CN112225467B - Preparation method of ultra-smooth aluminum oxide film - Google Patents
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- CN112225467B CN112225467B CN202011114447.3A CN202011114447A CN112225467B CN 112225467 B CN112225467 B CN 112225467B CN 202011114447 A CN202011114447 A CN 202011114447A CN 112225467 B CN112225467 B CN 112225467B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
- H01L21/02172—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides
- H01L21/02175—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal
- H01L21/02178—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal the material containing aluminium, e.g. Al2O3
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
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- H—ELECTRICITY
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/214—Al2O3
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Abstract
The invention discloses a preparation method of an ultra-smooth aluminum oxide film, belonging to the technical field of film material preparation. The method comprises the following steps: dissolving aluminum sec-butoxide in water according to the proportion of 8-12 g/L, adjusting the pH value to 2-3 by nitric acid to obtain alumina sol, and aging the sol for 5 days for later use; adding zinc acetate powder into the sol according to the proportion of 3-10 g/L, stirring and dissolving, and taking and cleaning and drying the glass or silicon chip for later use; film coating: coating a film on the carrier by a pulling method, a spin coater, a coating or spraying method, drying at room temperature, and sintering by a muffle furnace to obtain the ultra-smooth alumina film. The method has simple process, is suitable for preparing various plane and curved super-smooth oxide films, and the prepared alumina film has no defects and cracks and has the surface granularity of 2nm.
Description
Technical Field
The invention relates to a preparation method of an ultra-smooth aluminum oxide film, belonging to the technical field of film material preparation.
Background
The alumina film has excellent physical and chemical properties, such as high mechanical strength and hardness, good thermal stability, strong corrosion resistance, transparency in a wide wavelength range, excellent insulating property and wide application in the fields of machinery, photochemistry and microelectronics. The current methods for preparing thin films of aluminum oxide are relatively mature, and thin layers of aluminum oxide can be deposited on a substrate by Atomic Layer Deposition (ALD) or metal organic chemical vapor deposition (MOVCD). ALD is performed by alternating the supply of aluminum and oxygen precursors that are required to be deposited on a substrate. Typical aluminum precursors are aluminum trichloride, trimethylaluminum, triethylaluminum, dimethylaluminum chloride, aluminum ethoxide, aluminum isopropoxide.
At present, the preparation of the aluminum oxide film is mainly focused on the porous aluminum oxide film, with the rapid development of precision, ultra-precision, photoelectron and nano processing technology, the requirement on the smooth surface of the aluminum oxide film is higher and higher, at present, the ultra-smooth surface is mainly realized by methods such as chemical polishing, mechanical polishing and the like, the processes are easy to damage the surface of the film, chemical pollution exists and the like, and the application of the film is limited. In view of the above defects in the prior art, it is necessary to design a method for preparing an ultra-smooth alumina thin film to avoid the generation of defects such as pinholes and cracks, thereby expanding the application of the alumina thin film.
Disclosure of Invention
In view of the above technical problems, the present invention aims to provide a method for preparing an ultra-smooth alumina thin film, which specifically comprises the following steps:
(1) Preparation of alumina sol: dissolving the secondary butanol aluminum in water according to the proportion of 8-12 g/L, adjusting the pH value to 2-3 by nitric acid to obtain alumina sol, and aging the sol for 5 days for later use.
(2) Adding zinc acetate powder into the sol according to the proportion of 3-10 g/L, stirring and dissolving, taking the glass or the silicon chip for cleaning and drying for later use.
(3) Film coating: coating a film on the carrier by a pulling method, a spin coater, a coating or spraying method, drying for 1 day at room temperature, and sintering by a muffle furnace to obtain the ultra-smooth alumina film.
Preferably, the preparation method of the alumina sol in the step (1) of the present invention comprises: adding the secondary butyl alcohol aluminum into distilled water at the temperature of 80-90 ℃, magnetically stirring for 25-35 min, adjusting the pH to 2-3 by using nitric acid, and magnetically stirring for 25-35 min at the temperature of 80-90 ℃ to obtain the alumina sol.
Preferably, the cleaning process of the glass or silicon carrying wafer comprises the following steps: washing with 100ml ethyl acetate, 100ml 95% ethanol, and 100ml deionized water in sequence in an ultrasonic instrument for 30min.
Preferably, the sintering conditions in step (3) of the present invention are: the initial temperature of sintering is 25 ℃, the heating rate is 1 ℃/min, the temperature is kept at 100 ℃ for 1h,200 ℃ for 1h,300 ℃ for 1h,400 ℃ for 1h and 500 ℃ for 5h.
The invention has the beneficial effects that:
(1) The alumina film prepared by the method has a smooth surface, infrared detection shows that the granularity of the film surface is only about 2nm, and the film surface has no cracks or defects.
(2) According to the invention, by adding the zinc acetate powder and controlling the heat treatment process, the reaction is milder and more sufficient, so that an ultra-smooth aluminum oxide film is obtained, the film material is flat and compact, the surface is uniform, the defects generated in the reaction process are reduced, and the film can be used as a functional film with good insulating property.
Drawings
FIG. 1 is an AFM image and associated data for the preparation of an ultra-smooth alumina film of example 1;
FIG. 2 is an AFM image and associated data for a general method of preparing an alumina film.
FIG. 3 is a photograph of a smooth film of aluminum oxide with a silicon wafer as the substrate;
fig. 4 is a photograph of a smooth film of alumina with a glass substrate.
Detailed Description
The present invention is further described in detail with reference to the following specific examples, but the scope of the present invention is not limited to the above description.
Example 1
A preparation method of an ultra-smooth alumina film specifically comprises the following steps:
(1) Preparation of alumina sol: adding aluminum sec-butoxide into distilled water at 80 deg.C, magnetically stirring for 25min, adjusting pH to 2 with nitric acid, magnetically stirring at 85 deg.C for 30min to obtain alumina sol, and aging for 5 days.
(2) Adding zinc acetate powder into the sol according to the proportion of 8g/L, stirring and dissolving, taking glass or silicon chip, sequentially cleaning the glass or silicon chip with 100ml of ethyl acetate, 100ml of 95% ethanol and 100ml of deionized water in an ultrasonic instrument for 30min, and drying for later use.
(3) Film coating: coating a film on a carrier by a pulling method, a spin coater, a coating or spraying method, drying for 1 day at room temperature, sintering by a muffle furnace, wherein the initial sintering temperature is 25 ℃, the heating rate is 1 ℃/min, the temperature is maintained at 100 ℃ for 1h, the temperature is maintained at 200 ℃ for 1h, the temperature is maintained at 300 ℃ for 1h, the temperature is maintained at 400 ℃ for 1h, and the temperature is maintained at 500 ℃ for 5h to obtain the ultra-smooth alumina film, as shown in figure 1, the surface crystal grain of the film is fine, the average roughness of the film is 2.973nm, the square root roughness is 3.849nm, and the smoothness of the film is high.
Example 2
A preparation method of an ultra-smooth alumina film specifically comprises the following steps:
(1) Preparation of alumina sol: adding aluminum sec-butoxide into 90 deg.C distilled water, magnetically stirring for 30min, adjusting pH to 3 with nitric acid, magnetically stirring at 80 deg.C for 35min to obtain alumina sol, and aging for 5 days.
(2) Adding zinc acetate powder into the sol according to the proportion of 3g/L, stirring and dissolving, taking glass or silicon chip, sequentially cleaning the glass or silicon chip with 100ml of ethyl acetate, 100ml of 95% ethanol and 100ml of deionized water in an ultrasonic instrument for 30min, and drying for later use.
(3) Film coating: coating a film on a carrier by a pulling method, a spin coater, a coating or spraying method, drying for 1 day at room temperature, sintering by a muffle furnace, wherein the initial sintering temperature is 25 ℃, the heating rate is 1 ℃/min, the temperature is maintained at 100 ℃ for 1h, the temperature is maintained at 200 ℃ for 1h, the temperature is maintained at 300 ℃ for 1h, the temperature is maintained at 400 ℃ for 1h, and the temperature is maintained at 500 ℃ for 5h to obtain the ultra-smooth aluminum oxide film. The surface crystal grains of the film prepared by the embodiment are fine, the average roughness of the film is 2.983nm, the square root roughness is 3.860nm, and the smoothness of the film is high.
Example 3
A preparation method of an ultra-smooth alumina film specifically comprises the following steps:
(1) Preparation of alumina sol: adding aluminum sec-butoxide into 85 deg.C distilled water, magnetically stirring for 35min, adjusting pH to 2 with nitric acid, magnetically stirring at 90 deg.C for 25min to obtain alumina sol, and aging for 5 days.
(2) Adding zinc acetate powder into the sol according to the proportion of 10g/L, stirring and dissolving, taking glass or silicon chip, sequentially cleaning the glass or silicon chip with 100ml of ethyl acetate, 100ml of 95% ethanol and 100ml of deionized water in an ultrasonic instrument for 30min, and drying for later use.
(3) Film coating: coating a film on a carrier by a pulling method, a spin coater, a coating or spraying method, drying for 1 day at room temperature, sintering by a muffle furnace, wherein the initial sintering temperature is 25 ℃, the heating rate is 1 ℃/min, the temperature is maintained at 100 ℃ for 1h, the temperature is maintained at 200 ℃ for 1h, the temperature is maintained at 300 ℃ for 1h, the temperature is maintained at 400 ℃ for 1h, and the temperature is maintained at 500 ℃ for 5h, so that the ultra-smooth alumina film is obtained. The surface crystal grains of the film prepared by the embodiment are fine, the average roughness of the film is 2.985nm, the root roughness of the film is 3.950nm, and the smoothness of the film is very high.
Comparative example 1
(1) Preparation of alumina sol: adding 24.6g of secondary butyl aluminum into 180g of distilled water at 85 ℃, magnetically stirring for 30min, adjusting the pH to 2 by using 6ml of nitric acid, magnetically stirring for 30min at 85 ℃ to obtain alumina sol, and aging the sol for 5 days for later use.
(2) Preparation of glass carrier: and (3) taking the carrier fragment, sequentially washing the carrier fragment with 100ml of ethyl acetate, 100ml of 95% ethanol and 100ml of deionized water in an ultrasonic instrument for 30min, and drying for later use.
(3) Film coating: coating a film on a carrier by a pulling method, a spin coater, a coating or spraying method, drying at room temperature for 1 day, sintering by a muffle furnace, wherein the initial sintering temperature is 25 ℃, the heating rate is 1 ℃/min, and the temperature is kept at 500 ℃ for 5 hours to obtain the alumina film, as shown in figure 2, the surface of the film has large crystal grains and is petal-shaped, the average roughness of the film is 42.64nm, the square root roughness is 52.55nm, and the surface of the film is rough.
Claims (3)
1. The preparation method of the ultra-smooth aluminum oxide film is characterized by comprising the following steps:
(1) Preparation of alumina sol: dissolving aluminum sec-butoxide in water according to the proportion of 8-12g/L, adjusting the pH to 2~3 by nitric acid to obtain alumina sol, and aging the sol for 5 days for later use;
(2) Adding zinc acetate powder into the sol according to the proportion of 3-10g/L, stirring and dissolving, and cleaning and drying the glass or silicon chip for later use;
(3) Film coating: coating a film on a carrier by a pulling method, a spin coater, a coating or spraying method, drying at room temperature, and sintering by a muffle furnace to obtain an ultra-smooth alumina film;
wherein, the sintering conditions in the step (3) are as follows: the initial temperature of sintering is 25 ℃, the heating rate is 1 ℃/min, the temperature is kept for 1h at 100 ℃, 1h at 200 ℃, 1h at 300 ℃, 1h at 400 ℃ and 5h at 500 ℃.
2. The method for producing an ultra-smooth alumina thin film according to claim 1, characterized in that: the preparation method of the alumina sol comprises the following steps: adding aluminum sec-butoxide into distilled water at the temperature of 80-90 ℃, magnetically stirring for 25-35 min, adjusting the pH to 2~3 by nitric acid, and magnetically stirring for 25-35 min at the temperature of 80-90 ℃ to obtain the alumina sol.
3. The method for producing an ultra-smooth alumina thin film according to claim 1, characterized in that: the cleaning process of the glass or silicon carrying wafer comprises the following steps: the mixture was washed with ethyl acetate 100ml, 95% ethanol 100ml, and deionized water 100ml in sequence in a sonicator for 30min.
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| WO2012071507A1 (en) * | 2010-11-24 | 2012-05-31 | The Regents Of The University Of California | Colloidal infrared reflective and transparent conductive aluminum-doped zinc oxide nanocrystals |
| US8497199B1 (en) * | 2012-06-01 | 2013-07-30 | Institute Of Nuclear Energy Research Atomic Energy Council, Executive Yuan | Method for fabricating a thin film formed with a uniform single-size monolayer of spherical AZO nanoparticles |
| CN108374162A (en) * | 2018-02-05 | 2018-08-07 | 华南师范大学 | A kind of preparation method of aluminum-doped zinc oxide transparent conductive film |
| CN109487245A (en) * | 2018-12-14 | 2019-03-19 | 华南理工大学 | A kind of preparation method of super-hydrophobic aqua oxidation aluminium film |
| CN109761639A (en) * | 2019-03-05 | 2019-05-17 | 南京理工大学 | Nano-structure porous silicon aluminate films material and preparation method thereof |
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| CN102503162A (en) * | 2011-11-01 | 2012-06-20 | 昆明理工大学 | Preparation method for Ag-Al co-doped p type ZnO film |
| CN104368394B (en) * | 2014-10-21 | 2017-01-11 | 河南能源化工集团研究院有限公司 | Alumina carrier containing zinc and nickel and preparation method thereof |
| CN106835237B (en) * | 2017-01-06 | 2018-12-25 | 西北大学 | A kind of preparation method of petal-shaped film-type Zn-Al class gas sensitive |
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| WO2012071507A1 (en) * | 2010-11-24 | 2012-05-31 | The Regents Of The University Of California | Colloidal infrared reflective and transparent conductive aluminum-doped zinc oxide nanocrystals |
| US8497199B1 (en) * | 2012-06-01 | 2013-07-30 | Institute Of Nuclear Energy Research Atomic Energy Council, Executive Yuan | Method for fabricating a thin film formed with a uniform single-size monolayer of spherical AZO nanoparticles |
| CN108374162A (en) * | 2018-02-05 | 2018-08-07 | 华南师范大学 | A kind of preparation method of aluminum-doped zinc oxide transparent conductive film |
| CN109487245A (en) * | 2018-12-14 | 2019-03-19 | 华南理工大学 | A kind of preparation method of super-hydrophobic aqua oxidation aluminium film |
| CN109761639A (en) * | 2019-03-05 | 2019-05-17 | 南京理工大学 | Nano-structure porous silicon aluminate films material and preparation method thereof |
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