研究目的
To investigate the effect of thermal annealing on the crystalline structure and dispersion state of PMMA-modified graphene in PVDF nanocomposites.
研究成果
PMMA-modified graphene enhances b-crystalline structure in PVDF at 90°C annealing but leads to b-to-c phase conversion at 120°C. Graphene sheets tend to restack with increasing temperature, reducing dispersion. Modified graphene does not act as a nucleating agent for PVDF crystallization. Thermal stability improves with graphene addition up to 1 wt.%.
研究不足
The study is limited to specific annealing temperatures and graphene loadings; broader ranges were not explored. The restacking of graphene sheets at higher temperatures may limit dispersion stability in practical applications. The nucleating effect of modified graphene was not observed, indicating potential constraints in crystallization enhancement.
1：Experimental Design and Method Selection:
The study involved preparing PVDF-based nanocomposite films with PMMA-modified graphene using solution-mixing and solvent casting. Annealing was performed at three temperatures (50, 90, 120°C) to study crystalline structure changes. Characterization methods included XRD, DSC, TGA, TEM, FTIR, and AFM.
2：Sample Selection and Data Sources:
Samples were prepared with varying loadings of PMMA-modified graphene (0.5, 1, 2 wt.%) in PVDF matrix. Materials included natural graphite, PVDF, MMA, MAA, and other chemicals as specified.
3：5, 1, 2 wt.%) in PVDF matrix. Materials included natural graphite, PVDF, MMA, MAA, and other chemicals as specified. List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Equipment included TGA Q50 thermogravimetric analyzer, DSC Q100, Bruker AXS D8 advanced diffractometer, Ziess-902A TEM, Bruker IFS 113v FTIR, Bruker/Veeco AFM. Materials included graphite, PVDF (Kynar VR 1000HD), MMA, MAA, sulfuric acid, nitric acid, BPO, DMF, CH2Cl2, TEA.
4：Experimental Procedures and Operational Workflow:
Graphene was modified with PMMA via radical polymerization. Nanocomposites were prepared by dispersing modified graphene in PVDF solution, casting films, and annealing. Characterization involved heating/cooling scans, XRD measurements, TEM imaging, FTIR analysis, and TGA.
5：Data Analysis Methods:
Crystallinity was calculated from DSC melting enthalpy. XRD patterns were analyzed for phase identification. TGA data provided thermal stability metrics.
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Bruker AXS D8 advanced diffractometer
D8 advanced
Bruker
Recording X-ray diffraction patterns to analyze crystalline structures of samples.
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Ziess-902A TEM
902A
Ziess
Obtaining transmission electron microscopy images to examine the dispersed state of graphene in the matrix.
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Bruker IFS 113v FTIR
IFS 113v
Bruker
Performing Fourier transform infrared analysis to study functional groups on sample surfaces.
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TGA Q50 thermogravimetric analyzer
Q50
TA Instruments
Performing thermogravimetric analyses to measure weight loss and thermal stability of samples.
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DSC Q100
Q100
TA Instruments
Measuring thermal behavior through differential scanning calorimetry, including heating and cooling scans.
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Bruker/Veeco AFM
Bruker/Veeco
Carrying out atomic force microscopy measurements to analyze surface topography.
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PVDF pellets
Kynar VR 1000HD
Atofina
Used as the polymer matrix in nanocomposite preparation.
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Graphite powders
Iran Petrochemical Co
Source material for preparing graphene through chemical modification.
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