CN103194741A - 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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- CN103194741A CN103194741A CN2013101155838A CN201310115583A CN103194741A CN 103194741 A CN103194741 A CN 103194741A CN 2013101155838 A CN2013101155838 A CN 2013101155838A CN 201310115583 A CN201310115583 A CN 201310115583A CN 103194741 A CN103194741 A CN 103194741A
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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 the application in preparation aluminum oxide and aluminum oxide film of a kind of aluminum oxide precursor liquid solution, its preparation method and this solution.
Background technology
Aluminum oxide is a kind of very desirable oxide material, have strong volume effect, quantum size effect, surface effects and macro quanta tunnel effect, show a series of excellent properties at light, electricity, thermodynamics and chemical reaction etc. aspect many, be widely used as fields such as fine ceramics, matrix material, fluorescent material, wet quick property 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 photoelectricity electron devices such as solar cell, thin film transistor, detector, flash memory, storer, electrical condenser, phase inverter, photodiodes, and chemical catalyst etc.
The preparation method is to material, and particularly the characteristic of thin-film material has material impact.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).The raw materials used price height of sol-gel method wherein, organic solvent is toxic, and need high temperature (〉=300 ℃) heat treated, this has not only strengthened the consumption of the energy, and increased the complicacy of production cost and prepared, especially in the middle of the preparation of flexible aluminum oxide film product, pyroprocessing has seriously reduced the use properties of material; Remaining preparation method's process complexity, the preparation temperature height, the starting material loss is big, the production cost height.Pass through solution methods, namely preparation oxide precursor liquid solution passes through heat treatment process more earlier, obtain metal oxide and have many-sided advantages such as energy consumption is little, production cost is low, preparation technology is simple, wherein the preparation of precursor solution plays decisive action to the preparation technology of oxide compound.
Before the present invention made, Xia disclosed a kind of Al
2O
3The preparation method of film: the nitric hydrate al dissolution is formed precursor solution in ethylene glycol monomethyl ether, by method of spin coating precursor solution is formed film, under 600 ℃ film being annealed then forms Al
2O
3Film, this preparation method's thermal treatment temp is higher, and the height of thermal treatment temp directly has influence on the range of application of aluminum oxide film (referring to 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, to contain the persursor material of aluminum metal ion and stablizer earlier is dissolved in and forms precursor solution in the solvent, add the hot preparation film afterwards, its raw material consumption is big, most importantly preparation temperature height, need reach 300 ℃ even 500 ℃, perhaps handle 100 minutes at least under 200 ℃, and obtain the poor-performing of product.
So, develop a kind of aluminum oxide precursor liquid solution, necessary with preparation aluminum oxide and the aluminum oxide film of simple, low temperature, safety.
Summary of the invention
The object of the invention provides a kind of aluminum oxide precursor liquid solution and preparation method thereof, prepares aluminum oxide and the aluminum oxide film mould material of excellent properties by this precursor solution low temperature.
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) with Glacial acetic acid in 100～120 ℃ of heating 20～30 minutes, add Aluminum chloride anhydrous again, obtain translucent Burow Solution colloid in 100～120 ℃ 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, after 6000～8000rpm is centrifugal 10～15 minutes, obtain the Burow Solution particle;
(c) the Burow Solution particle in the step (b) is put into deionized water, acetone or alcoholic solvent, be mixed with mass concentration and be 20%～40% solution, shake or stir and be described aluminum oxide precursor liquid solution in 8～12 hours.
In the optimized technical scheme, the mass ratio of Aluminum chloride anhydrous and Glacial acetic acid is 1: 6 in the above-mentioned steps (a).
In the technique scheme, alcoholic solvent is selected from a kind of in 2-methyl cellosolve, methyl alcohol, ethanol, ethylene glycol, glycerol, the Virahol in the described step (c).
In the optimized technical scheme, solution also comprises thanomin in the above-mentioned steps (c); Described thanomin is monoethanolamine, diethanolamine or trolamine.Thanomin is water white thick liquid, is weakly alkaline, and extremely strong water absorbability is arranged, and can absorb sour gas, the gas that absorbs can be discharged again after the heating, and emulsification and bubble effect are arranged, and can generate salt with mineral acid and organic acid.So, in above-mentioned aluminum oxide precursor liquid solution, add adequate amount of ethanol amine, on the one hand can in and the acid ion in the precursor solution, promoted the hydrolysis of Burow Solution to a certain extent; Can strengthen the stability of precursor solution on the other hand; Of paramount importance is continuity and the compactness that can improve the preparation aluminum oxide film.
The solvability of the Burow Solution powder for preparing in the prior art in deionized water and alcoholic solvent (ethanol, Virahol, 2-methyl cellosolve etc.) is very poor, can't use the solution thin films, can not be decomposed to form aluminum oxide being lower than under 200 ℃ the temperature; The Burow Solution of the present invention's preparation is colloidal, can be dissolved in deionized water, acetone and alcoholic solvent (as: methyl alcohol, ethanol, ethylene glycol, glycerol, Virahol, 2-methyl cellosolve etc.), the Burow Solution colloid of prepared fresh is joined in the above-mentioned solvent concussion or stirred 8～12 hours, Burow Solution fully hydrolysis or and alcoholic solvent form hydrolysates such as class alkoxide, method can be decomposed to form aluminum oxide at low temperatures thus, and the preparation aluminum oxide film.
The invention also discloses the application of above-mentioned aluminum oxide precursor liquid solution in the preparation aluminum oxide.
The present invention further discloses the application of above-mentioned aluminum oxide precursor liquid solution in the preparation aluminum oxide film.
Among the present invention, can obtain aluminum oxide and aluminum oxide film by heating described aluminum oxide precursor liquid solution down at 150～180 ℃.The preparation aluminum oxide film can adopt spin-coating method, spray ink Printing printing technology method or doctor-blade casting process.For the aluminum oxide film of preparation different thickness, can realize by the concentration of regulating presoma.
Because technique scheme is used, the present invention compared with prior art has following advantage:
1. the raw material sources of the present invention's employing are extensive, cheap, and preparation temperature is low, the efficient rate height of using of material, and energy consumption is little, can significantly reduce industrial production cost.
2. the aluminum oxide precursor liquid solution long preservative period 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 preparation.
3. the aluminum oxide precursor liquid solution of the present invention exploitation is fit to various films, operates simple and easyly, is conducive to suitability for industrialized production.
Description of drawings
Fig. 1 is that the x-ray photoelectron of ultra-thin (thickness is less than the 2nm) aluminum oxide film after room temperature among the embodiment six, the 120 ℃ of processing can spectrogram;
Fig. 2 is that the x-ray photoelectron of ultra-thin (thickness is less than 2nm) aluminum oxide film after 150 ℃, 180 ℃ processing among the embodiment six can spectrogram;
Fig. 3 is ITO ultraviolet photoelectron spectroscopy (UPS) figure of ultra-thin (thickness is less than 2nm) aluminum oxide film modified after 150 ℃ of processing among the embodiment six;
Fig. 4 is the x-ray photoelectron energy spectrogram of three kinds of aluminum oxide films among the embodiment seven;
Fig. 5 carefully composes swarming figure for the x-ray photoelectron power spectrum of three kinds of aluminum oxide films among the embodiment seven;
Fig. 6 is ultra-thin (thickness is less than 2nm) aluminum oxide film under the embodiment eight different treatment temperature and the scanning electron microscope diagram of ito glass;
Fig. 7 be among the embodiment nine 180 ℃ handle 30 minutes atomic force microscope figure with 40 minutes rear oxidation aluminium films;
Fig. 8 be among the embodiment nine 180 ℃ handle 50 minutes atomic force microscope figure with 60 minutes rear oxidation aluminium films;
Fig. 9 be among the embodiment nine 180 ℃ handle 30 minutes atomic force microscope three-dimensional plot with 40 minutes rear oxidation aluminium films;
Figure 10 be among the embodiment nine 180 ℃ handle 50 minutes atomic force microscope three-dimensional plot with 60 minutes rear oxidation aluminium films.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is further described:
Embodiment one
The preparation of aluminum oxide precursor liquid solution comprises the steps:
(a) with the 60ml Glacial acetic acid in 100 ℃ of heating 30 minutes, add the 7g Aluminum chloride anhydrous again, obtain translucent Burow Solution colloid in 120 ℃ of reactions after 8 minutes;
(b) above-mentioned Burow Solution colloid is put into supercentrifuge, after 8000rpm is centrifugal 10 minutes, obtain the Burow Solution particle;
(c) the Burow Solution particle (3g) in the step (b) is put into the 10ml 2-methyl cellosolve and fully dissolve, be mixed with the aluminum oxide precursor liquid solution.
Embodiment two
The preparation of aluminum oxide precursor liquid solution comprises the steps:
(a) with the 60ml Glacial acetic acid in 100 ℃ of heating 30 minutes, add the 7g Aluminum chloride anhydrous again, obtain translucent Burow Solution colloid in 120 ℃ of reactions after 8 minutes;
(b) above-mentioned Burow Solution colloid is put into supercentrifuge, after 8000rpm is centrifugal 10 minutes, obtain the Burow Solution particle;
(c) the Burow Solution particle (2g) in the step (b) is put into the 10ml 2-methyl cellosolve and fully dissolve, add 30 μ l thanomins again and be mixed with the aluminum oxide precursor liquid solution.
Embodiment three
The preparation of aluminum oxide precursor liquid solution comprises the steps:
(a) with the 60ml Glacial acetic acid in 120 ℃ of heating 20 minutes, add the 10g Aluminum chloride anhydrous again, obtain translucent Burow Solution colloid in 100 ℃ of reactions after 10 minutes;
(b) above-mentioned Burow Solution colloid is put into supercentrifuge, after 6000rpm is centrifugal 15 minutes, obtain the Burow Solution particle;
(c) the Burow Solution particle (1.5g) in the step (b) is put into the 10ml 2-methyl cellosolve and fully dissolve, be mixed with the aluminum oxide precursor liquid solution.
Embodiment four
The preparation of aluminum oxide precursor liquid solution comprises the steps:
(a) with the 60ml Glacial acetic acid in 120 ℃ of heating 20 minutes, add the 10g Aluminum chloride anhydrous again, obtain translucent Burow Solution colloid in 100 ℃ of reactions after 10 minutes;
(b) above-mentioned Burow Solution colloid is put into supercentrifuge, after 6000rpm is centrifugal 15 minutes, obtain the Burow Solution particle;
(c) the Burow Solution particle (100mg) in the step (b) is put into the 10ml 2-methyl cellosolve and fully dissolve, add 40 μ l thanomins again and be mixed with the aluminum oxide precursor liquid solution.
Embodiment five
The preparation of alumina powder: the aluminum oxide precursor liquid solution among embodiment one or the embodiment two is put into the opening pottery, put into 180 ℃ of heat treated of baking box and namely obtain alumina particle after 80 minutes.
Embodiment six
The preparation of aluminum oxide film comprises: the aluminum oxide precursor liquid solution among the embodiment four is spin-coated on electroconductive indium tin oxide (ITO) substrate of glass, and rotating speed is 4500～5000r/m, and the spin coating time is 40 seconds; After spin coating is got rid of film and is finished, at once with film respectively at room temperature, 120 ℃, 150 ℃, 180 ℃ following anneal 10 minutes, 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 is less than the 2nm) aluminum oxide film under the above-mentioned treatment of different temperature, and therefrom as can be seen, the peak about 400 eV among the xps energy spectrum figure under the greenhouse is N 1s, comes from thanomin; On the xps energy spectrum figure of other annealing temperatures (120 ℃, 150 ℃, 180 ℃), thanomin disappears.XPS energy spectrogram from accompanying drawing 2 can calculate the ratio of aluminium element and the oxygen element of aluminum oxide: by the aluminium element (Al) of 10 minutes aluminum oxide of 150 ℃ of anneal and the ratio of oxygen element (O) be: n (Al): n (O)=1: 1.55; By the aluminium element (Al) of 10 minutes aluminum oxide of 180 ℃ of anneal 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 150 ℃ of annealing temperatures, anneal 10 minutes, test by ultraviolet photo-electron spectrometer as can be seen, the ITO work function of aluminum oxide film modified is 3.9 ± 0.05 eV, much smaller than the work function distribution (4.7～5.1 eV) of electroconductive indium tin oxide (ITO).
Embodiment seven
The preparation of aluminum oxide film comprises: the aluminum oxide precursor liquid solution among the embodiment three is spin-coated in silicon (Si) substrate, and rotating speed is 3000 r/m, and the spin coating time is 30 seconds; After spin coating is got rid of film and is finished, at once with film respectively at 120 ℃, 150 ℃, 180 ℃ following anneal 30 minutes, obtain three kinds of aluminum oxide films, carry out the 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 as can be seen, aluminum oxide forms; Accompanying drawing 5 is carefully composed swarming figure for the XPS of the aluminum oxide film under above-mentioned three kinds of Temperature Treatment, and Al 2p has only at the peak peak as can be seen, and 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: handled the aluminium element (Al) of the aluminum oxide that obtains in 30 minutes and the ratio of oxygen element (O) is: n (Al): n (O)=1: 1.98 by 120 ℃ of annealing; Handled the aluminium element (Al) of the aluminum oxide obtain in 30 minutes and the ratio of oxygen element (O) is: n (Al): n (O)=1: 1.65 by 150 ℃ of annealing; By the aluminium element (Al) of 180 ℃ of aluminum oxide of obtaining of annealing 30 divisional processing and the ratio of oxygen element (O) be: n (Al): n (O)=1: 1.49.So this programme can be implemented in preparation aluminum oxide and aluminum oxide film under the cold condition.
Embodiment eight
The preparation of aluminum oxide film comprises: the aluminum oxide precursor liquid solution among the embodiment four is spin-coated on electroconductive indium tin oxide (ITO) substrate of glass, and rotating speed is 4500～5000r/m, and the spin coating time is 40 seconds; After spin coating is got rid of film and is finished, at once with film respectively at 150 ℃, 180 ℃, 200 ℃ following anneal 10 minutes, obtain three kinds of aluminum oxide films, film thickness carries out scanning electron microscope test respectively less than 2nm.
Accompanying drawing 6 is the SEM figure of ultra-thin (thickness is less than 2nm) aluminum oxide film under the above-mentioned different treatment temperature and ito glass, a, b, c, d are respectively the aluminum oxide film after ito glass and 150 ℃, 180 ℃, the 200 ℃ processing, and therefrom continuity, the compactness of the film of 150 ℃ of annealing after 10 minutes are best as can be seen.
Embodiment nine
The preparation of aluminum oxide film comprises: the aluminum oxide precursor liquid solution among the embodiment three is spin-coated in silicon (Si) substrate, and rotating speed is 3000 r/m, and the spin coating time is 30 seconds; After spin coating is got rid of film and is finished, at once with film in 180 ℃ of following anneal 30 minutes, 40 minutes, 50 minutes, 60 minutes, obtain four kinds of aluminum oxide films, film thickness is about 40nm, carries out the atomic force microscope test respectively.
Accompanying drawing 7, accompanying drawing 8 are the atomic force microscope figure of the aluminum oxide film under the 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 the above-mentioned different treatment condition, in conjunction with 4 width of cloth figure as can be seen aluminum oxide film have lower roughness (Rms), be 0.545nm to the maximum.
According to above analysis, that the present invention can prepare at low temperatures is different thickness, continuous, fine and close, high-quality aluminum oxide and aluminum oxide film.
Prepare Pentacene thin film transistors with 30 minutes aluminum oxide film of above-mentioned 180 ℃ of following anneal 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, the charge field effect mobility
μ FE〉=2 cm
2/ Vs, and on-off ratio is greater than 10
5As can be seen, alumina material of the present invention can be realized functions such as low voltage, less energy-consumption, high on-off ratio as the thin film transistor of insulation dielectric layer.
Claims (9)
1. the preparation method of an aluminum oxide precursor liquid solution is characterized in that, comprises the steps:
(a) with Glacial acetic acid in 100～120 ℃ of heating 20～30 minutes, add Aluminum chloride anhydrous again, obtain translucent Burow Solution colloid in 100～120 ℃ 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, after 6000～8000rpm is centrifugal 10～15 minutes, obtain the Burow Solution particle;
(c) the Burow Solution particle in the step (b) is put into deionized water, acetone or alcoholic solvent, be mixed with mass concentration and be 20%～40% solution, shake or stir and be described aluminum oxide precursor liquid solution in 8～12 hours.
2. preparation method according to claim 1 is characterized in that: the mass ratio of Aluminum chloride anhydrous and Glacial acetic acid is 1: 6 in the described step (a).
3. preparation method according to claim 1 is characterized in that: alcoholic solvent is selected from a kind of in 2-methyl cellosolve, methyl alcohol, ethanol, ethylene glycol, glycerol, the Virahol in the described step (c).
4. preparation method according to claim 1 is characterized in that: solution also comprises thanomin in the described step (c).
5. preparation method according to claim 4, it is characterized in that: described thanomin is monoethanolamine, diethanolamine or trolamine.
6. the aluminum oxide precursor liquid solution that is prepared by any one method of claim 1～5.
7. the application of the described aluminum oxide precursor liquid solution of claim 6 in the preparation aluminum oxide.
8. the application of the described aluminum oxide precursor liquid solution of claim 6 in the preparation aluminum oxide film.
9. according to claim 7 or 8 described application, it is characterized in that: described preparation temperature is 150～180 ℃.
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| CN105161415A (en) * | 2015-08-31 | 2015-12-16 | 上海集成电路研发中心有限公司 | High dielectric constant thin film-aluminum oxide laminated structure insulating 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 |
| CN109980097A (en) * | 2017-12-27 | 2019-07-05 | Tcl集团股份有限公司 | A kind of preparation method of film and QLED device |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105161415A (en) * | 2015-08-31 | 2015-12-16 | 上海集成电路研发中心有限公司 | High dielectric constant thin film-aluminum oxide laminated structure insulating film and preparation method thereof |
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| 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 |
| CN109980097A (en) * | 2017-12-27 | 2019-07-05 | Tcl集团股份有限公司 | A kind of preparation method of film and QLED device |
| 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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