研究目的
Investigating the optimal parameters for the preparation of crack-free SiO2 ?lms experimentally so that they can be used in saturable absorber as optical elements, which can be applied to mode-locked and Q-switched lasers.
研究成果
Obtaining a crack-free SiO2 ?lm is very crucial in the preparation of composite materials using SiO2 as the base. It is the key to the success of Q-switched and mode-locked lasers. H2O, solvent, catalyst, aging time, spin coating speed, ammonia treatment, heat treatment, and substrate have e?ects on the ?lm properties. Therefore, a completely crack-free ?lm can be prepared only when the optimal parameters are maintained. The optimal molar ratios of TEOS, H2O, EtOH and HCl were found to be 1:15:10:0.1, the aging time was 240 h, the spin coating speed was 1500 r min?1 in this experiment. The test results showed that the prepared crack-free SiO2 ?lm was in amorphous form with some nanocrystals, and the size of SiO2 nanoparticles was in the range of 100–500 nm. The crack-free SiO2 nano?lms with tens of microns thickness could be repeatedly fabricated using the optimizing parameters, which had rarely been seen in previous reports.
研究不足
The technical and application constraints of the experiments, as well as potential areas for optimization.
1:Experimental Design and Method Selection:
The sol was prepared by magnetically stirring measured amounts of TEOS, H2O, and EtOH for 1 h. Then, speci?c quantities of HCl and dimethylacetamide were added as the catalyst and drying control agent and stirring was continued for further 5 h. The sol was aged at room temperature for a certain period of time to allow gel formation. This gel was then spin-coated at 1500 r min?1 20 times to form a liquid ?lm on a glass plate, which was hydrophilically treated with mixture of concentrated H2SO4:H2O2 = 1:
2:A uniform and dense SiO2 ?lm was prepared by heating the liquid ?lm after fumigation for 24 h in an atmosphere of saturated ammonia. In the heat treatment method, the ammonia treated ?lm was dried in a drying oven at 60 °C for 24 h, 80 °C for 24 h, and then placed it in a tube annealing furnace where the temperature was increased to 500 °C, based on the temperature curve under vacuum. Sample Selection and Data Sources:
The surface morphologies were studied under a metallographic microscope to determine the optimal parameters required for the preparation of SiO2 ?lm. The surface morphology and thickness of the crack-free ?lm was tested by scanning electron microscopy (SEM). The composition of the sample was analyzed by the X-ray photoelectron spectroscopy (XPS). The transmissivity of the sample was tested by UV–visible spectrophotometry. The crystal quality of the sample was analyzed by X-ray di?raction (XRD).
3:List of Experimental Equipment and Materials:
TEOS, H2O, EtOH, HCl, dimethylacetamide, glass plate, concentrated H2SO4, H2O2, ammonia, drying oven, tube annealing furnace, metallographic microscope, SEM, XPS, UV–visible spectrophotometer, XRD.
4:Experimental Procedures and Operational Workflow:
The sol was prepared by magnetically stirring measured amounts of TEOS, H2O, and EtOH for 1 h. Then, speci?c quantities of HCl and dimethylacetamide were added as the catalyst and drying control agent and stirring was continued for further 5 h. The sol was aged at room temperature for a certain period of time to allow gel formation. This gel was then spin-coated at 1500 r min?1 20 times to form a liquid ?lm on a glass plate, which was hydrophilically treated with mixture of concentrated H2SO4:H2O2 = 1:
5:A uniform and dense SiO2 ?lm was prepared by heating the liquid ?lm after fumigation for 24 h in an atmosphere of saturated ammonia. In the heat treatment method, the ammonia treated ?lm was dried in a drying oven at 60 °C for 24 h, 80 °C for 24 h, and then placed it in a tube annealing furnace where the temperature was increased to 500 °C, based on the temperature curve under vacuum. Data Analysis Methods:
The surface morphologies were studied under a metallographic microscope to determine the optimal parameters required for the preparation of SiO2 ?lm. The surface morphology and thickness of the crack-free ?lm was tested by scanning electron microscopy (SEM). The composition of the sample was analyzed by the X-ray photoelectron spectroscopy (XPS). The transmissivity of the sample was tested by UV–visible spectrophotometry. The crystal quality of the sample was analyzed by X-ray di?raction (XRD).
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TEOS
Precursor for the sol-gel method
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EtOH
Solvent in the sol-gel method
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HCl
Catalyst in the sol-gel method
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dimethylacetamide
Drying control agent in the sol-gel method
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glass plate
Substrate for the SiO2 ?lm
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concentrated H2SO4
Used in hydrophilic treatment of the glass plate
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H2O2
Used in hydrophilic treatment of the glass plate
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ammonia
Used in fumigation of the SiO2 ?lm
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drying oven
Used in the heat treatment of the SiO2 ?lm
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tube annealing furnace
Used in the heat treatment of the SiO2 ?lm
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metallographic microscope
Used to study the surface morphologies of the SiO2 ?lm
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SEM
Used to test the surface morphology and thickness of the crack-free ?lm
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XPS
Used to analyze the composition of the sample
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UV–visible spectrophotometer
Used to test the transmissivity of the sample
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XRD
Used to analyze the crystal quality of the sample
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