The development of a high-throughput gradient array apparatus for the study of porous polymer networks.
- North Dakota State University, Fargo, ND
A gradient array apparatus was constructed for the study of porous polymers produced using the process of chemically-induced phase separation (CIPS). The apparatus consisted of a 60 element, two-dimensional array in which a temperature gradient was placed in the y-direction and composition was varied in the x-direction. The apparatus allowed for changes in opacity of blends to be monitored as a function of temperature and cure time by taking images of the array with time. The apparatus was validated by dispense a single blend composition into all 60 wells of the array and curing them for 24 hours and doing the experiment in triplicate. Variations in micron scale phase separation were readily observed as a function of both curing time and temperature and there was very good well-to-well consistency as well as trial-to-trial consistency. Poragen of samples varying with respect to cure temperature was removed and SEM images were obtained. The results obtained showed that cure temperature had a dramatic affect on sample morphology, and combining data obtained from visual observations made during the curing process with SEM data can enable a much better understanding of the CIPS process and provide predictive capability through the relatively facile generation of composition-process-morphology relationships. Data quality could be greatly enhanced by making further improvements in the apparatus. The primary improvements contemplated include the use of a more uniform light source, an optical table, and a CCD camera with data analysis software. These improvements would enable quantification of the amount of scattered light generated from individual elements as a function of cure time. In addition to the gradient array development, porous composites were produced by incorporating metal particles into a blend of poragen, epoxy resin, and crosslinker. The variables involved in the experiment were metal particle composition, primary metal particle size, metal concentration, and poragen composition. A total of 16 different porous composites were produced and characterized using SEM. In general, the results showed that pore morphology and the distribution of metal particles was dependent on multiple factors. For example, the use of silver nanoparticles did not significantly affect pore morphology for composites derived from decanol as the poragen, but exceptionally large pores were obtained with the use of decane as the poragen. With regard to the effect of metal particle size, silver nanoparticles were essentially exclusively dispered in the polymer matrix while silver microparticles were found in pores. For nickel particles, both nanoparticles and microparticles were largely dispersed in the polymer matrix and not in the pores.
- Research Organization:
- Sandia National Laboratories (SNL), Albuquerque, NM, and Livermore, CA (United States)
- Sponsoring Organization:
- USDOE
- DOE Contract Number:
- AC04-94AL85000
- OSTI ID:
- 984130
- Report Number(s):
- SAND2010-0139; TRN: US201015%%1063
- Country of Publication:
- United States
- Language:
- English
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