Aggregation and Deposition Behavior of Carbon-Based Nanomaterials in Aquatic Environments

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1 Aggregation and Deposition Behavior of Carbon-Based Nanomaterials in Aquatic Environments Menachem Elimelech Department of Chemical Engineering Environmental Engineering Program Yale University 2007 NSF Nanoscale Science and Engineering Grantees Conference, Arlington, VA, December 3-6, 2007 NSF BES NSF BES

2 Engineered Carbon-Based Nanomaterials C 60 Nanoparticles SWNT 100 nm MWNT Exponential growth in production and potential applications Unique properties (shape, surface charge, reactivity) Environmental and health impacts are not known

3 Aggregation and Deposition Behavior Determines Fate and Transport Aggregation Sediment Deposition/ Attachment Mineral Surfaces Influences rate of settling and transport Removal from aqueous phase May influence reactivity and toxicity

4 Complex Interactions in Aquatic Systems Ions Na + Cl - Ca 2+ Mg 2+ NOM, biomolecules, minerals/suspended solids Nanomaterials

5 Aggregation Kinetics of Fullerene Nanoparticles

6 Fullerene Nanoparticles Buckminsterfullerene C 60 nc nm

7 Ordered Structure of C 60 Molecules Buckminsterfullerene C 60 nc nm

8 Two Synthesis Methods Sonicated C 60 Nanoparticles (Son-C 60 ) Fullerene (99.9% purity) Dissolve fullerene in toluene Sonicate with water and ethanol for 3 hr Filter with 0.45 then 0.2 µm filters Aqueous C 60 Nanoparticles (Aq-C 60 ) Stirring fullerene in deionized water for 40 days before filtration

9 Physical Characterization Son-C 60 Aq-C 60 R H = 50.5 nm R H = 83.1 nm 20 nm 50 nm

10 Physical Characterization Son-C 60 Aq-C nm 10 nm

11 Electrophoretic Mobility (EPM) in KCl EPM (10-8 m 2 /Vs) Son-C 60 ph 5.5 Aq-C 60 ph 5.5 Negatively charged Aq-C 60 more negatively charged than Son-C 60 EPM becomes less negative as KCl concentration increases KCl Conc. (mm)

12 ALV Light Scattering Setup Dynamic light scattering to derive hydrodynamic radius YAG laser with wavelength of 532 nm Scattered light intensity measured at 90 from incident beam

13 Time-Resolved Dynamic Light Scattering Hydrodynamic Radius (nm) mm NaCl 145 mm NaCl 100 mm NaCl 80 mm NaCl k A, fast Time (s) k A Initial aggregation kinetics: k A drh dt α =1 / W = ( t) k k t 0 Attachment Efficiency or Inverse Stability Ratio: A A, fast

14 Aggregation Kinetics in KCl Inverse Stability Ratio, 1/W Son-C 60 Aq-C mm mm ph KCl Conc. (M) Classic slow and fast aggregation regimes Aq-C 60 are much more stable (CCC of 200 mm)

15 Aggregation Kinetics in KCl and CaCl 2 Inverse Stability Ratio, 1/W Son-C 60 Aq-C mm 0.1 Inverse Stability Ratio, 1/W Son-C 60 Aq-C mm 50 mm ph mm ph KCl Conc. (M) CaCl 2 Conc. (M)

16 Increased Stability in Humic Acid with NaCl Hydrodynamic Radius (nm) No humic acid 1 mg/l TOC 5 mg/l TOC Diffusion-limited Time (s) NaCl concentration = 650 mm ph 8 Chen and Elimelech, J. Colloid Interface Sci. 2007, 309,

17 Increased Stability in Humic Acid with NaCl and MgCl 2 Hydrodynamic Radius (nm) No humic acid 1 mg/l TOC 5 mg/l TOC Diffusion-limited Time (s) Attachment Efficiency, α No humic acid 1 mg/l TOC ph 8 MgCl 2 Concentration (M) NaCl concentration = 650 mm CCC increases in humic acid ph 8 Chen and Elimelech, J. Colloid Interface Sci. 2007, 309,

18 Steric Stabilization with Humic Acid in NaCl and MgCl 2 EPM (10-8 m 2 /Vs) No humic acid Humic acid ph 8 10 mm 3 mm 3 mm NaCl CaCl 2 MgCl 2 Electrophoretic mobility (EPM) similar with and without humic acid Indication of steric stabilization

19 Enhanced Aggregation at High CaCl 2 Concentrations Hydrodynamic Radius (nm) Enhanced aggregation 1 mg/l TOC No humic acid Diffusion-limited Time (s) CaCl 2 concentration = 40 mm ph 8

20 Enhanced Aggregation at High CaCl 2 Concentrations Hydrodynamic Radius (nm) Enhanced aggregation 1 mg/l TOC No humic acid Diffusion-limited Time (s) Attachment Efficiency, α No humic acid 1 mg/l TOC ph E CaCl 2 Concentration (M) At 1 mg/l TOC, enhanced aggregation occurs above 10 mm CaCl 2

21 Humic Acid Clusters Bridge Fullerene Nanoparticles 200 nm 100 mm MgCl nm 40 mm CaCl 2

22 Humic Acid Clusters Bridge Fullerene Nanoparticles 500 nm 40 mm CaCl 2

23 Aggregation Kinetics of Multi-Walled Carbon Nanotubes (MWNTs)

24 MWNT Sample Preparation 10 mg MWNTs added to 100 ml DI water Sonicated for 30 minutes using ultrasonicating probe Supernatant collected Re-sonicated for 5 more cycles (30 minutes each) to obtain final sample

25 TEM Images of Untreated and Treated MWNTs Untreated Treated 100nm 500nm Tubes are bundled and long before treatment Sonication debundles and reduces average length

26 Diameter and Length Distributions of Treated MWNTs % MWCNT % MWCNT Diameter (nm) Length (μm) Diameter and length distributions are obtained with TEM Average diameter 18 nm and average length 1.5 μm

27 Aggregation Kinetics with Monovalent Salt (NaCl) Attachment Efficiency, α NaCl Conc. (M)

28 Aggregation Kinetics with CaCl 2 and MgCl 2 Attachment Efficiency, α CaCl 2 Concentration (M) Attachment Efficiency, α MgCl 2 Conc. (M) Classic aggregation behavior with slow and fast regimes

29 Deposition Kinetics of Fullerene Nanoparticles

30 Aggregation and Deposition Behavior Determines Fate and Transport Aggregation Deposition/ Attachment Sediment Mineral Surfaces

31 Quartz Crystal Microbalance (QCM) Flow Cell: Silica coating Quartz crystal AC Frequency Shift (Hz) Sauerbrey relationship: Δm = Deposition starts CΔf n Time (min) n

32 Deposition Kinetics Frequency Shift (Hz) mm 10 mm 30 mm Time (min)

33 Attachment Efficiency Frequency Shift (Hz) k D, fast PLL 1 mm 10 mm 30 mm α Time (min) D = k D Deposition attachment efficiency: k k D, D fast Favorable (fast) deposition: Quartz crystal PLL Pre-adsorption of +ve charged poly-l-lysine (PLL) on silica surface

34 Influence of NaCl and CaCl 2 on Deposition Kinetics Deposition Rate (Hz/min) CCC E NaCl Concentration (M) Deposition Rate (Hz/min) CaCl 2 Concentration (M) Attachment Efficiency, α D Below CCC, as electrolyte concentration increases faster deposition through charge shielding Towards CCC and above significant drop in deposition rate

35 Simultaneous Deposition and Aggregation at Higher Ionic Strength At 100 mm NaCl: Quartz crystal Aggregate formation lower convective-diffusive transport towards silica surface Frequency Shift (Hz) Time (min) Non-linear deposition behavior Bigger aggregates formed at later stages deposition rate decreases even more

36 Release of Deposited Nanoparticles Frequency Change (Hz) Frequency Change (Hz) A B C D E F A B Time (min) C D E F Time (min) NaCl CaCl 2 A Baseline (ph 5.7) B Deposition at 30 mm NaCl and 0.6 mm CaCl 2 (both α D ~ 1) C Rinsing with respective electrolytes D Rinsing with 1 mm NaCl E Rinsing with DI water F Rinsing with DI water (ph 12.3) Release at Stage F sudden increase in surface potential of C 60 nanoparticles and silica surface

37 Concluding Remarks Eelectrostatic interactions control the aggregation and deposition behavior of carbonbased nanomaterials (CBNs) Humic substances stabilize CBNs by electrosteric repulsion Under solution chemistries of natural waters, CBNs are stable and thus expected to be mobile

38 Acknowledgments NSF BES NSF BES

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