Additive-free hydrogelation of graphene oxide by ultrasonication

Owen C. Compton; Zhi An; Karl W. Putz; Bong Jin Hong; Brad G. Hauser; L. Catherine Brinson; Sonbinh T. Nguyen

doi:10.1016/j.carbon.2012.01.061

Additive-free hydrogelation of graphene oxide by ultrasonication

Owen C. Compton, Zhi An, Karl W. Putz, Bong Jin Hong, Brad G. Hauser, L. Catherine Brinson, Sonbinh T. Nguyen^*

^*Corresponding author for this work

Research output: Contribution to journal › Article › peer-review

133 Scopus citations

Abstract

Graphene oxide hydrogels have been prepared by ultrasonication of precursor aqueous dispersions. The ultrasonication fractures the nanosheets, reducing their dimensions and exposing new sheet edges that do not possess the stabilizing carboxyl functional groups found along the edge of the as-prepared material. Ultrasonication does not affect the overall chemical functionality of the graphene oxide nanosheets, as spectra (carbon-13 nuclear magnetic resonance spectroscopy, infrared spectroscopy, and X-ray photoelectron spectroscopy) of samples before and after ultrasonication are nearly identical. Gelation is induced after only 30 min of ultrasonication to achieve a relatively weak gel with a shear modulus of 0.3 kPa; however, extension of ultrasonic treatment to 120 min yields a more robust hydrogel with a shear modulus of 1.6 kPa. Such enhancement in the gel's physical properties can be attributed to the lack of stabilizing carboxyl groups on newly generated nanosheet fragments from the interior regions of the original nanosheets. As prepared, these hydrogels exhibit exceptionally low critical gelation concentrations ranging from ∼0.050 to ∼0.125 mg mL ^-1 that can be tuned according to the extent of ultrasonic treatment.

Original language	English (US)
Pages (from-to)	3399-3406
Number of pages	8
Journal	Carbon
Volume	50
Issue number	10
DOIs	https://doi.org/10.1016/j.carbon.2012.01.061
State	Published - Aug 2012

Funding

Support for this work is provided by the ARO (Award # W991NF-09-1-0541) and the United States NSF (Grant # DMR-0520513 through the Materials Research Science and Engineering Center at Northwestern University and NIRT-0404291). OCC is an ACC-NSF fellow (NSF award # CHE-0936924). XPS was performed in the Keck II/NUANCE facility at Northwestern University (NU). Solid-state 13 C MAS NMR spectra were collected in the IMSERC facility at NU. SEM images were gathered in the NEMS-MEMS Facility at NU. XRD patterns were collected in the J. B. Cohen X-ray Diffraction Facility at NU. We thank the Initiative for Sustainability and Energy (ISEN) at Northwestern for funding the purchase of the equipment used in this work. We thank Prof. Omar K. Farha for carrying out the scCO 2 -activation of the lyophilized hydrogel samples and Prof. Joseph T. Hupp for use of the critical point dryer and adsorption measurement instrumentation in his laboratory.

ASJC Scopus subject areas

General Chemistry
General Materials Science

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10.1016/j.carbon.2012.01.061

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@article{edb5c4690a484cdd992dbe028416fc37,

title = "Additive-free hydrogelation of graphene oxide by ultrasonication",

abstract = "Graphene oxide hydrogels have been prepared by ultrasonication of precursor aqueous dispersions. The ultrasonication fractures the nanosheets, reducing their dimensions and exposing new sheet edges that do not possess the stabilizing carboxyl functional groups found along the edge of the as-prepared material. Ultrasonication does not affect the overall chemical functionality of the graphene oxide nanosheets, as spectra (carbon-13 nuclear magnetic resonance spectroscopy, infrared spectroscopy, and X-ray photoelectron spectroscopy) of samples before and after ultrasonication are nearly identical. Gelation is induced after only 30 min of ultrasonication to achieve a relatively weak gel with a shear modulus of 0.3 kPa; however, extension of ultrasonic treatment to 120 min yields a more robust hydrogel with a shear modulus of 1.6 kPa. Such enhancement in the gel's physical properties can be attributed to the lack of stabilizing carboxyl groups on newly generated nanosheet fragments from the interior regions of the original nanosheets. As prepared, these hydrogels exhibit exceptionally low critical gelation concentrations ranging from ∼0.050 to ∼0.125 mg mL -1 that can be tuned according to the extent of ultrasonic treatment.",

author = "Compton, {Owen C.} and Zhi An and Putz, {Karl W.} and Hong, {Bong Jin} and Hauser, {Brad G.} and {Catherine Brinson}, L. and Nguyen, {Sonbinh T.}",

note = "Funding Information: Support for this work is provided by the ARO (Award # W991NF-09-1-0541) and the United States NSF (Grant # DMR-0520513 through the Materials Research Science and Engineering Center at Northwestern University and NIRT-0404291). OCC is an ACC-NSF fellow (NSF award # CHE-0936924). XPS was performed in the Keck II/NUANCE facility at Northwestern University (NU). Solid-state 13 C MAS NMR spectra were collected in the IMSERC facility at NU. SEM images were gathered in the NEMS-MEMS Facility at NU. XRD patterns were collected in the J. B. Cohen X-ray Diffraction Facility at NU. We thank the Initiative for Sustainability and Energy (ISEN) at Northwestern for funding the purchase of the equipment used in this work. We thank Prof. Omar K. Farha for carrying out the scCO 2 -activation of the lyophilized hydrogel samples and Prof. Joseph T. Hupp for use of the critical point dryer and adsorption measurement instrumentation in his laboratory. ",

year = "2012",

month = aug,

doi = "10.1016/j.carbon.2012.01.061",

language = "English (US)",

volume = "50",

pages = "3399--3406",

journal = "Carbon",

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AU - Compton, Owen C.

AU - An, Zhi

AU - Putz, Karl W.

AU - Hong, Bong Jin

AU - Hauser, Brad G.

AU - Catherine Brinson, L.

AU - Nguyen, Sonbinh T.

N1 - Funding Information: Support for this work is provided by the ARO (Award # W991NF-09-1-0541) and the United States NSF (Grant # DMR-0520513 through the Materials Research Science and Engineering Center at Northwestern University and NIRT-0404291). OCC is an ACC-NSF fellow (NSF award # CHE-0936924). XPS was performed in the Keck II/NUANCE facility at Northwestern University (NU). Solid-state 13 C MAS NMR spectra were collected in the IMSERC facility at NU. SEM images were gathered in the NEMS-MEMS Facility at NU. XRD patterns were collected in the J. B. Cohen X-ray Diffraction Facility at NU. We thank the Initiative for Sustainability and Energy (ISEN) at Northwestern for funding the purchase of the equipment used in this work. We thank Prof. Omar K. Farha for carrying out the scCO 2 -activation of the lyophilized hydrogel samples and Prof. Joseph T. Hupp for use of the critical point dryer and adsorption measurement instrumentation in his laboratory.

PY - 2012/8

Y1 - 2012/8

N2 - Graphene oxide hydrogels have been prepared by ultrasonication of precursor aqueous dispersions. The ultrasonication fractures the nanosheets, reducing their dimensions and exposing new sheet edges that do not possess the stabilizing carboxyl functional groups found along the edge of the as-prepared material. Ultrasonication does not affect the overall chemical functionality of the graphene oxide nanosheets, as spectra (carbon-13 nuclear magnetic resonance spectroscopy, infrared spectroscopy, and X-ray photoelectron spectroscopy) of samples before and after ultrasonication are nearly identical. Gelation is induced after only 30 min of ultrasonication to achieve a relatively weak gel with a shear modulus of 0.3 kPa; however, extension of ultrasonic treatment to 120 min yields a more robust hydrogel with a shear modulus of 1.6 kPa. Such enhancement in the gel's physical properties can be attributed to the lack of stabilizing carboxyl groups on newly generated nanosheet fragments from the interior regions of the original nanosheets. As prepared, these hydrogels exhibit exceptionally low critical gelation concentrations ranging from ∼0.050 to ∼0.125 mg mL -1 that can be tuned according to the extent of ultrasonic treatment.

AB - Graphene oxide hydrogels have been prepared by ultrasonication of precursor aqueous dispersions. The ultrasonication fractures the nanosheets, reducing their dimensions and exposing new sheet edges that do not possess the stabilizing carboxyl functional groups found along the edge of the as-prepared material. Ultrasonication does not affect the overall chemical functionality of the graphene oxide nanosheets, as spectra (carbon-13 nuclear magnetic resonance spectroscopy, infrared spectroscopy, and X-ray photoelectron spectroscopy) of samples before and after ultrasonication are nearly identical. Gelation is induced after only 30 min of ultrasonication to achieve a relatively weak gel with a shear modulus of 0.3 kPa; however, extension of ultrasonic treatment to 120 min yields a more robust hydrogel with a shear modulus of 1.6 kPa. Such enhancement in the gel's physical properties can be attributed to the lack of stabilizing carboxyl groups on newly generated nanosheet fragments from the interior regions of the original nanosheets. As prepared, these hydrogels exhibit exceptionally low critical gelation concentrations ranging from ∼0.050 to ∼0.125 mg mL -1 that can be tuned according to the extent of ultrasonic treatment.

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DO - 10.1016/j.carbon.2012.01.061

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VL - 50

SP - 3399

EP - 3406

JO - Carbon

JF - Carbon

IS - 10

ER -

Additive-free hydrogelation of graphene oxide by ultrasonication

Abstract

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ASJC Scopus subject areas

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