time of heat treatment is 2-3h, 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 |
|---|---|---|---|---|
| CN113830809A (en) * | 2021-10-27 | 2021-12-24 | 中国科学院青海盐湖研究所 | Preparation method of superfine alumina powder and product thereof |
| CN116042098A (en) * | 2023-02-08 | 2023-05-02 | 广东粤港澳大湾区黄埔材料研究院 | Nano alumina polishing solution and application thereof in polishing of infrared chalcogenide glass |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110052485A1 (en) * | 2007-08-31 | 2011-03-03 | Jps Micro-Tech Co., Ltd | Method of manufacturing flake aluminum oxide using microwave |
| CN102476819A (en) * | 2010-11-27 | 2012-05-30 | 中国科学院兰州化学物理研究所 | Preparation method of nano alpha-alumina powder |
| CN102659154A (en) * | 2012-05-17 | 2012-09-12 | 天津凯美科技有限公司 | Method for preparing nano alpha-Al2O3 powder |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110052485A1 (en) * | 2007-08-31 | 2011-03-03 | Jps Micro-Tech Co., Ltd | Method of manufacturing flake aluminum oxide using microwave |
| CN102476819A (en) * | 2010-11-27 | 2012-05-30 | 中国科学院兰州化学物理研究所 | Preparation method of nano alpha-alumina powder |
| CN102659154A (en) * | 2012-05-17 | 2012-09-12 | 天津凯美科技有限公司 | Method for preparing nano alpha-Al2O3 powder |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113830809A (en) * | 2021-10-27 | 2021-12-24 | 中国科学院青海盐湖研究所 | Preparation method of superfine alumina powder and product thereof |
| CN116042098A (en) * | 2023-02-08 | 2023-05-02 | 广东粤港澳大湾区黄埔材料研究院 | Nano alumina polishing solution and application thereof in polishing of infrared chalcogenide glass |
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