研究目的
To demonstrate rapid photocuring and vat photopolymerization additive manufacturing of fully amorphous polysiloxane terpolymers for producing elastomeric objects with low-temperature performance.
研究成果
The study successfully demonstrated VP-AM of amorphous siloxane terpolymers using thiol–ene chemistry, yielding elastomers with high thermal stability and absence of crystallinity. The DiEtS system is preferred for future ultra-low temperature applications due to better crystallization suppression potential. Limitations include branching in DiPhS systems and need for improved resolution and mechanical properties with additives.
研究不足
The DiPhS-containing system is prone to uncontrolled branching, which could affect mechanical properties. The DiEtS system showed minor crystallization due to synthetic method limitations. Future work needs to address resolution improvements with UV blockers and fillers, and use of pure cyclic monomers for complete crystallization suppression.
1：Experimental Design and Method Selection:
The study used vat photopolymerization (VP) additive manufacturing with thiol–ene chemistry for crosslinking amorphous PDMS terpolymers. Theoretical models included polymerization kinetics and thermal analysis methods.
2：Sample Selection and Data Sources:
Samples included PDMS7.0k-DiPhS and PDMS7.5k-DiEtS terpolymers synthesized previously, and a thiol-functional PDMS crosslinker (PDMS7.4k-SH). Data sources were from prior synthesis and characterization.
3：0k-DiPhS and PDMS5k-DiEtS terpolymers synthesized previously, and a thiol-functional PDMS crosslinker (PDMS4k-SH). Data sources were from prior synthesis and characterization. List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Equipment included rheometers (TA Instruments DHR-2), DSC (TA Instruments Q2000), TGA (TA Instruments Q500), DMA (TA Instruments Q800), NMR spectrometer (Agilent U4-DD2 500 MHz), UV light sources (Omnicure S2000, BlueWave 75), and VP apparatus. Materials included photoinitiators (DMPA, TPO), UV absorber (BBOT), solvents (chloroform), and polymers from Gelest and Sigma-Aldrich.
4：Experimental Procedures and Operational Workflow:
Photopolymer mixtures were prepared with stoichiometric functional groups, photoinitiator, and UV absorber. Photocuring was done in a sandwich setup for films, and VP was performed layer-wise with UV irradiation. Characterization involved photorheology, photocalorimetry, TGA, DSC, DMA, and Soxhlet extraction.
5：Data Analysis Methods:
Data were analyzed using integrated heat flow for exotherms, modulus crossover times, gel fractions from extraction, and thermal stability parameters from TGA and DMA.
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NMR Spectrometer
U4-DD2 500 MHz
Agilent
Used for 1H NMR spectroscopy to characterize polymer structures.
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UV Light Source
BlueWave 75
Dymax
Used for vat photopolymerization as a UV spot curing lamp.
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Photoinitiator
DMPA
Sigma-Aldrich
Used as a photoinitiator for UV-induced crosslinking.
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Photoinitiator
TPO
Sigma-Aldrich
Used as a photoinitiator for vat photopolymerization due to spectral compatibility.
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UV Absorber
BBOT
Sigma-Aldrich
Used to minimize cure-through during vat photopolymerization.
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Rheometer
DHR-2
TA Instruments
Used for photorheology to measure shear storage modulus and loss modulus during UV irradiation.
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Differential Scanning Calorimeter
Q2000
TA Instruments
Used for photocalorimetry to measure polymerization exotherms and thermal transitions.
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Thermogravimetric Analyzer
Q500
TA Instruments
Used for TGA to measure thermal stability and weight loss.
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Dynamic Mechanical Analyzer
Q800
TA Instruments
Used for DMA to measure thermomechanical properties like storage modulus and tan δ.
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UV Light Source
Omnicure S2000
Used for photorheology and photocalorimetry as a high-pressure mercury light source.
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Thiol-functional PDMS
SMS-042
Gelest
Used as a crosslinker in thiol–ene reactions.
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