研究目的
To enhance the anti-icing property of titanium dioxide (TiO2) particles through fluorine modification to create a very hydrophobic surface.
研究成果
Fluorine modification on TiO2 particles successfully creates a very hydrophobic surface with a water contact angle of 146°, significantly lowering the crystallization temperature to -19.4°C and increasing freezing delay time to over 25 minutes at -10°C, demonstrating excellent anti-icing properties. The optimal AIBN content for maximum grafting efficiency is 2.0 wt%. This approach is effective for enhancing the anti-icing performance of inorganic particles through surface chemistry modifications.
研究不足
The grafting efficiency is limited by steric effects during reactions, leading to only a small part of DFHMA being chemisorbed. The study focuses on TiO2 particles and may not generalize to other materials. The anti-icing performance is tested under specific conditions (-10°C), and long-term durability or real-world application constraints are not addressed.
1：Experimental Design and Method Selection:
The study involved a two-step modification process: first, TiO2 was modified with MPS to introduce C=C bonds, then DFHMA monomers were grafted via free radical polymerization initiated by AIBN. The rationale was to use fluorine-organic reagents for low surface energy and long chains to improve hydrophobicity and anti-icing performance.
2：Sample Selection and Data Sources:
Unmodified TiO2 particles (VK-T02H) were used as the base material. Chemicals like MPS, DFHMA, AIBN, and solvents were sourced from specified suppliers.
3：List of Experimental Equipment and Materials:
Equipment included FTIR spectrometer (Nicolet IS5, Thermo Fisher), TGA analyzer (Q500, TA instruments), XPS spectrometer (ESCALAB 250Xi, ThermoScientific), TEM (JEOL 2100 Plus, JEOL), DLS spectrometer (90Plus, Brookhaven), contact angle meter (DSA100, Krüss), DSC (DSC 4000, PerkinElmer), macro camera (KS1A14, Kingcent), and refrigerator (BCD-108GQ, Rongsheng). Materials included TiO2, MPS, DFHMA, AIBN, ethanol, methylbenzene, etc.
4：Experimental Procedures and Operational Workflow:
TiO2 was dispersed in methylbenzene, MPS and triethylamine were added for initial modification. Then, MPS-modified TiO2 was reacted with DFHMA and AIBN in methylbenzene under nitrogen at 75°C with stirring, followed by centrifugation, purification, and drying. Characterization involved FTIR, TGA, XPS, TEM, DLS, contact angle measurement, DSC, and freezing delay time tests.
5：Data Analysis Methods:
Data were analyzed using software tools for spectroscopy and microscopy; surface tension was calculated using Owens and Wendt method; statistical analysis included averaging multiple measurements.
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Fourier Transformed Infrared spectrometer
Nicolet IS5
Thermo Fisher
To collect FTIR spectra of particles in transmittance mode for chemical component analysis.
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XPS spectrometer
ESCALAB 250Xi
ThermoScientific
To conduct X-ray photoelectron spectroscopy for surface chemical composition analysis.
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Transmission electron microscope
JEOL 2100 Plus
JEOL
To obtain micrographs of TiO2 particles for morphology analysis.
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Differential scanning calorimetry analyzer
DSC 4000
PerkinElmer
To measure crystallization temperature of water droplets on TiO2 surface.
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Thermogravimetric analyzer
Q500
TA instruments
To investigate the grafted amount of samples by measuring weight loss under nitrogen flow.
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Dynamic light scattering spectrometer
90Plus
Brookhaven
To measure particle size and size distribution.
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Optical contact angle meter
DSA100
Krüss
To determine static contact angle values using sessile water drop method.
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Macro camera
KS1A14
Kingcent
To record videos for freezing delay time measurement under isothermal conditions.
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Refrigerator
BCD-108GQ
Rongsheng
To maintain testing temperature at -10 oC for freezing delay time experiments.
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TiO2 particles
VK-T02H
Xuancheng Jingrui New Materials Co. Ltd.
Base inorganic particles used for surface modification.
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3-methacryloxypropyl-trimethoxysilane
AR
Sinopharm Chemical Reagent Co. Ltd.
Silane coupling agent to introduce C=C bonds on TiO2 surface.
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Azobisisobutyronitrile
CP
Shanghai NO.4 Reagent & H.V. Chemical Co. Ltd.
Free radical initiator for polymerization reaction.
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Dodecafluoroheptyl methacrylate
AR
Maya Reagent Co. Ltd.
Fluorine-organic reagent for grafting onto TiO2 to enhance hydrophobicity.
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