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- Creators: Lin, Jerry
Description
The flow of liquid PDMS (10:1 v/v base to cross-linker ratio) in open, rectangular silicon micro channels, with and without a hexa-methyl-di-silazane (HMDS) or poly-tetra-fluoro-ethylene (PTFE) (120 nm) coat, was studied. Photolithographic patterning and etching of silicon wafers was used to create micro channels with a range of widths (5-50 μm) and depths (5-20 μm). The experimental PDMS flow rates were compared to an analytical model based on the work of Lucas and Washburn. The experimental flow rates closely matched the predicted flow rates for channels with an aspect ratio (width to depth), p, between one and two. Flow rates in channels with p less than one were higher than predicted whereas the opposite was true for channels with p greater than two. The divergence between the experimental and predicted flow rates steadily increased with increasing p. These findings are rationalized in terms of the effect of channel dimensions on the front and top meniscus morphology and the possible deviation from the no-slip condition at the channel walls at high shear rates.
In addition, a preliminary experimental setup for calibration tests on ultrasensitive PDMS cantilever beams is reported. One loading and unloading cycle is completed on a microcantilever PDMS beam (theoretical stiffness 0.5 pN/ µm). Beam deflections are actuated by adjusting the buoyancy force on the beam, which is submerged in water, by the addition of heat. The expected loading and unloading curve is produced, albeit with significant noise. The experimental results indicate that the beam stiffness is a factor of six larger than predicted theoretically. One probable explanation is that the beam geometry may change when it is removed from the channel after curing, making assumptions about the beam geometry used in the theoretical analysis inaccurate. This theory is bolstered by experimental data discussed in the report. Other sources of error which could partially contribute to the divergent results are discussed. Improvements to the experimental setup for future work are suggested.
In addition, a preliminary experimental setup for calibration tests on ultrasensitive PDMS cantilever beams is reported. One loading and unloading cycle is completed on a microcantilever PDMS beam (theoretical stiffness 0.5 pN/ µm). Beam deflections are actuated by adjusting the buoyancy force on the beam, which is submerged in water, by the addition of heat. The expected loading and unloading curve is produced, albeit with significant noise. The experimental results indicate that the beam stiffness is a factor of six larger than predicted theoretically. One probable explanation is that the beam geometry may change when it is removed from the channel after curing, making assumptions about the beam geometry used in the theoretical analysis inaccurate. This theory is bolstered by experimental data discussed in the report. Other sources of error which could partially contribute to the divergent results are discussed. Improvements to the experimental setup for future work are suggested.
ContributorsSowers, Timothy Wayne (Author) / Rajagopalan, Jagannathan (Thesis advisor) / Herrmann, Marcus (Committee member) / Huang, Huei-Ping (Committee member) / Arizona State University (Publisher)
Created2014
Description
Membranes are a key part of pervaporation processes, which is generally a more
efficient process for selective removal of alcohol from water than distillation. It is
necessary that the membranes have high alcohol permeabilities and selectivities.
Polydimethylsiloxane (PDMS) based mixed matrix membranes (MMMs) have
demonstrated very promising results. Zeolitic imidazolate framework-71 (ZIF-71)
demonstrated promising alcohol separation abilities. In this dissertation, we present
fundamental studies on the synthesis of ZIF-71/PDMS MMMs.
Free-standing ZIF-71/ PDMS membranes with 0, 5, 25 and 40 wt % ZIF-71
loadings were prepared and the pervaporation separation for ethanol and 1-butanol from
water was measured. ZIF-71/PDMS MMMs were formed through addition cure and
condensation cure methods. Addition cure method was not compatible with ZIF-71
resulting in membranes with poor mechanical properties, while the condensation cure
method resulted in membranes with good mechanical properties. The 40 wt % ZIF-71
loading PDMS nanocomposite membranes achieved a maximum ethanol/water selectivity
of 0.81 ± 0.04 selectivity and maximum 1-butnaol/water selectivity of 5.64 ± 0.15.
The effects of synthesis time, temperature, and reactant ratio on ZIF-71 particle
size and the effect of particle size on membrane performance were studied. Temperature
had the greatest effect on ZIF-71 particle size as the synthesis temperature varied from -
20 to 35 ºC. The ZIF-71 synthesized had particle diameters ranging from 150 nm to 1
μm. ZIF-71 particle size is critical in ZIF-71/PDMS composite membrane performance
for alcohol removal from water through pervaporation. The membranes made with
micron sized ZIF-71 particles showed higher alcohol/water selectivity than those with
smaller particles. Both alcohol and water permeability increased when larger sized ZIF-
71 particles were incorporated.
ZIF-71 particles were modified with four ligands through solvent assisted linker
exchange (SALE) method: benzimidazole (BIM), 5-methylbenzimidazole (MBIM), 5,6-
dimethylbenzimidazole (DMBIM) and 4-Phenylimidazole (PI). The morphology of ZIF-
71 were maintained after the modification. ZIF-71/PDMS composite membranes with 25
wt% loading modified ZIF-71 particles were made for alcohol/water separation. Better
particle dispersion in PDMS polymer matrix was observed with the ligand modified ZIFs.
For both ethanol/water and 1-butanol/water separations, the alcohol permeability and
alcohol/water selectivity were lowered after the ZIF-71 ligand exchange reaction.
efficient process for selective removal of alcohol from water than distillation. It is
necessary that the membranes have high alcohol permeabilities and selectivities.
Polydimethylsiloxane (PDMS) based mixed matrix membranes (MMMs) have
demonstrated very promising results. Zeolitic imidazolate framework-71 (ZIF-71)
demonstrated promising alcohol separation abilities. In this dissertation, we present
fundamental studies on the synthesis of ZIF-71/PDMS MMMs.
Free-standing ZIF-71/ PDMS membranes with 0, 5, 25 and 40 wt % ZIF-71
loadings were prepared and the pervaporation separation for ethanol and 1-butanol from
water was measured. ZIF-71/PDMS MMMs were formed through addition cure and
condensation cure methods. Addition cure method was not compatible with ZIF-71
resulting in membranes with poor mechanical properties, while the condensation cure
method resulted in membranes with good mechanical properties. The 40 wt % ZIF-71
loading PDMS nanocomposite membranes achieved a maximum ethanol/water selectivity
of 0.81 ± 0.04 selectivity and maximum 1-butnaol/water selectivity of 5.64 ± 0.15.
The effects of synthesis time, temperature, and reactant ratio on ZIF-71 particle
size and the effect of particle size on membrane performance were studied. Temperature
had the greatest effect on ZIF-71 particle size as the synthesis temperature varied from -
20 to 35 ºC. The ZIF-71 synthesized had particle diameters ranging from 150 nm to 1
μm. ZIF-71 particle size is critical in ZIF-71/PDMS composite membrane performance
for alcohol removal from water through pervaporation. The membranes made with
micron sized ZIF-71 particles showed higher alcohol/water selectivity than those with
smaller particles. Both alcohol and water permeability increased when larger sized ZIF-
71 particles were incorporated.
ZIF-71 particles were modified with four ligands through solvent assisted linker
exchange (SALE) method: benzimidazole (BIM), 5-methylbenzimidazole (MBIM), 5,6-
dimethylbenzimidazole (DMBIM) and 4-Phenylimidazole (PI). The morphology of ZIF-
71 were maintained after the modification. ZIF-71/PDMS composite membranes with 25
wt% loading modified ZIF-71 particles were made for alcohol/water separation. Better
particle dispersion in PDMS polymer matrix was observed with the ligand modified ZIFs.
For both ethanol/water and 1-butanol/water separations, the alcohol permeability and
alcohol/water selectivity were lowered after the ZIF-71 ligand exchange reaction.
ContributorsYin, Huidan (Author) / Lind, Mary Laura (Thesis advisor) / Mu, Bin (Committee member) / Nielsen, David (Committee member) / Seo, Don (Committee member) / Lin, Jerry (Committee member) / Arizona State University (Publisher)
Created2017