Scalable Manufacturing of Layer-by-Layer Membranes for Water Purification
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1 2016 U.S. Frontiers of Engineering Symposium September 20, 2016 Scalable Manufacturing of Layer-by-Layer Membranes for Water Purification Christopher M. Stafford Materials Science & Engineering Division National Institute of Standards and Technology Material Measurement Laboratory
2 MEMBRANES FOR DESALINATION molecular size H 2 O 2.8 Å Na Å hydrated Na Å 2
3 OVERVIEW Thin film composite (TFC) membranes Current (TFC) innovations Measurement innovations Opportunities 3
4 THIN FILM COMPOSITE MEMBRANES (TFC) Membrane active layer has to be: incredibly thin (10s 100s nm) defect free mechanically robust chlorine tolerant fouling resistant Crosslinked aromatic polyamide h ~200 nm Porous polysulfone Nonwoven polyester Thin film composite (TFC) 4
5 THIN FILM COMPOSITE MEMBRANES (TFC) Membrane active layer has to be: incredibly thin (10s 100s nm) defect free mechanically robust chlorine tolerant fouling resistant 5
6 THIN FILM COMPOSITE MEMBRANES (TFC) Membrane technologist sees: 6
7 THIN FILM COMPOSITE MEMBRANES (TFC) Chemical engineer sees: 7
8 THIN FILM COMPOSITE MEMBRANES (TFC) Polymer scientist sees: 8
9 THIN FILM COMPOSITE MEMBRANES (TFC) The lack of correlation between film thickness and permeability suggests the entire film thickness may not contribute to separation - J. Membrane Sci. 311, (2008) 9
10 THIN FILM COMPOSITE MEMBRANES (TFC) Chemistry/process has not changed much in 40 years. Analytical tools and polymer science have outpaced this technology. 10
11 OVERVIEW Thin film composite (TFC) membranes Current (TFC) innovations Measurement innovations Opportunities 11
12 MEMBRANE INNOVATION TWEAKING THE PROCESS Inkjet printing was used to control dosing (concentration) of amine available for interfacial polymerization amine solution Multiple passes of the inkjet printer leads to increased dose of amine solution available for polymerization S. Badalov and C.J. Arnusch; J Memb Sci 2016, 515,
13 MEMBRANE INNOVATION ADJUSTING DEPOSITION Inkjet printing was used to control dosing (concentration) of amine available for interfacial polymerization Multiple passes of the inkjet printer leads to increased dose of amine solution available for polymerization S. Badalov and C.J. Arnusch; J Memb Sci 2016, 515,
14 MEMBRANE INNOVATION ALTERING REACTION ZONE Co-solvent assisted interfacial polymerization (CAIP) CAIP Addition of a co-solvent in the organic phase IP Controls the miscibility and/or solubility of the amine at the interface of the two immiscible fluids C. Kong et al.; J Memb Sci 2010, 362,
15 MEMBRANE INNOVATION ALTERING THE SUPPORT Sacrificial nanofiber layer [Cd(OH) 2 )] Cadmium hydroxide nanostrands act to gate amine arrival at the interface Nanostrands can then be removed via acid treatment S. Karan et al.; Science 2015, 348,
16 THIN FILM COMPOSITE MEMBRANES (TFC) How do we measure something like this? Can we provide a platform for fundamental measurements of structure/property/transport? 16
17 MEMBRANE INNOVATION DISRUPTIVE TECHNOLOGY molecular Layer-by-Layer (mlbl) IP mlbl P. M. Johnson, et al.; JPSB 2011, 50,
18 MEMBRANE INNOVATION DISRUPTIVE TECHNOLOGY molecular Layer-by-Layer (mlbl) In collaboration with S. George and D. Higgs, UC Boulder. 18
19 MEMBRANE INNOVATION DEMONSTRATION molecular Layer-by-Layer (mlbl) Throughput - Spatial ALD = 20 cycles/min. - mlbl = 0.5 cycle/min. Comparable growth rate In collaboration with S. George and D. Higgs, UC Boulder. 19
20 MEMBRANE INNOVATION R2R OPPORTUNITIES 20
21 OVERVIEW Thin film composite (TFC) membranes Current (TFC) innovations Measurement innovations Opportunities 21
22 THIN FILM COMPOSITE MEMBRANES (TFC) Water Salt increased flux decreased flux 22
23 Concentration mmol/g Absorbance (Normalized) MEASUREMENT INNOVATION CHEMICAL ANALYSIS Traditional vibrational spectroscopy is not sensitive enough to measure extremely thin membranes z Si Substrate Polymer Ge Crystal y x um 60 layers 30 layers 15 layers 10 layers Gold substrate Silicon Substrate Free Acid IR Wavenumber Cycle (cm -1 ) There is thought to be a correlation between free acid and water flux We now have a measurement tool to track free acid content as we change variables in the system In collaboration with TJ Zimudzi and M. Hickner, Penn State. 23
24 MEASUREMENT INNOVATION CHEMICAL ANALYSIS mlbl Functional Polymers 1 um 2 um 1660, 1540: Amide I,II : Amide III, C-N stretch from Amine 1712: Free carboxylic acid (C=O) 1607: hydrogen bonded C=O + aromatic C-C stretch 1488: C-N bend In collaboration with Anasys Instruments. 24
25 MEASUREMENT INNOVATION CHEMICAL ANALYSIS Resonant soft x-ray reflectivity (RSoXR) Near an atomic absorption edge, the refractive index profile will change based on the functional group, distance from the edge and functional group density. 25
26 MEASUREMENT INNOVATION SWELLING RH ellipsometer t eq swelling in-situ liquid cell h diffusion t Swelling behavior is a measure of the water content within the film Can correlate water content with free acid content in the membrane 26
27 MEASUREMENT INNOVATION DYNAMICS hydrated w/ H 2 O hydrated w/ D 2 O Probes molecular motions Influence of polymer dynamics contrast H 2 O D 2 O D O H Ca Si 27
28 MEASUREMENT INNOVATION TRANSPORT (WATER) Fickian Diffusion: Γ Q 2 HWHM, (mev) T = 280 K T = 300 K T = 320 K T = 280 K (fit) T = 300 K (fit) T = 320 K (fit) Fraction of non-mobile species (bound water) Effective cage size where water rattles around Residence time of water in that cage Q 2 (A 2 ) 28
29 MEASUREMENT INNOVATION TRANSPORT (SALT) Electrochemical Impedance Spectroscopy Traditionally a tool for electrochemists/metallurgists C m = A δ εε 0 R m = δ A RT 1 F 2 σ D i K i c i 29
30 OVERVIEW Thin film composite (TFC) membranes Current (TFC) innovations Measurement innovations Opportunities 30
31 OPPORTUNITIES New membranes, nanomaterials Modeling New measurement platforms 31
32 CONCLUDING THOUGHTS Water and water purification is critical to economic and national security Immense opportunities for the polymer science and beyond Membrane innovations go hand-inhand with innovations in measurement science (structure/property) Scalable manufacturing is needed to make these new membranes a reality 32
33 ACKNOWLEDGEMENTS NIST Dr. Edwin Chan Dr. Daniel Sunday Ai Nguyen Dr. Bradley Frieberg Penn State University Dr. TJ Zimudzi Dr. Michael Hickner UC Boulder Dr. Daniel Higgs Dr. Steven George GE Global Research Dr. Hua Wang Dr. Yanju Wang Dow Water Process & Solutions Dr. Abhishek Roy Dr. Steve Rosenberg 33
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