研究目的
To develop a new acid hydrolysis and subsequent alkaline condensation method for preparing SiO2 microspheres with functional groups (amine or sulfydryl) on the surface, addressing the low efficiency of post-modification methods.
研究成果
The acid hydrolysis and subsequent alkaline condensation method successfully produced SiO2 microspheres with amine or sulfydryl functional groups, as confirmed by characterization techniques. This approach offers a promising one-step alternative to inefficient post-modification methods for functional silica materials.
研究不足
The method may have constraints in controlling particle size uniformity and functional group density; optimization is needed for scalability and application-specific requirements.
1:Experimental Design and Method Selection:
A new acid hydrolysis and subsequent alkaline condensation method was used to prepare SiO2 microspheres by self-condensing or co-condensing functional organosilane precursors (APTES, MPTES, MPTMS) with PTMS.
2:Sample Selection and Data Sources:
Precursors including APTES, MPTES, MPTMS, and PTMS were used without purification; double distilled water was used.
3:List of Experimental Equipment and Materials:
Chemicals from Sinopharm Chemical Reagent Co., Ltd.; equipment includes laser particle size analyzer, TEM, SEM, XPS, IR spectrometer, Raman microscope, TGA analyzer, and specific surface area analyzer.
4:Experimental Procedures and Operational Workflow:
Dilute nitric acid was added to water, heated to 60°C, purged with nitrogen; organosilane precursors were added with stirring, followed by ammonia addition; stirring continued for 1 h; microspheres were separated by centrifugation and washed.
5:Data Analysis Methods:
Particle size measured by laser analyzer; morphologies by TEM and SEM; surface composition by XPS; surface groups by IR and Raman; thermal analysis by TGA; porosity by N2 adsorption-desorption.
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field emission transmission electron microscope
Tecnai G2 F20 S-TWIN
FEI Company
Characterizing the morphologies of microspheres
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environmental scanning electron microscope
Quanta 400 FEG
FEI Company
Characterizing surface morphologies of samples
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X-ray photoelectron spectroscopy
Axis Ultra DLD
Kratos
Analyzing surface elemental composition
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fourier infrared spectrometer
TENSOR27
Bruke
Characterizing surface groups of SiO2 microspheres
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laser particle size analyzer
LS13320
Beckman Coulter
Measuring the diameters and distributions of microspheres
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Raman microscope
InVia
Renishaw
Characterizing surface groups of SiO2 microspheres
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thermogravimetric analyzer
TGA/DAC 3+ Star System
Mettler Toledo
Measuring thermogravimetric analysis
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specific surface area and pore size analyzer
TriStar II 3020
Micromertics
Obtaining N2-adsorption desorption isotherms and pore size distributions
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