CN103194741B - Alumina precursor solution, and preparation method and application thereof - Google Patents
Alumina precursor solution, and preparation method and application thereof Download PDFInfo
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- CN103194741B CN103194741B CN201310115583.8A CN201310115583A CN103194741B CN 103194741 B CN103194741 B CN 103194741B CN 201310115583 A CN201310115583 A CN 201310115583A CN 103194741 B CN103194741 B CN 103194741B
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Abstract
The invention discloses alumina precursor solution and a preparation method and application thereof. The preparation method comprises the following steps of: (a), adding anhydrous aluminium chloride in heated glacial acetic acid, and reacting at constant temperature for 8-10 min to obtain semi-transparent aluminium acetate colloid; (b), centrifuging the aluminium acetate colloid at a high speed for 10-15min in a high-speed centrifugal machine to obtain aluminium acetate particles; and (C), putting the aluminium acetate particles obtained in the step (b) into deionized water, acetone or alcohol solvent, so as to obtain a solution with the mass concentration of 20-40%, and oscillating or stirring to obtain the alumina precursor solution. The preparation method disclosed by the invention is simple and convenient to operate and low in cost; the prepared precursor solution can be stored for a long time, therefore, alumina and an alumina film prepared from the solution at a low temperature are excellent in performance; particularly, the film is uniform in thickness, continuous and dense and is applicable to the photoelectric and chemical fields.
Description
Technical field
The present invention relates to a kind of aluminum oxide precursor liquid solution, its preparation method and this solution and prepare the application in aluminum oxide and aluminum oxide film.
Background technology
Aluminum oxide is a kind of ideal oxide material, there is strong volume effect, quantum size effect, surface effects and macro quanta tunnel effect, in optical, electrical, thermodynamics and chemical reaction etc. are many, show a series of excellent properties, are widely used as the fields such as fine ceramics, matrix material, fluorescent material, moisture-sensitive sensor and infrared absorbing material.Aluminum oxide film has nontoxic, good specific inductivity and chemical stability, and low surface density of states, have a wide range of applications at photoelectric field and chemical field, as Photon-Electron electrons devices such as solar cell, thin film transistor, detector, flash memory, storer, electrical condenser, phase inverter, photodiodes, and chemical catalyst etc.
Preparation method to material, the particularly characteristic important of thin-film material.At present, the method for the preparation of aluminum oxide and aluminum oxide film has ald (atomic layer deposition), chemical vapour deposition (chemical vapour deposition), laser deposition (plus vapour deposition), plasma to strengthen ald (plasma-enhanced atomic-layer-deposition), magnetron sputtering (magnetron sputtering) and sol-gel method (sol-gel).Wherein the raw materials used price of sol-gel method is high, organic solvent is toxic, and need high temperature (>=300 DEG C) heat treated, this not only increases the consumption of the energy, and add complicacy prepared by production cost and technique, especially, in the middle of the preparation of flexible aluminum oxide film product, pyroprocessing seriously reduces the use properties of material; Remaining preparation method's process is complicated, and preparation temperature is high, and starting material loss is large, and production cost is high.Pass through solution methods, namely oxide precursor liquid solution is first prepared again through heat treatment process, obtain metal oxide and there is many-sided advantages such as energy consumption is little, production cost is low, preparation technology is simple, wherein the preparation technology of preparation to oxide compound of precursor solution plays decisive action.
Before the present invention makes, Xia discloses a kind of Al
2o
3the preparation method of film: nitric hydrate al dissolution is formed precursor solution in ethylene glycol monomethyl ether, by method of spin coating, precursor solution is formed film, then carries out annealing to film and forms Al at 600 DEG C
2o
3film, the thermal treatment temp of this preparation method is higher, and the height of thermal treatment temp directly has influence on the range of application of aluminum oxide film (see Xia.D.X; Xu.J.B. High mobility and low operating voltage ZnGaO and ZnGaLiO transistors with spin-coated Al2O3 as gate dielectric. J.Phys.D:Appl.Phys. 2,010 43 (44): 442001); Chinese patent CN 102787309A discloses a kind of preparation method of aluminum oxide film, first the persursor material containing aluminum metal ion and stablizer are dissolved in solvent and form precursor solution, post-heating prepare film, its raw material consumption is large, most importantly preparation temperature is high, need to reach 300 DEG C even 500 DEG C, or at least process 100 minutes at 200 DEG C, and obtain the poor-performing of product.
So, develop a kind of aluminum oxide precursor liquid solution, with simple, low temperature, safety prepare aluminum oxide and aluminum oxide film is necessary.
The solvability of the Burow Solution powder prepared in prior art in deionized water and alcoholic solvent (ethanol, Virahol, 2-methyl cellosolve etc.) is very poor, film cannot be prepared by solution method, aluminum oxide can not be decomposed to form at lower than the temperature of 200 DEG C; Burow Solution prepared by the present invention is colloidal, deionized water, acetone and alcoholic solvent (as: methyl alcohol, ethanol, ethylene glycol, glycerol, Virahol, 2-methyl cellosolve etc.) can be dissolved in, the Burow Solution colloid of fresh preparation is joined in above-mentioned solvent and shake or stir 8 ~ 12 hours, Burow Solution fully can be hydrolyzed or form the hydrolysates such as class alkoxide with alcoholic solvent, method can be decomposed to form aluminum oxide at low temperatures thus, and prepares aluminum oxide film.
The invention also discloses above-mentioned aluminum oxide precursor liquid solution and prepare the application in aluminum oxide.
The present invention further discloses above-mentioned aluminum oxide precursor liquid solution and prepare the application in aluminum oxide film.
In the present invention, aluminum oxide and aluminum oxide film can be obtained by heating described aluminum oxide precursor liquid solution at 150 ~ 180 DEG C.Prepare aluminum oxide film and can adopt spin-coating method, spray ink Printing printing technology method or doctor-blade casting process.For the aluminum oxide film preparing different thickness, can realize by regulating the concentration of presoma.
Because technique scheme is used, the present invention compared with prior art has following advantages:
1. the raw material sources of the present invention's employing are extensive, and cheap, preparation temperature is low, and the efficient rate of material is high, and energy consumption is little, significantly can reduce industrial production cost.
2. the alumina precursor solution shelf-life of the present invention's exploitation reaches the several months, excellent performance even, continuous, fine and close by the aluminum oxide film film thickness of its low-temperature growth.
3. the aluminum oxide precursor liquid solution of the present invention's exploitation is applicable to various film, operates simple and easy, is conducive to suitability for industrialized production.
Summary of the invention
The object of the invention is to provide a kind of aluminum oxide precursor liquid solution and preparation method thereof, is obtained aluminum oxide and the aluminum oxide film mould material of excellent properties by this precursor solution low-temperature growth.
For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of aluminum oxide precursor liquid solution, comprises the steps:
A Glacial acetic acid heats 20 ~ 30 minutes in 100 ~ 120 DEG C by (), then add Aluminum chloride anhydrous, obtains translucent Burow Solution colloid in 100 ~ 120 DEG C of reactions after 8 ~ 10 minutes; The mass ratio of Aluminum chloride anhydrous and Glacial acetic acid is 1: 5 ~ 10;
B above-mentioned Burow Solution colloid is put into supercentrifuge by (), after 6000 ~ 8000rpm is centrifugal 10 ~ 15 minutes, obtain Burow Solution particle;
C Burow Solution particle in step (b) is put into deionized water, acetone or alcoholic solvent by (), be mixed with the solution that mass concentration is 20% ~ 40%, and concussion or stirring are described aluminum oxide precursor liquid solution for 8 ~ 12 hours.
In preferred technical scheme, in above-mentioned steps (a), the mass ratio of Aluminum chloride anhydrous and Glacial acetic acid is 1: 6.
In technique scheme, in described step (c), alcoholic solvent is selected from the one in 2-methyl cellosolve, methyl alcohol, ethanol, ethylene glycol, glycerol, Virahol.
In preferred technical scheme, in above-mentioned steps (c), solution also comprises thanomin; Described thanomin is monoethanolamine, diethanolamine or trolamine.Thanomin is water white thick liquid, in weakly alkaline, has extremely strong water absorbability, can absorb sour gas, and the air release that can will absorb again after heating, has emulsification and bubble, can generate salt with mineral acid and organic acid.So, in above-mentioned aluminum oxide precursor liquid solution, add appropriate thanomin, on the one hand can in and acid ion in precursor solution, facilitate the hydrolysis of Burow Solution to a certain extent; The stability of precursor solution can be strengthened on the other hand; Most importantly the continuity preparing aluminum oxide film and compactness can be improved.
Accompanying drawing explanation
Fig. 1 is the x-ray photoelectron energy spectrogram of ultra-thin (thickness the is less than 2nm) aluminum oxide film after room temperature in embodiment six, 120 DEG C of process;
Fig. 2 is the x-ray photoelectron energy spectrogram of ultra-thin (thickness the is less than 2nm) aluminum oxide film in embodiment six after 150 DEG C, 180 DEG C process;
Fig. 3 is ITO ultraviolet photoelectron spectroscopy (UPS) figure of ultra-thin (thickness is less than 2nm) the aluminum oxide film modified in embodiment six after 150 DEG C of process;
Fig. 4 is the x-ray photoelectron energy spectrogram of three kinds of aluminum oxide films in embodiment seven;
Fig. 5 is that the x-ray photoelectron power spectrum of three kinds of aluminum oxide films in embodiment seven carefully composes swarming figure;
Fig. 6 is the scanning electron microscope diagram of ultra-thin (thickness is less than 2nm) aluminum oxide film at embodiment eight different treatment temperature and ito glass;
Fig. 7 is 180 DEG C of process 30 minutes and the atomic force microscope figure of 40 minutes rear oxidation aluminium films in embodiment nine;
Fig. 8 is 180 DEG C of process 50 minutes and the atomic force microscope figure of 60 minutes rear oxidation aluminium films in embodiment nine;
Fig. 9 is 180 DEG C of process 30 minutes and the atomic force microscope three-dimensional plot of 40 minutes rear oxidation aluminium films in embodiment nine;
Figure 10 is 180 DEG C of process 50 minutes and the atomic force microscope three-dimensional plot of 60 minutes rear oxidation aluminium films in embodiment nine.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the invention will be further described:
Embodiment one
The preparation of aluminum oxide precursor liquid solution, comprises the steps:
A 60ml Glacial acetic acid heats 30 minutes in 100 DEG C by (), then add 7g Aluminum chloride anhydrous, obtains translucent Burow Solution colloid in 120 DEG C of reactions after 8 minutes;
B above-mentioned Burow Solution colloid is put into supercentrifuge by (), after 8000rpm is centrifugal 10 minutes, obtain Burow Solution particle;
C Burow Solution particle (3g) in step (b) is put into 10ml 2-methyl cellosolve and is fully dissolved by (), be mixed with aluminum oxide precursor liquid solution.
Embodiment two
The preparation of aluminum oxide precursor liquid solution, comprises the steps:
A 60ml Glacial acetic acid heats 30 minutes in 100 DEG C by (), then add 7g Aluminum chloride anhydrous, obtains translucent Burow Solution colloid in 120 DEG C of reactions after 8 minutes;
B above-mentioned Burow Solution colloid is put into supercentrifuge by (), after 8000rpm is centrifugal 10 minutes, obtain Burow Solution particle;
C Burow Solution particle (2g) in step (b) is put into 10ml 2-methyl cellosolve and is fully dissolved by (), then add 30 μ l thanomins and be mixed with aluminum oxide precursor liquid solution.
Embodiment three
The preparation of aluminum oxide precursor liquid solution, comprises the steps:
A 60ml Glacial acetic acid heats 20 minutes in 120 DEG C by (), then add 10g Aluminum chloride anhydrous, obtains translucent Burow Solution colloid in 100 DEG C of reactions after 10 minutes;
B above-mentioned Burow Solution colloid is put into supercentrifuge by (), after 6000rpm is centrifugal 15 minutes, obtain Burow Solution particle;
C Burow Solution particle (1.5g) in step (b) is put into 10ml 2-methyl cellosolve and is fully dissolved by (), be mixed with aluminum oxide precursor liquid solution.
Embodiment four
The preparation of aluminum oxide precursor liquid solution, comprises the steps:
A 60ml Glacial acetic acid heats 20 minutes in 120 DEG C by (), then add 10g Aluminum chloride anhydrous, obtains translucent Burow Solution colloid in 100 DEG C of reactions after 10 minutes;
B above-mentioned Burow Solution colloid is put into supercentrifuge by (), after 6000rpm is centrifugal 15 minutes, obtain Burow Solution particle;
C Burow Solution particle (100mg) in step (b) is put into 10ml 2-methyl cellosolve and is fully dissolved by (), then add 40 μ l thanomins and be mixed with aluminum oxide precursor liquid solution.
Embodiment five
The preparation of alumina powder: the aluminum oxide precursor liquid solution in embodiment one or embodiment two is put into opening pottery, puts into baking box 180 DEG C of heat treated and namely obtains alumina particle after 80 minutes.
Embodiment six
The preparation of aluminum oxide film, comprising: be spin-coated on by the aluminum oxide precursor liquid solution in embodiment four in electroconductive indium tin oxide (ITO) substrate of glass, rotating speed is 4500 ~ 5000r/m, and spin-coating time is 40 seconds; Spin coating is got rid of after film completes, at once by film respectively at room temperature, anneal 10 minutes at 120 DEG C, 150 DEG C, 180 DEG C, obtain four kinds of ultra-thin (thickness is less than 2nm) aluminum oxide films, carry out the test of x-ray photoelectron power spectrum respectively.
Accompanying drawing 1, accompanying drawing 2 are the XPS figure of ultra-thin (thickness the is less than 2nm) aluminum oxide film under above-mentioned treatment of different temperature, and therefrom can find out, the peak of about 400 eV in the xps energy spectrum figure under greenhouse is N 1s, comes from thanomin; On the xps energy spectrum figure of other annealing temperatures (120 DEG C, 150 DEG C, 180 DEG C), thanomin disappears.The aluminium element of aluminum oxide and the ratio of oxygen element can be calculated by spectrogram: by the aluminium element (Al) of 150 DEG C of anneal aluminum oxide of 10 minutes and the ratio of oxygen element (O) be: n (Al): n (O)=1: 1.55 from the XPS accompanying drawing 2; By the aluminium element (Al) of 180 DEG C of anneal aluminum oxide of 10 minutes and the ratio of oxygen element (O) be: n (Al): n (O)=1: 1.46.
Accompanying drawing 3 is ITO ultraviolet photoelectron spectroscopy (UPS) figure of ultra-thin (thickness is less than 2nm) aluminum oxide film modified, wherein annealing temperature 150 DEG C, anneal 10 minutes, can find out and to be tested by ultraviolet photo-electron spectrometer, the ITO work function of aluminum oxide film modified is 3.9 ± 0.05 eV, and the work function much smaller than electroconductive indium tin oxide (ITO) distributes (4.7 ~ 5.1 eV).
Embodiment seven
The preparation of aluminum oxide film, comprising: be spin-coated on by the aluminum oxide precursor liquid solution in embodiment three in silicon (Si) substrate, rotating speed is 3000 r/m, and spin-coating time is 30 seconds; Spin coating is got rid of after film completes, at once by film respectively at anneal at 120 DEG C, 150 DEG C, 180 DEG C 30 minutes, obtain three kinds of aluminum oxide films, carry out photoelectron spectrum test respectively.
Accompanying drawing 4 is the XPS figure of the aluminum oxide film under above-mentioned three kinds of Temperature Treatment, and therefrom can find out, aluminum oxide is formed; Accompanying drawing 5 is that the XPS of aluminum oxide film under above-mentioned three kinds of Temperature Treatment carefully composes swarming figure, and can find out that Al 2p peak only has a peak, O 1s peak can be divided into 3 peaks.
By reference to the accompanying drawings 4 and accompanying drawing 5 can calculate the ratio of aluminium element and oxygen element: within 30 minutes, process by 120 DEG C of annealing the aluminium element (Al) of aluminum oxide that obtains and the ratio of oxygen element (O) is: n (Al): n (O)=1: 1.98; The aluminium element (Al) of aluminum oxide obtained by 150 DEG C of annealing process in 30 minutes and the ratio of oxygen element (O) are: n (Al): n (O)=1: 1.65; The aluminium element (Al) of aluminum oxide obtained by 180 DEG C of annealing 30 divisional processing and the ratio of oxygen element (O) are: n (Al): n (O)=1: 1.49.So this programme prepares aluminum oxide and aluminum oxide film under can be implemented in cold condition.
Embodiment eight
The preparation of aluminum oxide film, comprising: be spin-coated on by the aluminum oxide precursor liquid solution in embodiment four in electroconductive indium tin oxide (ITO) substrate of glass, rotating speed is 4500 ~ 5000r/m, and spin-coating time is 40 seconds; Spin coating is got rid of after film completes, at once by film respectively at anneal at 150 DEG C, 180 DEG C, 200 DEG C 10 minutes, obtain three kinds of aluminum oxide films, film thickness is less than 2nm, carries out scanning electron microscope test respectively.
Accompanying drawing 6 is the SEM figure of ultra-thin (thickness is less than 2nm) aluminum oxide film at above-mentioned different treatment temperature and ito glass, a, b, c, d are respectively the aluminum oxide film after ito glass and 150 DEG C, 180 DEG C, 200 DEG C process, therefrom can find out that the continuity of the film of 150 DEG C of annealing after 10 minutes, compactness are best.
Embodiment nine
The preparation of aluminum oxide film, comprising: be spin-coated on by the aluminum oxide precursor liquid solution in embodiment three in silicon (Si) substrate, rotating speed is 3000 r/m, and spin-coating time is 30 seconds; Spin coating is got rid of after film completes, and at once by film anneal 30 minutes, 40 minutes, 50 minutes, 60 minutes at 180 DEG C, obtain four kinds of aluminum oxide films, film thickness is about 40nm, carries out atomic force microscope test respectively.
Accompanying drawing 7, accompanying drawing 8 are the atomic force microscope figure of the aluminum oxide film under above-mentioned different treatment condition, accompanying drawing 9, accompanying drawing 10 are the atomic force microscope three-dimensional plot of the aluminum oxide film under above-mentioned different treatment condition, can find out that aluminum oxide film has lower roughness (Rms) in conjunction with 4 width figure, be 0.545nm to the maximum.
According to above analysis, the present invention can prepare at low temperatures different thickness, continuous print, fine and close, high-quality aluminum oxide and aluminum oxide film.
At above-mentioned 180 DEG C, the anneal aluminum oxide film of 30 minutes prepares Pentacene thin film transistors as insulation dielectric layer, through test: the leakage current of aluminum oxide film is less than 0.1 nA, and operating voltage is less than-3 V, charge field effect mobility
μ fE>=2 cm
2/ Vs, and on-off ratio is greater than 10
5.Can find out, alumina material of the present invention can realize the functions such as low voltage, less energy-consumption, high on-off ratio as the thin film transistor of insulation dielectric layer.
Claims (7)
1. a preparation method for aluminum oxide precursor liquid solution, is characterized in that, comprises the steps:
A Glacial acetic acid heats 20 ~ 30 minutes in 100 ~ 120 DEG C by (), then add Aluminum chloride anhydrous, obtains translucent Burow Solution colloid in 100 ~ 120 DEG C of reactions after 8 ~ 10 minutes; The mass ratio of Aluminum chloride anhydrous and Glacial acetic acid is 1: 5 ~ 10;
B above-mentioned Burow Solution colloid is put into supercentrifuge by (), after 6000 ~ 8000rpm is centrifugal 10 ~ 15 minutes, obtain Burow Solution particle;
C Burow Solution particle in step (b) is put into deionized water, acetone or alcoholic solvent by (), add thanomin again, be mixed with the solution that Burow Solution mass concentration is 20% ~ 40%, concussion or stirring are described aluminum oxide precursor liquid solution for 8 ~ 12 hours.
2. preparation method according to claim 1, is characterized in that: in described step (a), the mass ratio of Aluminum chloride anhydrous and Glacial acetic acid is 1: 6.
3. preparation method according to claim 1, is characterized in that: in described step (c), alcoholic solvent is selected from the one in 2-methyl cellosolve, methyl alcohol, ethanol, ethylene glycol, glycerol, Virahol.
4. preparation method according to claim 1, is characterized in that: described thanomin is monoethanolamine, diethanolamine or trolamine.
5. the aluminum oxide precursor liquid solution prepared by any one method of Claims 1 to 4.
6. aluminum oxide precursor liquid solution according to claim 5 is preparing the application in aluminum oxide, it is characterized in that: temperature when preparing aluminum oxide is 150 ~ 180 DEG C.
7. aluminum oxide precursor liquid solution according to claim 5 is preparing the application in aluminum oxide film, it is characterized in that: temperature when preparing aluminum oxide film is 150 ~ 180 DEG C.
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| CN105161415B (en) * | 2015-08-31 | 2018-06-22 | 上海集成电路研发中心有限公司 | High dielectric constant film-aluminium oxide laminated construction insulation film and preparation method thereof |
| CN106216212A (en) * | 2016-07-27 | 2016-12-14 | 王虹 | The preparation technology of anti-bacteria stainless steel |
| CN107722427A (en) * | 2017-10-30 | 2018-02-23 | 杭州富阳鼎创科技有限公司 | A kind of wearability polythene material and preparation method thereof |
| CN109980097B (en) * | 2017-12-27 | 2020-08-18 | Tcl科技集团股份有限公司 | Preparation method of thin film and QLED device |
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| CN1884398A (en) * | 2005-06-21 | 2006-12-27 | 中国科学院合肥物质科学研究院 | Alumina insulating coating and its preparation method |
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| CN101717257A (en) * | 2009-12-01 | 2010-06-02 | 西安交通大学 | Technology of preparing aluminium oxide based continuous fibers by sol-gel process |
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