CN108483474A - A kind of preparation method of nano-level sphere aluminium oxide - Google Patents
A kind of preparation method of nano-level sphere aluminium oxide Download PDFInfo
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- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/34—Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
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Abstract
The present invention relates to a kind of preparation methods of nano-level sphere aluminium oxide, belong to aluminium oxide processing technique field.The preparation method of the nano-level sphere aluminium oxide of the present invention, includes the following steps：1) by aluminum soluble salt, ammonium citrate, water, with after ethyl alcohol mixing in 150 DEG C~200 DEG C solvent thermal reactions 15~for 24 hours, postcooling, filter to obtain product, product be dried, obtain presoma；2) presoma obtained by step 1) is kept the temperature into 2~7h in 400 DEG C~600 DEG C to obtain the final product.The preparation method of the nano-level sphere aluminium oxide of the present invention, breach the limitation for using the alkaline matters such as urea, ammonium hydroxide, sodium hydroxide to prepare ball-aluminium oxide in the prior art, and the aluminium oxide regular appearance obtained by the method for the present invention, reunite without apparent, particle size is tiny, reach Nano grade, the application prospect having had.
Description
Technical field
The present invention relates to a kind of preparation methods of nano-level sphere aluminium oxide, belong to aluminium oxide processing technique field.
Background technology
Aluminium oxide (Al2O3) it is a kind of amphoteric oxide, there is high intensity, high rigidity, high-wearing feature, high stability, good
Corrosion resistance and the excellent properties such as ionic conductivity, therefore in electronics, refractory material, abrasive material and aerospace field all
To being widely applied.Wherein ball-aluminium oxide has well-regulated pattern, smaller specific surface area, larger bulk density and good
Good mobility, so be widely used in making polishing material, catalyst etc. again.
Nano-level sphere aluminium oxide is widely used in conventional industries (light industry, chemical industry, building materials etc.) and new material, micro- electricity
The high-tech areas such as son, aerospace industry, application prospect are very wide.For example, being added as ceramics using nano-level sphere aluminium oxide
Add agent, it can be with effective solution ceramics be due to black brittleness and problem that application range is narrow, so as to which cold plasticity ball is made
Shape aluminium oxide ceramics；Nano-level sphere aluminium oxide is extremely sensitive to humidity, there is high application value on humidity sensor,
In addition it is also widely applied to the substrate material of large scale integrated circuit.Currently, domestic and international market is to nano-level sphere aluminium oxide
Demand constantly increase, therefore, further exploration prepares the new method of nano-level sphere alumina powder just and has very heavy
The meaning wanted.
It is recorded according to pertinent literature, the preparation of aluminium oxide is mostly used the substances such as aluminum nitrate, aluminum sulfate, urea as raw material, through reality
It is found after testing：Using urea as precipitating reagent, with Al (NO3)3·9H2O carry out hydro-thermal reaction prepare it is mostly be needle-shaped alumina,
Its suppression performance and sintering characteristic are not so good as ball-shaped micro powder；Using urea as precipitating reagent, with Al2(SO4)3·18H2O carries out hydro-thermal reaction
Though what is prepared is ball-aluminium oxide, reunite serious, particle size is coarseer, Nano grade is not achieved, correlated performance is not
It is ideal.
Application publication number is that the Chinese invention patent of CN 104591240A discloses a kind of preparation of ball-aluminium oxide powder
The preparation method of technology, the ball-aluminium oxide powder of the patent disclosure includes the following steps：It is molten that aluminum nitrate is added dropwise with ammonia spirit
Liquid occurs flocculent deposit in reaction system, and full of entire liquid without sinking, when the pH value of reaction system reaches 7~10,
Stop that ammonium hydroxide is added dropwise, then reaction solution is spray-dried using various sizes of nozzle, obtains ball-aluminium oxide predecessor；
The predecessor is obtained into micron order γ type ball-aluminium oxide powders by 450 DEG C~600 DEG C 1~3h of calcining.The patent disclosure
The ball-aluminium oxide powder ball-aluminium oxide powder that carries out, and obtain in alkaline system be micron order, still need into one
Step is improved.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of nano-level sphere aluminium oxide, breach and exist in the prior art
The limitation of nano-level sphere aluminium oxide is prepared under alkaline condition.
To achieve the above object, the technical scheme is that：
A kind of preparation method of nano-level sphere aluminium oxide, includes the following steps：
1) by aluminum soluble salt, ammonium citrate, water, with ethyl alcohol mixing after in 150 DEG C~200 DEG C solvent thermal reactions 15~
For 24 hours, postcooling filters to obtain product, product is dried, obtains presoma；
2) presoma obtained by step 1) is kept the temperature into 2~7h in 400 DEG C~600 DEG C to obtain the final product.
The aluminum soluble salt is aluminum nitrate.
The aluminum soluble salt, ammonium citrate, water and ethyl alcohol mixing be by soluble aluminum salting liquid, ammonium citrate solution with
Ethyl alcohol mixing.
A concentration of 1~1.5mol/L of the soluble aluminum salting liquid, ammonium citrate solution a concentration of 0.1~
0.5mol/L。
The soluble aluminum salting liquid is aluminum nitrate solution.The preparation of the aluminum nitrate solution includes the following steps：It will match
Al (the NO just measured3)3·9H2O is added in deionized water, is stirred to dissolve with glass bar to obtain the final product.
The aluminum nitrate solution is clear solution.
Al (the NO3)3·9H2O is that analysis is pure.
The preparation of the ammonium citrate solution includes the following steps：By the C of formula ratio6H5(NH4)3O7·2H2O addition go from
In sub- water, with glass bar stir to dissolve to get.
The ammonium citrate solution is clear solution.
Above-mentioned soluble aluminum salting liquid, ammonium citrate solution and ethyl alcohol mixing are：Ammonium citrate solution is added to solvable
In property aluminum salt solution, ethyl alcohol mixing is added after mixing.Ethyl alcohol is as dispersant so that the nanoscale γ-AlOOH and oxygen of generation
Change aluminum particulate dispersion, reduces and reunite.
The ratio between the sum of volume of the soluble aluminum salting liquid and ammonium citrate solution and the volume of ethyl alcohol are 1~3:1.
Al in the soluble aluminum salting liquid3+With the molar ratio of the citrate ion in ammonium citrate solution be 2~
5:1。
Solvent thermal reaction in step 1) carries out in a kettle.The liner of the reaction kettle is polytetrafluoroethylene (PTFE) material.
70%-80% of the compactedness control of the reaction kettle in reaction kettle volume.
It is cooled to cooled to room temperature in step 1).
It is washed after being separated by solid-liquid separation in step 1).The separation of solid and liquid is to topple over supernatant liquor.Vacuum pumping is carried out after washing
Filter.
Drying in step 1) is in 90~120 DEG C of dry 6~12h.The drying carries out in vacuum drying chamber.
The washing is washed with ethyl alcohol again to be first washed with water.
It is ground after above-mentioned drying.
Ammonium citrate solution used in the present invention is acid solution, and ammonium citrate is dissolved in water power and separates out citrate ion and ammonium
Radical ion, ammonium ion hydrolysis generate hydrogen ion：NH4 ++H2O=NH4OH+H+。
After aluminum nitrate solution and ammonium citrate solution are mixed, the aluminium ion in solution and citrate ion
(citrate3-) there can be following combination：
But it can be carried out to the left under the high temperature and pressure of the reaction under hydrothermal conditions (because the formation of chemical bond is that heat release is anti-
Answer, be unfavorable for the progress of exothermic reaction under the high temperature and pressure of hydro-thermal, so reaction carries out to the left), that is, there is a large amount of free aluminium
Ion exists, at this point, aluminium ion meeting and NH4OH reactions generate aluminium hydroxide.Aluminium hydroxide can be with hydrogen ion hair under general condition
Raw neutralization reaction so that aluminum hydroxide precipitation can not retain, but since neutralization reaction is exothermic reaction, and in the high temperature of hydro-thermal height
Pressure is unfavorable for the progress of exothermic reaction, therefore neutralization reaction can not be normally carried out, to which aluminum hydroxide precipitation is retained；
Under 150 DEG C~200 DEG C of hydrothermal temperature and the high pressure of hydro-thermal reaction, aluminium hydroxide can be decomposed to form γ-AlOOH, that is, occur anti-
It answers：Al(OH)3→γ-AlOOH+H2O。
The present invention ammonium citrate, ammonium ion hydrolysis be used as precipitating reagent, citrate ion as pattern controlling agent with
Stabilizer forms complicated micro-structure.Self assembly is considered as forming the effective means of complicated superstructure, and self assembly is usually logical
It crosses Van der Waals force and hydrogen bond pushes nano-particle to form orderly arrangement architecture.In the present invention, citrate ion selectivity
γ-AlOOH nanoparticle surfaces are adsorbed on, it is made to grow into shorter nanometer rods, while citrate ion in one direction
In carboxyl and γ-AlOOH in octahedral structure AlO6In hydroxyl formed hydrogen bond, under the interaction of these hydrogen bonds,
Nanometer rods can be self-assembly of spherical micro-structure.Later using the high-temperature calcination of step 2), spherical AlOOH is converted to spherical shape
Aluminium oxide.
The preparation method of the nano-level sphere aluminium oxide of the present invention, using ammonium citrate as precipitating reagent and pattern controlling agent,
Hydrated alumina is prepared using hydro-thermal method under acidic environment, then prepares nano-level sphere alumina particle after calcining, is broken through
In the prior art using the limitation for preparing ball-aluminium oxide using alkaline matters such as urea, ammonium hydroxide, sodium hydroxides, and the present invention
Aluminium oxide regular appearance obtained by method is reunited without apparent, and particle size is tiny, reaches Nano grade, before the application having had
Scape.
Description of the drawings
Fig. 1 is the XRD diagram of 1 gained alumina particle of embodiment；
Fig. 2 is the SEM figures of the alumina particle of 1 gained of embodiment；
Fig. 3 is the SEM figures of the alumina particle of 2 gained of embodiment；
Fig. 4 is the SEM figures of the alumina particle of 3 gained of embodiment；
Fig. 5 is the SEM figures of the alumina particle of 4 gained of embodiment.
Specific implementation mode
Embodiments of the present invention are described further below in conjunction with the accompanying drawings.
Embodiment 1
The preparation method of the nano-level sphere aluminium oxide of the present embodiment, includes the following steps：
1) by analytically pure Al (NO3)3·9H2O is added in deionized water, is stirred to dissolve with glass bar, and Al is made3+
The clear solution A of a concentration of 1.2mol/L, it is spare；By analytically pure C6H5(NH4)3O7·2H2O is added in deionized water, uses glass
Glass stick stirs to dissolve, and the clear solution B of a concentration of 0.3mol/L is made, spare；
2) a certain amount of ammonium citrate solution B is added in solution A so that Al3+Molar ratio with citrate ion is
4:1, it is stirred with glass bar, obtained solution C；A certain amount of absolute ethyl alcohol is added into solution C, makes solution C and second
Alcohol volume ratio is 1:1, it is stirred with glass bar, obtained solution D；
3) solution D is poured into the hydrothermal reaction kettle liner of polytetrafluoroethylene (PTFE) material, compactedness control is 80%, sealing water
Thermal response kettle, puts it into electric heating constant-temperature blowing drying box, and hydrothermal temperature is controlled at 200 DEG C, is reacted 15 hours, reaction terminates
After naturally cool to room temperature；Then hydrothermal reaction kettle is opened, supernatant liquid is toppled over, precipitated product is washed with deionized three
It after secondary, then is washed three times with absolute ethyl alcohol, is filtered by vacuum, then be placed in 90 DEG C of vacuum drying chamber 10 hours dry, done
It after the completion of dry, is ground, keeps the temperature 5 hours in 550 DEG C to get nano-level sphere alumina particle later.
The XRD diagram of the nano-level sphere alumina particle of the present embodiment by Fig. 1 as shown in Figure 1, can be determined that products therefrom
For nano-level sphere aluminium oxide.
The SEM figures of the nano-level sphere alumina particle of the present embodiment are shown in Fig. 2, as shown in Figure 2, the present embodiment products therefrom
For nano level spheric granules, shape is regular.
Embodiment 2
The preparation method of the nano-level sphere alumina particle of the present embodiment, includes the following steps：
1) by analytically pure Al (NO3)3·9H2O is added in deionized water, is stirred to dissolve with glass bar, and Al is made3+
The clear solution A of a concentration of 1.2mol/L, it is spare；By analytically pure C6H5(NH4)3O7·2H2O is added in deionized water, uses glass
Glass stick stirs to dissolve, and the clear solution B of a concentration of 0.4mol/L is made, spare；
2) a certain amount of ammonium citrate solution B is added in solution A so that Al3+Molar ratio with citrate ion is
3:1, it is stirred with glass bar, obtained solution C；A certain amount of absolute ethyl alcohol is added into solution C, makes solution C and second
Alcohol volume ratio is 1:1, it is stirred with glass bar, obtained solution D；
3) solution D is poured into the hydrothermal reaction kettle liner of polytetrafluoroethylene (PTFE) material, compactedness control is 75%, sealing water
Thermal response kettle, puts it into electric heating constant-temperature blowing drying box, and hydrothermal temperature is controlled at 150 DEG C, is reacted 20 hours, reaction terminates
After naturally cool to room temperature；Then hydrothermal reaction kettle is opened, supernatant liquid is toppled over, precipitated product is washed with deionized three
It after secondary, then is washed three times with absolute ethyl alcohol, is filtered by vacuum, then be placed in 100 DEG C of vacuum drying chamber 8 hours dry, done
It after the completion of dry, is ground, keeps the temperature 2 hours in 600 DEG C to get nano-level sphere alumina particle later.
The SEM figures of the nano-level sphere alumina particle of the present embodiment are shown in Fig. 3, from the figure 3, it may be seen that the present embodiment products therefrom
For nano level spheric granules, shape is regular.
Embodiment 3
The preparation method of the nano-level sphere alumina particle of the present embodiment, includes the following steps：
1) by analytically pure Al (NO3)3·9H2O is added in deionized water, is stirred to dissolve with glass bar, and Al is made3+
The clear solution A of a concentration of 1.4mol/L, it is spare；By analytically pure C6H5(NH4)3O7·2H2O is added in deionized water, uses glass
Glass stick stirs to dissolve, and the clear solution B of a concentration of 0.35mol/L is made, spare；
2) a certain amount of ammonium citrate solution B is added in solution A so that Al3+Molar ratio with citrate ion is
4:1, it is stirred with glass bar, obtained solution C；A certain amount of absolute ethyl alcohol is added into solution C, makes solution C and second
Alcohol volume ratio is 1:1, it is stirred with glass bar, obtained solution D；
3) solution D is poured into the hydrothermal reaction kettle liner of polytetrafluoroethylene (PTFE) material, compactedness control is 80%, sealing water
Thermal response kettle, puts it into electric heating constant-temperature blowing drying box, and hydrothermal temperature is controlled at 170 DEG C, is reacted 15 hours, reaction terminates
After naturally cool to room temperature；Then hydrothermal reaction kettle is opened, supernatant liquid is toppled over, precipitated product is washed with deionized three
It after secondary, then is washed three times with absolute ethyl alcohol, is filtered by vacuum, then be placed in 90 DEG C of vacuum drying chamber 12 hours dry, done
It after the completion of dry, is ground, keeps the temperature 6 hours in 500 DEG C to get nano-level sphere alumina particle later.
The SEM figures of the nano-level sphere alumina particle of the present embodiment are shown in Fig. 4, as shown in Figure 4, the present embodiment products therefrom
For nano level spheric granules, shape is regular.
Embodiment 4
The preparation method of the nano-level sphere alumina particle of the present embodiment, includes the following steps：
1) by analytically pure Al (NO3)3·9H2O is added in deionized water, is stirred to dissolve with glass bar, and Al is made3+
The clear solution A of a concentration of 1.3mol/L, it is spare；By analytically pure C6H5(NH4)3O7·2H2O is added in deionized water, uses glass
Glass stick stirs to dissolve, and the clear solution B of a concentration of 0.3mol/L is made, spare；
2) a certain amount of ammonium citrate solution B is added in solution A so that Al3+Molar ratio with citrate ion is
4:1, it is stirred with glass bar, obtained solution C；A certain amount of absolute ethyl alcohol is added into solution C, makes solution C and second
Alcohol volume ratio is 2:1, it is stirred with glass bar, obtained solution D；
3) solution D is poured into the hydrothermal reaction kettle liner of polytetrafluoroethylene (PTFE) material, compactedness control is 80%, sealing water
Thermal response kettle, puts it into electric heating constant-temperature blowing drying box, and hydrothermal temperature is controlled at 200 DEG C, is reacted 24 hours, reaction terminates
After naturally cool to room temperature；Then hydrothermal reaction kettle is opened, supernatant liquid is toppled over, precipitated product is washed with deionized three
After secondary, then washed three times with absolute ethyl alcohol, be filtered by vacuum, then be placed in 95 DEG C of vacuum drying chamber it is 9 hours dry, it is dry
After the completion, it is ground, keeps the temperature 5 hours in 450 DEG C to get nano-level sphere alumina particle later.
The SEM figures of the nano-level sphere alumina particle of the present embodiment are shown in Fig. 5, as shown in Figure 5, the present embodiment products therefrom
For nano level spheric granules, shape is regular.
Embodiment 5
The preparation method of the nano-level sphere alumina particle of the present embodiment, includes the following steps：
1) by analytically pure Al (NO3)3·9H2O is added in deionized water, is stirred to dissolve with glass bar, and Al is made3+
The clear solution A of a concentration of 1.5mol/L, it is spare；By analytically pure C6H5(NH4)3O7·2H2O is added in deionized water, uses glass
Glass stick stirs to dissolve, and the clear solution B of a concentration of 0.3mol/L is made, spare；
2) a certain amount of ammonium citrate solution B is added in solution A so that Al3+Molar ratio with citrate ion is
5:1, it is stirred with glass bar, obtained solution C；A certain amount of absolute ethyl alcohol is added into solution C, makes solution C and second
Alcohol volume ratio is 3:1, it is stirred with glass bar, obtained solution D；
3) solution D is poured into the hydrothermal reaction kettle liner of polytetrafluoroethylene (PTFE) material, compactedness control is 80%, sealing water
Thermal response kettle, puts it into electric heating constant-temperature blowing drying box, and hydrothermal temperature is controlled at 200 DEG C, is reacted 20 hours, reaction terminates
After naturally cool to room temperature；Then hydrothermal reaction kettle is opened, supernatant liquid is toppled over, by precipitated product by product deionized water
After washing three times, then wash three times with absolute ethyl alcohol, be filtered by vacuum, then is placed in 120 DEG C of vacuum drying chamber that dry 6 small
When, it after the completion of dry, is ground, keeps the temperature 7 hours in 400 DEG C to get nano-level sphere alumina particle later.
Claims (10)
1. a kind of preparation method of nano-level sphere aluminium oxide, which is characterized in that include the following steps：
1) by aluminum soluble salt, ammonium citrate, water, with after ethyl alcohol mixing in 150 DEG C~200 DEG C solvent thermal reactions 15~for 24 hours, it
Postcooling is separated by solid-liquid separation to obtain product, product is dried, obtains presoma；
2) presoma obtained by step 1) is kept the temperature into 2~7h in 400 DEG C~600 DEG C to obtain the final product.
2. the preparation method of nano-level sphere aluminium oxide according to claim 1, which is characterized in that the aluminum soluble salt
For aluminum nitrate.
3. the preparation method of nano-level sphere aluminium oxide according to claim 1, which is characterized in that the soluble aluminum
Salt, ammonium citrate, water and ethyl alcohol mixing are by soluble aluminum salting liquid, ammonium citrate solution and ethyl alcohol mixing.
4. the preparation method of nano-level sphere aluminium oxide according to claim 3, which is characterized in that the aluminum soluble salt
A concentration of 1~1.5mol/L of solution, a concentration of 0.1~0.5mol/L of ammonium citrate solution.
5. the preparation method of nano-level sphere aluminium oxide according to claim 3, which is characterized in that the aluminum soluble salt
The ratio between the sum of volume of solution and ammonium citrate solution and the volume of ethyl alcohol are 1~3:1.
6. the preparation method of nano-level sphere aluminium oxide according to claim 3, which is characterized in that the aluminum soluble salt
Al in solution3+Molar ratio with the citrate ion in ammonium citrate solution is 2~5:1.
7. the preparation method of nano-level sphere aluminium oxide according to claim 1, which is characterized in that solid-liquid point in step 1)
From rear washing.
8. the preparation method of nano-level sphere aluminium oxide according to claim 7, which is characterized in that carry out vacuum after washing
It filters.
9. the preparation method of nano-level sphere aluminium oxide according to claim 1, which is characterized in that the drying in step 1)
For in 90~120 DEG C of dry 6~12h.
10. the preparation method of nano-level sphere aluminium oxide according to claim 7 or 8, which is characterized in that the washing is
It is first washed with water and is washed again with ethyl alcohol.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109534379A (en) * | 2019-01-09 | 2019-03-29 | 上海大学(浙江·嘉兴)新兴产业研究院 | A kind of nano-level sphere γ-Al2O3The low cost preparation method of powder |
| CN109999774A (en) * | 2019-04-25 | 2019-07-12 | 河南科技大学 | Nano-titanium dioxide/gama-alumina composite powder preparation method |
| CN111484050A (en) * | 2020-04-21 | 2020-08-04 | 北京邮电大学 | Preparation method of sphere-like α phase nano-alumina |
| CN111960809A (en) * | 2020-08-26 | 2020-11-20 | 武汉理工大学 | Spherical Al for photocuring 3D printing2O3Method for preparing powder |
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| CN109534379A (en) * | 2019-01-09 | 2019-03-29 | 上海大学(浙江·嘉兴)新兴产业研究院 | A kind of nano-level sphere γ-Al2O3The low cost preparation method of powder |
| CN109999774A (en) * | 2019-04-25 | 2019-07-12 | 河南科技大学 | Nano-titanium dioxide/gama-alumina composite powder preparation method |
| CN111484050A (en) * | 2020-04-21 | 2020-08-04 | 北京邮电大学 | Preparation method of sphere-like α phase nano-alumina |
| CN111484050B (en) * | 2020-04-21 | 2021-05-18 | 北京邮电大学 | Preparation method of spheroidal alpha-phase nano-alumina |
| CN111960809A (en) * | 2020-08-26 | 2020-11-20 | 武汉理工大学 | Spherical Al for photocuring 3D printing2O3Method for preparing powder |
| CN111960809B (en) * | 2020-08-26 | 2022-07-19 | 武汉理工大学 | Spherical Al for photocuring 3D printing2O3Method for preparing powder |
| CN112374514A (en) * | 2020-11-11 | 2021-02-19 | 广州大学 | Method for rapidly preparing bayer stone microspheres with uniform particle size by double hydrolysis at room temperature |
| CN112374514B (en) * | 2020-11-11 | 2022-09-30 | 广州大学 | Method for rapidly preparing bayer stone microspheres with uniform particle size by double hydrolysis at room temperature |
| CN115057457A (en) * | 2022-07-26 | 2022-09-16 | 杭州晶祥新材料科技有限公司 | Preparation method of high-purity spheroidized nano aluminum oxide |
| CN115057457B (en) * | 2022-07-26 | 2023-12-12 | 杭州晶祥新材料科技有限公司 | Preparation method of high-purity spheroidized nano alumina |
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