Patent
Atlas literature
Patent
US 10,995,003Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Zhao, B.; Liu, P.; Jiang, Y.; Pan, D.; Tao, H.; Song, J.; Fang, T.; Xu, W., Supercapacitor performances of thermally reduced graphene oxide. Jou rn al of Power Sources 2012, 198, 423-427.
Li, D.; Muller, M. B.; G il je, S.; Kaner, R. B.; Wallace, G. G., Processable aqueous dispersions of graphene nanosheets. Nat Nano 2008, 3 (2), 101- 105.
Shin, H.-J.; Kim, K. K.; Benayad, A.; Yoon, S.-M.; Park, H. K.; Jung, I.- S.; Jin, M. H.; Jeong, H.- K.; Kim, J. M.; Choi, J.-Y.; Lee, Y. H., Efficient Reduction of Graphite Oxide by Sodium Borohydride and Its Effect on El ectrical Conductance. Advanced Functional Materials 2009, 19 (12), 1987-1992.
Wang, X.; Xing, W.; Song, L.; Yang, H.; Hu, Y.; Ye o h, G. H., Fabrication and characterization of graphene-reinforced waterborne polyurethane nanocomposite coatings by the sol-gel method. Surface and Coatings Technology 2012, 206 (23), 4778-4784.
Schniepp, H. C.; Li, J.-L.; McAllister, M. J.; Sai, H.; Herrera-Alonso, M.; Adamson, D. H.; Prud'homme, R. K.; Car, R.; Saville, D. A.; Aksay, I. A., Functionalized Single Graphene Sheets Derived from Splitting Graphite Oxide. The Journal of Physical Chemist r y B 2006, 110 (17), 8535-8539.
Xiao, Y.; Li, X.; Zai, J.; Wang, K.; Gong, Y.; Li, B.; Han, Q.; Qian, X., CoFe₂ 0 4-Graphene Nanocomposites Synthesized through An Ultrasonic Method with Enhanced Performances as Anode Materials for Li-ion Batteries. Nano-Micro Letters 2014, 6 (4), 307-315.
Song, Z.; Zhang, Y.; Liu, W.; Zhang, S.; Liu, G.; Chen, H.; Qiu, J., Hydrothermal synthesis and electrochemical performance of Co₃ 0 4/reduced graphene oxide nanosheet composites for supercapacitors. Electrochimica Acta 2013, 112, 120-126.
Nassar, M. Y.; Ahmed, I. S., Hydrothermal synthesis of cobalt carbonates using different counter ions: An efficient precursor to nano- sized cobalt oxide (Co₃ 0 4). Polyhedron 2011, 30 (15), 2431-2437.
Cies i elski, W.; Tomasik, P., Thermal properties of complexes of amaranthus starch with selected metal salts. Thermochim Acta 2003, 403. 10. Wang, H.; Cui, L.-F.; Yang, Y.; Sanchez Casalongue, H.; Robinson, J. T.; Liang, Y.; Cui, Y.; Dai, H., Mn₃ 0 4-Graphene Hybrid as a High-Capacity Anode Material for Lithium I on Batteries. Journal of the American Chemical Society 2010, 132 (40), 13978-13980. 11. Li, Y.; Gao, W.; Ci, L.; Wang, C.; Ajayan, P. M., Catalytic performance of Pt nanoparticles on reduced graphene oxide for methanol electro- oxidation. Carbon 2010, 48 (4), 1124-1130. 12. Antony, R. P.; Preethi, L. K.; Gupta, B.; Mathews, T.; Dash, S.; Tyagi, A. K., Efficient electrocatalytic performance of thermally exfoliated reduced graphene oxide-Pt hybrid. Materials Research Bulletin 2015, 70, 60-67.
Gao, M.; Peh, C. K. N.; Ong, W. L.; Ho, G. W., Green chemistry synthesis of a nanocomposite graphene hydrogel with three-dimensional nano-mesopores for photocatalytic H₂ production. RSC Advances 2013, 3 (32), 13169-13177.
Lin, Z.; Liu, Y.; Yao, Y.; Hildreth, O. J.; Li, Z.; Moon, K.; Wong, C.-p., Superior Capacitance of Functionalized Graphene. The Jou rn al of Physical Chemist r y C 2011, 115 (14), 7120-7125. 15. Low, Q. X.; Ho, G. W., Facile structural tuning and compositing of iron oxide-graphene anode towards enhanced supacapacitive performance. Nano Energy 2014, 5, 28-35.
Choi, H.-J.; Jung, S.-M.; Seo, J.-M.; Chang, D. W.; Dai, L.; Baek, J.- B., Graphene for energy conversion and storage in fuel cells and supercapacitors. Nano Energy 2012, 1 (4), 534-551. 17. Granadeiro, C. M.; Cruz, S. M. A.; Goncalves, G.; Marques, P. A. A. P.; Costa, P. M. F. J.; Ferreira, R. A. S.; Carlos, L. D.; Nogueira, H. I. S., Photoluminescent bimetallic-3-hydroxypicolinate/graphene oxide nanocomposite. RSC Advances 2012, 2 (25), 9443-9447. 18. Ma, X.; Tao, H.; Yang, K.; Feng, L.; Cheng, L.; Shi, X.; Li, Y.; Guo, L.; Liu, Z., A functionalized graphene oxide-iron oxide nanocomposite for magnetically targeted drug delivery, photothermal therapy, and magnetic resonance imaging. Nano Res. 2012, 5 (3), 199-212. 19. Zhao, C.; Chou, S.-L.; Wang, Y.; Zhou, C.; Liu, H.-K.; Dou, S.-X., A facile route to synthesize transition metal oxide/reduced graphene oxide composites and their lithium storage performance. RSC Advances 2013, 3 (37), 16597-16603.
Du, M.; Sun, J.; Chang, J.; Yang, F.; Shi, L.; Gao, L., Synthesis of nitrogen-doped reduced graphene oxide directly from nitrogen-doped graphene oxide as a high-performance lithium ion battery anode. RSC Advances 2014, 4 (80), 42412-42417. 21. Vermisoglou, E. C.; Giannakopoulou, T.; Romanos, G.; Giannouri, M.; Boukos, N.; Lei, C.; Lekakou, C.; Trapalis, C., Effect of hydrothermal reaction time and alkaline conditions on the electrochemical properties of reduced graphene oxide. Applied surface Science 2015, 358, Part A, 100- 109.
Park, S.; An, J.; Potts, J. R.; Velamakanni, A.; Murali, S.; Ruoff, R. S., Hydrazine-reduction of graphite- and graphene oxide. Carbon 2011, 49 (9), 3019-3023.
Wong, C. P. P.; Lai, C. W.; Lee, K. M.; Hamid, S. B. A., Advanced Chemical Reduction of Reduced Graphene Oxide and I ts Photocatalytic Activity in Degrading Reactive Black 5. Materials 2015, 8 (10), 7118-7128.
Xu, C.; Shi, X.; Ji, A.; Shi, L.; Zhou, C.; C ui, Y., Fabrication and Characteristics of Reduced Graphene Oxide Produced with Different Green Reductants. P lo S one 2015, 10 (12), e01 44 842.
Zhang, X.; Sui, Z.; Xu, B.; Yue, S.; Luo, Y.; Zhan, W.; Liu, B., Mechanically strong and highly conductive graphene aerogel and its use as electrodes for electrochemical power sources. Journal of Materials Chemist r y 2011, 21 (18), 6494-6497. 26. Talbot, M. J.; White, R. G., Methanol fixation of plant tissue for Scanning Electron Microscopy improves preservation of tissue morphology and dimensions. Plant Methods 2013, 9 (1), 1-7. 27. Dohnalkova, A. C.; Marshall, M. J.; Arey, B. W.; Williams, K. H.; Buck, E. C.; Fredrickson, J. K., I maging hydrated microbial extracellular polymers: comparative analysis by electron microscopy. Applied and environmenta l microbio l ogy 2011, 77 (4), 1254-1262. 28. Lalwani, G.; Kwaczala, A. T.; Kanakia, S.; Patel, S. C.; Judex, S.; Sitharaman, B., Fabrication and characterization of three-dimensional macroscopic all-carbon scaffolds. Carbon 2013, 53, 90-100. 29. Marcano, D. C.; Kosynkin, D. V.; Berlin, J. M.; Sinitskii, A.; Sun, Z.; Slesarev, A.; Alemany, L. B.; Lu, W.; Tour, J. M., Improved Synthesis of Graphene Oxide. ACS Nano 2010, 4 (8), 4806-4814. 30. Alazmi, A.; Rasul, S.; Patole, S. P.; Costa, P. M., Comparative study of synthesis and reduction methods for graphene oxide. Polyhedron Forthcoming 2016;doi:10.101 6/j.poly.2016.04.044).
Luo, Z.; Yang, D.; Qi, G.; Shang, J.; Yang, H.; Wang, Y.; Yuwen, L.; Yu, T.; Huang, W.; Wang, L., Microwave-assisted solvothermal preparation of nitrogen and sulfur co-doped reduced graphene oxide and graphene quantum dots hybrids for highly efficient oxygen reduction. Jou rn al of Materials Chemist ry A 2014, 2 (48), 20605-20611. 32. Sawangphruk, M.; Suksomboon, M.; Kongsupornsak, K.; Khuntilo, J.; Srimuk, P.; Sanguansak, Y.; Klunbud, P.; Suktha, P.; Chiochan, P., High- performance supercapacitors based on silver nanoparticle-polyaniline- graphene nanocomposites coated on flexible carbon fiber paper. Jou rnal of Materials Chemist ry A 2013, 1 (34), 9630-9636. 33. Ramimoghadam, D.; Bin Hussein, M. Z.; Taufiq-Yap, Y. H., Hydrothermal synthesis of zinc oxide nanoparticles using rice as soft biotemplate. Chemistry Central Journal 2013, 7 (1), 1-10. 34. Hayes, W. I.; Joseph, P.; Mughal, M. Z.; Papakonstantinou, P., Production of reduced graphene oxide via hydrothermal reduction in an aqueous sulphuric acid suspension and its electrochemical behaviour. Jou rn al of solid state electrochemistry 2015, 19 (2), 361-380. 35. Feng, X., Nanocarbons for Advanced Energy Storage. Wiley: 2015. 36. Yan, J.; Wang, Q.; Wei, T.; Jiang, L.; Zhang, M.; Jing, X.; Fan, Z., Template-Assisted Low Temperature Synthesis of Functionalized Graphene for Ultrahigh Volumetric Performance Supercapacitors. A CS Nano 2014, 8 (5), 4720-4729.
Kumar, R.; Singh, R. K.; Savu, R.; Dubey, P. K.; Kumar, P.; Moshkalev, S. A., Microwave-assisted synthesis of void-induced graphene-wrapped nickel oxide hybrids for supercapacitor applications. RSC Advances 2016, 6 (32), 26612-26620. 38. Yan, J.; Liu, J.; Fan, Z.; Wei, T.; Zhang, L., High-performance supercapacitor electrodes based on highly corrugated graphene sheets. Carbon 2012, 50 (6), 2179-2188.
Shi, W.; Zhu, J.; Sim, D. H.; Tay, Y. Y.; Lu, Z.; Zhang, X.; Sharma, Y.; Srinivasan, M.; Zhang, H.; Hng, H. H.; Yan, Q., Achieving high specific charge capacitances in Fe₃ 0 4/reduced graphene oxide nanocomposites. Journal of Materials Chemistry 2011, 21 (10), 3422-3427. 40. He, P.; Yang, K.; Wang, W.; Dong, F.; Du, L.; Deng, Y., Reduced graphene oxide-CoFe₂ 0 4 composites for supercapacitor electrode. Russian Journal of Electrochemistry 2013, 49 (4), 359-364. 41. Bai, Y.; Rakhi, R. B.; Chen, W.; A l shareef, H. N., Effect of pH-induced chemical modification of hydrothermally reduced graphene oxide on supercapacitor performance. Journal of Power Sources 2013, 233, 313- 319.
Kumar, N. A.; Choi, H.-J.; Shin, Y. R.; Chang, D. W.; Dai, L.; Baek, J.-B., Polyaniline-Grafted Reduced Graphene Oxide for Efficient Electrochemical Supercapacitors. ACS Nano 2012, 6 (2), 1715-1723. 43. Lim, H. N.; Huang, N. M.; Lim, S. S.; Harrison, I.; Chia, C. H., Fabrication and characterization of graphene hydrogel via hydrothermal approach as a scaffold for preliminary study of cell growth. International Journal of Nanomedicine 2011, 6, 1817-1823. 44. Kumar, N. A.; Gambarelli, S.; Duclairoir, F.; Bidan, G.; Dubois, L., Synthesis of high quality reduced graphene oxide nanosheets free of paramagnetic metallic impurities. Journal of Materials Chemistry A 2013, 1 (8), 2789-2794. EMBODIMENTS FOR CARBON DIOXIDE CAPTURE Another application for the compositions and materials (and methods of making them) described herein is carbon dioxide capture. See, in particular, Figures 16-19. The effective capture of C 0 2 emitted by fossil-fuel-based power plants and other large industrial facilities is a top global priority to reduce the impact of global climate change and energy crisis (Chowdhury, S.; Balasubramanian, R., Highly efficient, rapid and selective C 0 2 capture by thermally treated graphene nanosheets. Jou rn al of C 0 2 Utilization 2016, 13, 50-60). As a result, several adsorbent materials have been studied for separation and storage of C 0 2 from fuel gases and other industrial exhaust streams. Recently, graphite and graphene have received a great deal of attention for gas adsorption, however, there has been little work carried out on graphene oxide (GO) for gas adsorption (Table I V) (Burress, J. W.; Gadipelli, S.; Ford, J.; Simmons, J. M.; Zhou, W.; Yildirim, T., G r aphene Oxide Framework Materials: Theoretical Predictions and Experimental Results. Angewandte Chemie International Edition 2010, 49 (47), 8902- 8904). Moreover, while GO with different degrees of oxidation and functionalization have been studied, the characterization of their porosity and/or gas adsorption properties is still overlooked. The most common GO production process is the so-called Hummer's method (or an adaptation of this). Not surprisingly, the few studies that have delved into C O 2 capture using GO have been based in GO derived from the Hummer's method without serious concerns on the steps involved. One such step, that is key is the drying methodology used after the GO product is obtained. The reported specific surface area of GO materials are less than or about 100 m 2 g-(Table V), possibly due to the GO pore network collapse and sheet re-aggregation taking place during the drying step. In this study, we illustrate that GO can be turned into a potentially relevant gas storage material by using an adapted ("Improved") Hummer's method that results in a material (improved GO, or IGO) with a higher degree of oxidation (A. Alazmi et al., Polyhedron, DOI: 10.1016/j.poly.20 1 6.04.044). Depending on the post-synthesis drying method employed, it is possible to partially tune the pore width/volume and specific surface area of the GO material. In line with this, the effect of employing vacuum, freeze and critical point drying (CPD) on the morphology, specific surface area, porosity and gas adsorption properties of I GO can be and has been determined. Our findings demonstrate for the first time that the CPD process can have a positive influence on the characteristic of GO materials, and it represents an effective strategy in the design and development of GO-based solid adsorbents for C₀ 2 capture. Overall, GO-vacuum dried material and GO-freeze-dried material are exclusively made up of micro-pores in the material. On the other hand, the GO-CPD dried material comprises micro, meso and macro pores. At the range of pressure of 0-1 bar, the micro pores are filled, while the meso and macro pores will only be filled at higher pressures (>10 bar). From the t-plot, the micro pore volume of the GO-CPD is comparable with the micro pore volume of GO-Vacuum and GO-freeze (Table 4). This can explain the comparable C₀ 2-uptake values for GO- vacuum dried, GO-freeze dried, and GO-CPD dried materials. On the other hand, our observation demonstrated that the GO prepared using Improved-Hummers' method has higher C 0 2-uptake than the GO prepared using Hummers' method (Figure 17). The filling of the meso/macro pores of GO-CPD at higher pressure (>10 bar) canimprove the C₀ SVG 16313726.12-27-2018.JQ₇ERIIURXEAPX0.SPEC.27.25.697.2595.775.2639.svg 0.147 0.26 Chemistry Black and white uptake value of these materials. Table IV. Comparison o f C O₂ adsorption by GO Adsorbent Synthesis method Drying method Porosity Temperature CO 2 Uptake at 1 bar References SVG 16313726.12-27-2018.JQ₇ERIIURXEAPX0.SPEC.28.4.358.539.2255.679.svg 0.467 6.323 Chemistry Black and white GO GO by modified Under vacuum at 50 Micropores 273 0.93 Xueta l.NanoscaleResearch t ette Hummers' method a C rs (2015)10:318 GO GO by I mproved CPD Micro/macro 273 1.8 Our work Hummer s' pores Table V. Comparison of specific surface area of GO SVG 16313726.12-27-2018.JQ₇ERIIURXEAPX0.SPEC.28.13.357.1479.2198.1582.svg 0.343 6.137 Chemistry Black and white GO from porous graphite (355 GO by Hummers' method I n vacuum 161 Ad v. Fu n ct, Mater. 2010,20,1670-1679 m z/g),+ GO from graphite (14.36 m 2/g) GO by modified Hummer's freeze-dried 102.29 Journal of S olid State Electrochem i stry, 2014. 19(2): p. 361-380 GO GO by modified Stau-denma l er's Dried at room 5.7 E. C. Vermisoglou et al./Applied surface method [temperature Sci ence 358 358 (2015) (2015) 100-109 Claims What is claimed is:
Layer stacks claimed or described, ordered top of device to substrate.
supercapacitor electrode
Materials described outside the worked examples.
graphene oxide (GO)
reduced graphene oxide (rGO)
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
BET specific surface area of rGO/CPD | 364 m2/g | reduced graphene oxide (rGO) |
supercapacitance of rGO/CPD electrode |
Patent
Atlas literature
Patent
US 10,995,003Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Zhao, B.; Liu, P.; Jiang, Y.; Pan, D.; Tao, H.; Song, J.; Fang, T.; Xu, W., Supercapacitor performances of thermally reduced graphene oxide. Jou rn al of Power Sources 2012, 198, 423-427.
Li, D.; Muller, M. B.; G il je, S.; Kaner, R. B.; Wallace, G. G., Processable aqueous dispersions of graphene nanosheets. Nat Nano 2008, 3 (2), 101- 105.
Shin, H.-J.; Kim, K. K.; Benayad, A.; Yoon, S.-M.; Park, H. K.; Jung, I.- S.; Jin, M. H.; Jeong, H.- K.; Kim, J. M.; Choi, J.-Y.; Lee, Y. H., Efficient Reduction of Graphite Oxide by Sodium Borohydride and Its Effect on El ectrical Conductance. Advanced Functional Materials 2009, 19 (12), 1987-1992.
Wang, X.; Xing, W.; Song, L.; Yang, H.; Hu, Y.; Ye o h, G. H., Fabrication and characterization of graphene-reinforced waterborne polyurethane nanocomposite coatings by the sol-gel method. Surface and Coatings Technology 2012, 206 (23), 4778-4784.
Schniepp, H. C.; Li, J.-L.; McAllister, M. J.; Sai, H.; Herrera-Alonso, M.; Adamson, D. H.; Prud'homme, R. K.; Car, R.; Saville, D. A.; Aksay, I. A., Functionalized Single Graphene Sheets Derived from Splitting Graphite Oxide. The Journal of Physical Chemist r y B 2006, 110 (17), 8535-8539.
Xiao, Y.; Li, X.; Zai, J.; Wang, K.; Gong, Y.; Li, B.; Han, Q.; Qian, X., CoFe₂ 0 4-Graphene Nanocomposites Synthesized through An Ultrasonic Method with Enhanced Performances as Anode Materials for Li-ion Batteries. Nano-Micro Letters 2014, 6 (4), 307-315.
Song, Z.; Zhang, Y.; Liu, W.; Zhang, S.; Liu, G.; Chen, H.; Qiu, J., Hydrothermal synthesis and electrochemical performance of Co₃ 0 4/reduced graphene oxide nanosheet composites for supercapacitors. Electrochimica Acta 2013, 112, 120-126.
Nassar, M. Y.; Ahmed, I. S., Hydrothermal synthesis of cobalt carbonates using different counter ions: An efficient precursor to nano- sized cobalt oxide (Co₃ 0 4). Polyhedron 2011, 30 (15), 2431-2437.
Cies i elski, W.; Tomasik, P., Thermal properties of complexes of amaranthus starch with selected metal salts. Thermochim Acta 2003, 403. 10. Wang, H.; Cui, L.-F.; Yang, Y.; Sanchez Casalongue, H.; Robinson, J. T.; Liang, Y.; Cui, Y.; Dai, H., Mn₃ 0 4-Graphene Hybrid as a High-Capacity Anode Material for Lithium I on Batteries. Journal of the American Chemical Society 2010, 132 (40), 13978-13980. 11. Li, Y.; Gao, W.; Ci, L.; Wang, C.; Ajayan, P. M., Catalytic performance of Pt nanoparticles on reduced graphene oxide for methanol electro- oxidation. Carbon 2010, 48 (4), 1124-1130. 12. Antony, R. P.; Preethi, L. K.; Gupta, B.; Mathews, T.; Dash, S.; Tyagi, A. K., Efficient electrocatalytic performance of thermally exfoliated reduced graphene oxide-Pt hybrid. Materials Research Bulletin 2015, 70, 60-67.
Gao, M.; Peh, C. K. N.; Ong, W. L.; Ho, G. W., Green chemistry synthesis of a nanocomposite graphene hydrogel with three-dimensional nano-mesopores for photocatalytic H₂ production. RSC Advances 2013, 3 (32), 13169-13177.
Lin, Z.; Liu, Y.; Yao, Y.; Hildreth, O. J.; Li, Z.; Moon, K.; Wong, C.-p., Superior Capacitance of Functionalized Graphene. The Jou rn al of Physical Chemist r y C 2011, 115 (14), 7120-7125. 15. Low, Q. X.; Ho, G. W., Facile structural tuning and compositing of iron oxide-graphene anode towards enhanced supacapacitive performance. Nano Energy 2014, 5, 28-35.
Choi, H.-J.; Jung, S.-M.; Seo, J.-M.; Chang, D. W.; Dai, L.; Baek, J.- B., Graphene for energy conversion and storage in fuel cells and supercapacitors. Nano Energy 2012, 1 (4), 534-551. 17. Granadeiro, C. M.; Cruz, S. M. A.; Goncalves, G.; Marques, P. A. A. P.; Costa, P. M. F. J.; Ferreira, R. A. S.; Carlos, L. D.; Nogueira, H. I. S., Photoluminescent bimetallic-3-hydroxypicolinate/graphene oxide nanocomposite. RSC Advances 2012, 2 (25), 9443-9447. 18. Ma, X.; Tao, H.; Yang, K.; Feng, L.; Cheng, L.; Shi, X.; Li, Y.; Guo, L.; Liu, Z., A functionalized graphene oxide-iron oxide nanocomposite for magnetically targeted drug delivery, photothermal therapy, and magnetic resonance imaging. Nano Res. 2012, 5 (3), 199-212. 19. Zhao, C.; Chou, S.-L.; Wang, Y.; Zhou, C.; Liu, H.-K.; Dou, S.-X., A facile route to synthesize transition metal oxide/reduced graphene oxide composites and their lithium storage performance. RSC Advances 2013, 3 (37), 16597-16603.
Du, M.; Sun, J.; Chang, J.; Yang, F.; Shi, L.; Gao, L., Synthesis of nitrogen-doped reduced graphene oxide directly from nitrogen-doped graphene oxide as a high-performance lithium ion battery anode. RSC Advances 2014, 4 (80), 42412-42417. 21. Vermisoglou, E. C.; Giannakopoulou, T.; Romanos, G.; Giannouri, M.; Boukos, N.; Lei, C.; Lekakou, C.; Trapalis, C., Effect of hydrothermal reaction time and alkaline conditions on the electrochemical properties of reduced graphene oxide. Applied surface Science 2015, 358, Part A, 100- 109.
Park, S.; An, J.; Potts, J. R.; Velamakanni, A.; Murali, S.; Ruoff, R. S., Hydrazine-reduction of graphite- and graphene oxide. Carbon 2011, 49 (9), 3019-3023.
Wong, C. P. P.; Lai, C. W.; Lee, K. M.; Hamid, S. B. A., Advanced Chemical Reduction of Reduced Graphene Oxide and I ts Photocatalytic Activity in Degrading Reactive Black 5. Materials 2015, 8 (10), 7118-7128.
Xu, C.; Shi, X.; Ji, A.; Shi, L.; Zhou, C.; C ui, Y., Fabrication and Characteristics of Reduced Graphene Oxide Produced with Different Green Reductants. P lo S one 2015, 10 (12), e01 44 842.
Zhang, X.; Sui, Z.; Xu, B.; Yue, S.; Luo, Y.; Zhan, W.; Liu, B., Mechanically strong and highly conductive graphene aerogel and its use as electrodes for electrochemical power sources. Journal of Materials Chemist r y 2011, 21 (18), 6494-6497. 26. Talbot, M. J.; White, R. G., Methanol fixation of plant tissue for Scanning Electron Microscopy improves preservation of tissue morphology and dimensions. Plant Methods 2013, 9 (1), 1-7. 27. Dohnalkova, A. C.; Marshall, M. J.; Arey, B. W.; Williams, K. H.; Buck, E. C.; Fredrickson, J. K., I maging hydrated microbial extracellular polymers: comparative analysis by electron microscopy. Applied and environmenta l microbio l ogy 2011, 77 (4), 1254-1262. 28. Lalwani, G.; Kwaczala, A. T.; Kanakia, S.; Patel, S. C.; Judex, S.; Sitharaman, B., Fabrication and characterization of three-dimensional macroscopic all-carbon scaffolds. Carbon 2013, 53, 90-100. 29. Marcano, D. C.; Kosynkin, D. V.; Berlin, J. M.; Sinitskii, A.; Sun, Z.; Slesarev, A.; Alemany, L. B.; Lu, W.; Tour, J. M., Improved Synthesis of Graphene Oxide. ACS Nano 2010, 4 (8), 4806-4814. 30. Alazmi, A.; Rasul, S.; Patole, S. P.; Costa, P. M., Comparative study of synthesis and reduction methods for graphene oxide. Polyhedron Forthcoming 2016;doi:10.101 6/j.poly.2016.04.044).
Luo, Z.; Yang, D.; Qi, G.; Shang, J.; Yang, H.; Wang, Y.; Yuwen, L.; Yu, T.; Huang, W.; Wang, L., Microwave-assisted solvothermal preparation of nitrogen and sulfur co-doped reduced graphene oxide and graphene quantum dots hybrids for highly efficient oxygen reduction. Jou rn al of Materials Chemist ry A 2014, 2 (48), 20605-20611. 32. Sawangphruk, M.; Suksomboon, M.; Kongsupornsak, K.; Khuntilo, J.; Srimuk, P.; Sanguansak, Y.; Klunbud, P.; Suktha, P.; Chiochan, P., High- performance supercapacitors based on silver nanoparticle-polyaniline- graphene nanocomposites coated on flexible carbon fiber paper. Jou rnal of Materials Chemist ry A 2013, 1 (34), 9630-9636. 33. Ramimoghadam, D.; Bin Hussein, M. Z.; Taufiq-Yap, Y. H., Hydrothermal synthesis of zinc oxide nanoparticles using rice as soft biotemplate. Chemistry Central Journal 2013, 7 (1), 1-10. 34. Hayes, W. I.; Joseph, P.; Mughal, M. Z.; Papakonstantinou, P., Production of reduced graphene oxide via hydrothermal reduction in an aqueous sulphuric acid suspension and its electrochemical behaviour. Jou rn al of solid state electrochemistry 2015, 19 (2), 361-380. 35. Feng, X., Nanocarbons for Advanced Energy Storage. Wiley: 2015. 36. Yan, J.; Wang, Q.; Wei, T.; Jiang, L.; Zhang, M.; Jing, X.; Fan, Z., Template-Assisted Low Temperature Synthesis of Functionalized Graphene for Ultrahigh Volumetric Performance Supercapacitors. A CS Nano 2014, 8 (5), 4720-4729.
Kumar, R.; Singh, R. K.; Savu, R.; Dubey, P. K.; Kumar, P.; Moshkalev, S. A., Microwave-assisted synthesis of void-induced graphene-wrapped nickel oxide hybrids for supercapacitor applications. RSC Advances 2016, 6 (32), 26612-26620. 38. Yan, J.; Liu, J.; Fan, Z.; Wei, T.; Zhang, L., High-performance supercapacitor electrodes based on highly corrugated graphene sheets. Carbon 2012, 50 (6), 2179-2188.
Shi, W.; Zhu, J.; Sim, D. H.; Tay, Y. Y.; Lu, Z.; Zhang, X.; Sharma, Y.; Srinivasan, M.; Zhang, H.; Hng, H. H.; Yan, Q., Achieving high specific charge capacitances in Fe₃ 0 4/reduced graphene oxide nanocomposites. Journal of Materials Chemistry 2011, 21 (10), 3422-3427. 40. He, P.; Yang, K.; Wang, W.; Dong, F.; Du, L.; Deng, Y., Reduced graphene oxide-CoFe₂ 0 4 composites for supercapacitor electrode. Russian Journal of Electrochemistry 2013, 49 (4), 359-364. 41. Bai, Y.; Rakhi, R. B.; Chen, W.; A l shareef, H. N., Effect of pH-induced chemical modification of hydrothermally reduced graphene oxide on supercapacitor performance. Journal of Power Sources 2013, 233, 313- 319.
Kumar, N. A.; Choi, H.-J.; Shin, Y. R.; Chang, D. W.; Dai, L.; Baek, J.-B., Polyaniline-Grafted Reduced Graphene Oxide for Efficient Electrochemical Supercapacitors. ACS Nano 2012, 6 (2), 1715-1723. 43. Lim, H. N.; Huang, N. M.; Lim, S. S.; Harrison, I.; Chia, C. H., Fabrication and characterization of graphene hydrogel via hydrothermal approach as a scaffold for preliminary study of cell growth. International Journal of Nanomedicine 2011, 6, 1817-1823. 44. Kumar, N. A.; Gambarelli, S.; Duclairoir, F.; Bidan, G.; Dubois, L., Synthesis of high quality reduced graphene oxide nanosheets free of paramagnetic metallic impurities. Journal of Materials Chemistry A 2013, 1 (8), 2789-2794. EMBODIMENTS FOR CARBON DIOXIDE CAPTURE Another application for the compositions and materials (and methods of making them) described herein is carbon dioxide capture. See, in particular, Figures 16-19. The effective capture of C 0 2 emitted by fossil-fuel-based power plants and other large industrial facilities is a top global priority to reduce the impact of global climate change and energy crisis (Chowdhury, S.; Balasubramanian, R., Highly efficient, rapid and selective C 0 2 capture by thermally treated graphene nanosheets. Jou rn al of C 0 2 Utilization 2016, 13, 50-60). As a result, several adsorbent materials have been studied for separation and storage of C 0 2 from fuel gases and other industrial exhaust streams. Recently, graphite and graphene have received a great deal of attention for gas adsorption, however, there has been little work carried out on graphene oxide (GO) for gas adsorption (Table I V) (Burress, J. W.; Gadipelli, S.; Ford, J.; Simmons, J. M.; Zhou, W.; Yildirim, T., G r aphene Oxide Framework Materials: Theoretical Predictions and Experimental Results. Angewandte Chemie International Edition 2010, 49 (47), 8902- 8904). Moreover, while GO with different degrees of oxidation and functionalization have been studied, the characterization of their porosity and/or gas adsorption properties is still overlooked. The most common GO production process is the so-called Hummer's method (or an adaptation of this). Not surprisingly, the few studies that have delved into C O 2 capture using GO have been based in GO derived from the Hummer's method without serious concerns on the steps involved. One such step, that is key is the drying methodology used after the GO product is obtained. The reported specific surface area of GO materials are less than or about 100 m 2 g-(Table V), possibly due to the GO pore network collapse and sheet re-aggregation taking place during the drying step. In this study, we illustrate that GO can be turned into a potentially relevant gas storage material by using an adapted ("Improved") Hummer's method that results in a material (improved GO, or IGO) with a higher degree of oxidation (A. Alazmi et al., Polyhedron, DOI: 10.1016/j.poly.20 1 6.04.044). Depending on the post-synthesis drying method employed, it is possible to partially tune the pore width/volume and specific surface area of the GO material. In line with this, the effect of employing vacuum, freeze and critical point drying (CPD) on the morphology, specific surface area, porosity and gas adsorption properties of I GO can be and has been determined. Our findings demonstrate for the first time that the CPD process can have a positive influence on the characteristic of GO materials, and it represents an effective strategy in the design and development of GO-based solid adsorbents for C₀ 2 capture. Overall, GO-vacuum dried material and GO-freeze-dried material are exclusively made up of micro-pores in the material. On the other hand, the GO-CPD dried material comprises micro, meso and macro pores. At the range of pressure of 0-1 bar, the micro pores are filled, while the meso and macro pores will only be filled at higher pressures (>10 bar). From the t-plot, the micro pore volume of the GO-CPD is comparable with the micro pore volume of GO-Vacuum and GO-freeze (Table 4). This can explain the comparable C₀ 2-uptake values for GO- vacuum dried, GO-freeze dried, and GO-CPD dried materials. On the other hand, our observation demonstrated that the GO prepared using Improved-Hummers' method has higher C 0 2-uptake than the GO prepared using Hummers' method (Figure 17). The filling of the meso/macro pores of GO-CPD at higher pressure (>10 bar) canimprove the C₀ SVG 16313726.12-27-2018.JQ₇ERIIURXEAPX0.SPEC.27.25.697.2595.775.2639.svg 0.147 0.26 Chemistry Black and white uptake value of these materials. Table IV. Comparison o f C O₂ adsorption by GO Adsorbent Synthesis method Drying method Porosity Temperature CO 2 Uptake at 1 bar References SVG 16313726.12-27-2018.JQ₇ERIIURXEAPX0.SPEC.28.4.358.539.2255.679.svg 0.467 6.323 Chemistry Black and white GO GO by modified Under vacuum at 50 Micropores 273 0.93 Xueta l.NanoscaleResearch t ette Hummers' method a C rs (2015)10:318 GO GO by I mproved CPD Micro/macro 273 1.8 Our work Hummer s' pores Table V. Comparison of specific surface area of GO SVG 16313726.12-27-2018.JQ₇ERIIURXEAPX0.SPEC.28.13.357.1479.2198.1582.svg 0.343 6.137 Chemistry Black and white GO from porous graphite (355 GO by Hummers' method I n vacuum 161 Ad v. Fu n ct, Mater. 2010,20,1670-1679 m z/g),+ GO from graphite (14.36 m 2/g) GO by modified Hummer's freeze-dried 102.29 Journal of S olid State Electrochem i stry, 2014. 19(2): p. 361-380 GO GO by modified Stau-denma l er's Dried at room 5.7 E. C. Vermisoglou et al./Applied surface method [temperature Sci ence 358 358 (2015) (2015) 100-109 Claims What is claimed is:
Layer stacks claimed or described, ordered top of device to substrate.
supercapacitor electrode
Materials described outside the worked examples.
graphene oxide (GO)
reduced graphene oxide (rGO)
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
BET specific surface area of rGO/CPD | 364 m2/g | reduced graphene oxide (rGO) |
supercapacitance of rGO/CPD electrode |
Patent
Atlas literature
Patent
US 10,995,003Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Zhao, B.; Liu, P.; Jiang, Y.; Pan, D.; Tao, H.; Song, J.; Fang, T.; Xu, W., Supercapacitor performances of thermally reduced graphene oxide. Jou rn al of Power Sources 2012, 198, 423-427.
Li, D.; Muller, M. B.; G il je, S.; Kaner, R. B.; Wallace, G. G., Processable aqueous dispersions of graphene nanosheets. Nat Nano 2008, 3 (2), 101- 105.
Shin, H.-J.; Kim, K. K.; Benayad, A.; Yoon, S.-M.; Park, H. K.; Jung, I.- S.; Jin, M. H.; Jeong, H.- K.; Kim, J. M.; Choi, J.-Y.; Lee, Y. H., Efficient Reduction of Graphite Oxide by Sodium Borohydride and Its Effect on El ectrical Conductance. Advanced Functional Materials 2009, 19 (12), 1987-1992.
Wang, X.; Xing, W.; Song, L.; Yang, H.; Hu, Y.; Ye o h, G. H., Fabrication and characterization of graphene-reinforced waterborne polyurethane nanocomposite coatings by the sol-gel method. Surface and Coatings Technology 2012, 206 (23), 4778-4784.
Schniepp, H. C.; Li, J.-L.; McAllister, M. J.; Sai, H.; Herrera-Alonso, M.; Adamson, D. H.; Prud'homme, R. K.; Car, R.; Saville, D. A.; Aksay, I. A., Functionalized Single Graphene Sheets Derived from Splitting Graphite Oxide. The Journal of Physical Chemist r y B 2006, 110 (17), 8535-8539.
Xiao, Y.; Li, X.; Zai, J.; Wang, K.; Gong, Y.; Li, B.; Han, Q.; Qian, X., CoFe₂ 0 4-Graphene Nanocomposites Synthesized through An Ultrasonic Method with Enhanced Performances as Anode Materials for Li-ion Batteries. Nano-Micro Letters 2014, 6 (4), 307-315.
Song, Z.; Zhang, Y.; Liu, W.; Zhang, S.; Liu, G.; Chen, H.; Qiu, J., Hydrothermal synthesis and electrochemical performance of Co₃ 0 4/reduced graphene oxide nanosheet composites for supercapacitors. Electrochimica Acta 2013, 112, 120-126.
Nassar, M. Y.; Ahmed, I. S., Hydrothermal synthesis of cobalt carbonates using different counter ions: An efficient precursor to nano- sized cobalt oxide (Co₃ 0 4). Polyhedron 2011, 30 (15), 2431-2437.
Cies i elski, W.; Tomasik, P., Thermal properties of complexes of amaranthus starch with selected metal salts. Thermochim Acta 2003, 403. 10. Wang, H.; Cui, L.-F.; Yang, Y.; Sanchez Casalongue, H.; Robinson, J. T.; Liang, Y.; Cui, Y.; Dai, H., Mn₃ 0 4-Graphene Hybrid as a High-Capacity Anode Material for Lithium I on Batteries. Journal of the American Chemical Society 2010, 132 (40), 13978-13980. 11. Li, Y.; Gao, W.; Ci, L.; Wang, C.; Ajayan, P. M., Catalytic performance of Pt nanoparticles on reduced graphene oxide for methanol electro- oxidation. Carbon 2010, 48 (4), 1124-1130. 12. Antony, R. P.; Preethi, L. K.; Gupta, B.; Mathews, T.; Dash, S.; Tyagi, A. K., Efficient electrocatalytic performance of thermally exfoliated reduced graphene oxide-Pt hybrid. Materials Research Bulletin 2015, 70, 60-67.
Gao, M.; Peh, C. K. N.; Ong, W. L.; Ho, G. W., Green chemistry synthesis of a nanocomposite graphene hydrogel with three-dimensional nano-mesopores for photocatalytic H₂ production. RSC Advances 2013, 3 (32), 13169-13177.
Lin, Z.; Liu, Y.; Yao, Y.; Hildreth, O. J.; Li, Z.; Moon, K.; Wong, C.-p., Superior Capacitance of Functionalized Graphene. The Jou rn al of Physical Chemist r y C 2011, 115 (14), 7120-7125. 15. Low, Q. X.; Ho, G. W., Facile structural tuning and compositing of iron oxide-graphene anode towards enhanced supacapacitive performance. Nano Energy 2014, 5, 28-35.
Choi, H.-J.; Jung, S.-M.; Seo, J.-M.; Chang, D. W.; Dai, L.; Baek, J.- B., Graphene for energy conversion and storage in fuel cells and supercapacitors. Nano Energy 2012, 1 (4), 534-551. 17. Granadeiro, C. M.; Cruz, S. M. A.; Goncalves, G.; Marques, P. A. A. P.; Costa, P. M. F. J.; Ferreira, R. A. S.; Carlos, L. D.; Nogueira, H. I. S., Photoluminescent bimetallic-3-hydroxypicolinate/graphene oxide nanocomposite. RSC Advances 2012, 2 (25), 9443-9447. 18. Ma, X.; Tao, H.; Yang, K.; Feng, L.; Cheng, L.; Shi, X.; Li, Y.; Guo, L.; Liu, Z., A functionalized graphene oxide-iron oxide nanocomposite for magnetically targeted drug delivery, photothermal therapy, and magnetic resonance imaging. Nano Res. 2012, 5 (3), 199-212. 19. Zhao, C.; Chou, S.-L.; Wang, Y.; Zhou, C.; Liu, H.-K.; Dou, S.-X., A facile route to synthesize transition metal oxide/reduced graphene oxide composites and their lithium storage performance. RSC Advances 2013, 3 (37), 16597-16603.
Du, M.; Sun, J.; Chang, J.; Yang, F.; Shi, L.; Gao, L., Synthesis of nitrogen-doped reduced graphene oxide directly from nitrogen-doped graphene oxide as a high-performance lithium ion battery anode. RSC Advances 2014, 4 (80), 42412-42417. 21. Vermisoglou, E. C.; Giannakopoulou, T.; Romanos, G.; Giannouri, M.; Boukos, N.; Lei, C.; Lekakou, C.; Trapalis, C., Effect of hydrothermal reaction time and alkaline conditions on the electrochemical properties of reduced graphene oxide. Applied surface Science 2015, 358, Part A, 100- 109.
Park, S.; An, J.; Potts, J. R.; Velamakanni, A.; Murali, S.; Ruoff, R. S., Hydrazine-reduction of graphite- and graphene oxide. Carbon 2011, 49 (9), 3019-3023.
Wong, C. P. P.; Lai, C. W.; Lee, K. M.; Hamid, S. B. A., Advanced Chemical Reduction of Reduced Graphene Oxide and I ts Photocatalytic Activity in Degrading Reactive Black 5. Materials 2015, 8 (10), 7118-7128.
Xu, C.; Shi, X.; Ji, A.; Shi, L.; Zhou, C.; C ui, Y., Fabrication and Characteristics of Reduced Graphene Oxide Produced with Different Green Reductants. P lo S one 2015, 10 (12), e01 44 842.
Zhang, X.; Sui, Z.; Xu, B.; Yue, S.; Luo, Y.; Zhan, W.; Liu, B., Mechanically strong and highly conductive graphene aerogel and its use as electrodes for electrochemical power sources. Journal of Materials Chemist r y 2011, 21 (18), 6494-6497. 26. Talbot, M. J.; White, R. G., Methanol fixation of plant tissue for Scanning Electron Microscopy improves preservation of tissue morphology and dimensions. Plant Methods 2013, 9 (1), 1-7. 27. Dohnalkova, A. C.; Marshall, M. J.; Arey, B. W.; Williams, K. H.; Buck, E. C.; Fredrickson, J. K., I maging hydrated microbial extracellular polymers: comparative analysis by electron microscopy. Applied and environmenta l microbio l ogy 2011, 77 (4), 1254-1262. 28. Lalwani, G.; Kwaczala, A. T.; Kanakia, S.; Patel, S. C.; Judex, S.; Sitharaman, B., Fabrication and characterization of three-dimensional macroscopic all-carbon scaffolds. Carbon 2013, 53, 90-100. 29. Marcano, D. C.; Kosynkin, D. V.; Berlin, J. M.; Sinitskii, A.; Sun, Z.; Slesarev, A.; Alemany, L. B.; Lu, W.; Tour, J. M., Improved Synthesis of Graphene Oxide. ACS Nano 2010, 4 (8), 4806-4814. 30. Alazmi, A.; Rasul, S.; Patole, S. P.; Costa, P. M., Comparative study of synthesis and reduction methods for graphene oxide. Polyhedron Forthcoming 2016;doi:10.101 6/j.poly.2016.04.044).
Luo, Z.; Yang, D.; Qi, G.; Shang, J.; Yang, H.; Wang, Y.; Yuwen, L.; Yu, T.; Huang, W.; Wang, L., Microwave-assisted solvothermal preparation of nitrogen and sulfur co-doped reduced graphene oxide and graphene quantum dots hybrids for highly efficient oxygen reduction. Jou rn al of Materials Chemist ry A 2014, 2 (48), 20605-20611. 32. Sawangphruk, M.; Suksomboon, M.; Kongsupornsak, K.; Khuntilo, J.; Srimuk, P.; Sanguansak, Y.; Klunbud, P.; Suktha, P.; Chiochan, P., High- performance supercapacitors based on silver nanoparticle-polyaniline- graphene nanocomposites coated on flexible carbon fiber paper. Jou rnal of Materials Chemist ry A 2013, 1 (34), 9630-9636. 33. Ramimoghadam, D.; Bin Hussein, M. Z.; Taufiq-Yap, Y. H., Hydrothermal synthesis of zinc oxide nanoparticles using rice as soft biotemplate. Chemistry Central Journal 2013, 7 (1), 1-10. 34. Hayes, W. I.; Joseph, P.; Mughal, M. Z.; Papakonstantinou, P., Production of reduced graphene oxide via hydrothermal reduction in an aqueous sulphuric acid suspension and its electrochemical behaviour. Jou rn al of solid state electrochemistry 2015, 19 (2), 361-380. 35. Feng, X., Nanocarbons for Advanced Energy Storage. Wiley: 2015. 36. Yan, J.; Wang, Q.; Wei, T.; Jiang, L.; Zhang, M.; Jing, X.; Fan, Z., Template-Assisted Low Temperature Synthesis of Functionalized Graphene for Ultrahigh Volumetric Performance Supercapacitors. A CS Nano 2014, 8 (5), 4720-4729.
Kumar, R.; Singh, R. K.; Savu, R.; Dubey, P. K.; Kumar, P.; Moshkalev, S. A., Microwave-assisted synthesis of void-induced graphene-wrapped nickel oxide hybrids for supercapacitor applications. RSC Advances 2016, 6 (32), 26612-26620. 38. Yan, J.; Liu, J.; Fan, Z.; Wei, T.; Zhang, L., High-performance supercapacitor electrodes based on highly corrugated graphene sheets. Carbon 2012, 50 (6), 2179-2188.
Shi, W.; Zhu, J.; Sim, D. H.; Tay, Y. Y.; Lu, Z.; Zhang, X.; Sharma, Y.; Srinivasan, M.; Zhang, H.; Hng, H. H.; Yan, Q., Achieving high specific charge capacitances in Fe₃ 0 4/reduced graphene oxide nanocomposites. Journal of Materials Chemistry 2011, 21 (10), 3422-3427. 40. He, P.; Yang, K.; Wang, W.; Dong, F.; Du, L.; Deng, Y., Reduced graphene oxide-CoFe₂ 0 4 composites for supercapacitor electrode. Russian Journal of Electrochemistry 2013, 49 (4), 359-364. 41. Bai, Y.; Rakhi, R. B.; Chen, W.; A l shareef, H. N., Effect of pH-induced chemical modification of hydrothermally reduced graphene oxide on supercapacitor performance. Journal of Power Sources 2013, 233, 313- 319.
Kumar, N. A.; Choi, H.-J.; Shin, Y. R.; Chang, D. W.; Dai, L.; Baek, J.-B., Polyaniline-Grafted Reduced Graphene Oxide for Efficient Electrochemical Supercapacitors. ACS Nano 2012, 6 (2), 1715-1723. 43. Lim, H. N.; Huang, N. M.; Lim, S. S.; Harrison, I.; Chia, C. H., Fabrication and characterization of graphene hydrogel via hydrothermal approach as a scaffold for preliminary study of cell growth. International Journal of Nanomedicine 2011, 6, 1817-1823. 44. Kumar, N. A.; Gambarelli, S.; Duclairoir, F.; Bidan, G.; Dubois, L., Synthesis of high quality reduced graphene oxide nanosheets free of paramagnetic metallic impurities. Journal of Materials Chemistry A 2013, 1 (8), 2789-2794. EMBODIMENTS FOR CARBON DIOXIDE CAPTURE Another application for the compositions and materials (and methods of making them) described herein is carbon dioxide capture. See, in particular, Figures 16-19. The effective capture of C 0 2 emitted by fossil-fuel-based power plants and other large industrial facilities is a top global priority to reduce the impact of global climate change and energy crisis (Chowdhury, S.; Balasubramanian, R., Highly efficient, rapid and selective C 0 2 capture by thermally treated graphene nanosheets. Jou rn al of C 0 2 Utilization 2016, 13, 50-60). As a result, several adsorbent materials have been studied for separation and storage of C 0 2 from fuel gases and other industrial exhaust streams. Recently, graphite and graphene have received a great deal of attention for gas adsorption, however, there has been little work carried out on graphene oxide (GO) for gas adsorption (Table I V) (Burress, J. W.; Gadipelli, S.; Ford, J.; Simmons, J. M.; Zhou, W.; Yildirim, T., G r aphene Oxide Framework Materials: Theoretical Predictions and Experimental Results. Angewandte Chemie International Edition 2010, 49 (47), 8902- 8904). Moreover, while GO with different degrees of oxidation and functionalization have been studied, the characterization of their porosity and/or gas adsorption properties is still overlooked. The most common GO production process is the so-called Hummer's method (or an adaptation of this). Not surprisingly, the few studies that have delved into C O 2 capture using GO have been based in GO derived from the Hummer's method without serious concerns on the steps involved. One such step, that is key is the drying methodology used after the GO product is obtained. The reported specific surface area of GO materials are less than or about 100 m 2 g-(Table V), possibly due to the GO pore network collapse and sheet re-aggregation taking place during the drying step. In this study, we illustrate that GO can be turned into a potentially relevant gas storage material by using an adapted ("Improved") Hummer's method that results in a material (improved GO, or IGO) with a higher degree of oxidation (A. Alazmi et al., Polyhedron, DOI: 10.1016/j.poly.20 1 6.04.044). Depending on the post-synthesis drying method employed, it is possible to partially tune the pore width/volume and specific surface area of the GO material. In line with this, the effect of employing vacuum, freeze and critical point drying (CPD) on the morphology, specific surface area, porosity and gas adsorption properties of I GO can be and has been determined. Our findings demonstrate for the first time that the CPD process can have a positive influence on the characteristic of GO materials, and it represents an effective strategy in the design and development of GO-based solid adsorbents for C₀ 2 capture. Overall, GO-vacuum dried material and GO-freeze-dried material are exclusively made up of micro-pores in the material. On the other hand, the GO-CPD dried material comprises micro, meso and macro pores. At the range of pressure of 0-1 bar, the micro pores are filled, while the meso and macro pores will only be filled at higher pressures (>10 bar). From the t-plot, the micro pore volume of the GO-CPD is comparable with the micro pore volume of GO-Vacuum and GO-freeze (Table 4). This can explain the comparable C₀ 2-uptake values for GO- vacuum dried, GO-freeze dried, and GO-CPD dried materials. On the other hand, our observation demonstrated that the GO prepared using Improved-Hummers' method has higher C 0 2-uptake than the GO prepared using Hummers' method (Figure 17). The filling of the meso/macro pores of GO-CPD at higher pressure (>10 bar) canimprove the C₀ SVG 16313726.12-27-2018.JQ₇ERIIURXEAPX0.SPEC.27.25.697.2595.775.2639.svg 0.147 0.26 Chemistry Black and white uptake value of these materials. Table IV. Comparison o f C O₂ adsorption by GO Adsorbent Synthesis method Drying method Porosity Temperature CO 2 Uptake at 1 bar References SVG 16313726.12-27-2018.JQ₇ERIIURXEAPX0.SPEC.28.4.358.539.2255.679.svg 0.467 6.323 Chemistry Black and white GO GO by modified Under vacuum at 50 Micropores 273 0.93 Xueta l.NanoscaleResearch t ette Hummers' method a C rs (2015)10:318 GO GO by I mproved CPD Micro/macro 273 1.8 Our work Hummer s' pores Table V. Comparison of specific surface area of GO SVG 16313726.12-27-2018.JQ₇ERIIURXEAPX0.SPEC.28.13.357.1479.2198.1582.svg 0.343 6.137 Chemistry Black and white GO from porous graphite (355 GO by Hummers' method I n vacuum 161 Ad v. Fu n ct, Mater. 2010,20,1670-1679 m z/g),+ GO from graphite (14.36 m 2/g) GO by modified Hummer's freeze-dried 102.29 Journal of S olid State Electrochem i stry, 2014. 19(2): p. 361-380 GO GO by modified Stau-denma l er's Dried at room 5.7 E. C. Vermisoglou et al./Applied surface method [temperature Sci ence 358 358 (2015) (2015) 100-109 Claims What is claimed is:
Layer stacks claimed or described, ordered top of device to substrate.
supercapacitor electrode
Materials described outside the worked examples.
graphene oxide (GO)
reduced graphene oxide (rGO)
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
BET specific surface area of rGO/CPD | 364 m2/g | reduced graphene oxide (rGO) |
supercapacitance of rGO/CPD electrode |
Patent
Atlas literature
Patent
US 10,995,003Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Zhao, B.; Liu, P.; Jiang, Y.; Pan, D.; Tao, H.; Song, J.; Fang, T.; Xu, W., Supercapacitor performances of thermally reduced graphene oxide. Jou rn al of Power Sources 2012, 198, 423-427.
Li, D.; Muller, M. B.; G il je, S.; Kaner, R. B.; Wallace, G. G., Processable aqueous dispersions of graphene nanosheets. Nat Nano 2008, 3 (2), 101- 105.
Shin, H.-J.; Kim, K. K.; Benayad, A.; Yoon, S.-M.; Park, H. K.; Jung, I.- S.; Jin, M. H.; Jeong, H.- K.; Kim, J. M.; Choi, J.-Y.; Lee, Y. H., Efficient Reduction of Graphite Oxide by Sodium Borohydride and Its Effect on El ectrical Conductance. Advanced Functional Materials 2009, 19 (12), 1987-1992.
Wang, X.; Xing, W.; Song, L.; Yang, H.; Hu, Y.; Ye o h, G. H., Fabrication and characterization of graphene-reinforced waterborne polyurethane nanocomposite coatings by the sol-gel method. Surface and Coatings Technology 2012, 206 (23), 4778-4784.
Schniepp, H. C.; Li, J.-L.; McAllister, M. J.; Sai, H.; Herrera-Alonso, M.; Adamson, D. H.; Prud'homme, R. K.; Car, R.; Saville, D. A.; Aksay, I. A., Functionalized Single Graphene Sheets Derived from Splitting Graphite Oxide. The Journal of Physical Chemist r y B 2006, 110 (17), 8535-8539.
Xiao, Y.; Li, X.; Zai, J.; Wang, K.; Gong, Y.; Li, B.; Han, Q.; Qian, X., CoFe₂ 0 4-Graphene Nanocomposites Synthesized through An Ultrasonic Method with Enhanced Performances as Anode Materials for Li-ion Batteries. Nano-Micro Letters 2014, 6 (4), 307-315.
Song, Z.; Zhang, Y.; Liu, W.; Zhang, S.; Liu, G.; Chen, H.; Qiu, J., Hydrothermal synthesis and electrochemical performance of Co₃ 0 4/reduced graphene oxide nanosheet composites for supercapacitors. Electrochimica Acta 2013, 112, 120-126.
Nassar, M. Y.; Ahmed, I. S., Hydrothermal synthesis of cobalt carbonates using different counter ions: An efficient precursor to nano- sized cobalt oxide (Co₃ 0 4). Polyhedron 2011, 30 (15), 2431-2437.
Cies i elski, W.; Tomasik, P., Thermal properties of complexes of amaranthus starch with selected metal salts. Thermochim Acta 2003, 403. 10. Wang, H.; Cui, L.-F.; Yang, Y.; Sanchez Casalongue, H.; Robinson, J. T.; Liang, Y.; Cui, Y.; Dai, H., Mn₃ 0 4-Graphene Hybrid as a High-Capacity Anode Material for Lithium I on Batteries. Journal of the American Chemical Society 2010, 132 (40), 13978-13980. 11. Li, Y.; Gao, W.; Ci, L.; Wang, C.; Ajayan, P. M., Catalytic performance of Pt nanoparticles on reduced graphene oxide for methanol electro- oxidation. Carbon 2010, 48 (4), 1124-1130. 12. Antony, R. P.; Preethi, L. K.; Gupta, B.; Mathews, T.; Dash, S.; Tyagi, A. K., Efficient electrocatalytic performance of thermally exfoliated reduced graphene oxide-Pt hybrid. Materials Research Bulletin 2015, 70, 60-67.
Gao, M.; Peh, C. K. N.; Ong, W. L.; Ho, G. W., Green chemistry synthesis of a nanocomposite graphene hydrogel with three-dimensional nano-mesopores for photocatalytic H₂ production. RSC Advances 2013, 3 (32), 13169-13177.
Lin, Z.; Liu, Y.; Yao, Y.; Hildreth, O. J.; Li, Z.; Moon, K.; Wong, C.-p., Superior Capacitance of Functionalized Graphene. The Jou rn al of Physical Chemist r y C 2011, 115 (14), 7120-7125. 15. Low, Q. X.; Ho, G. W., Facile structural tuning and compositing of iron oxide-graphene anode towards enhanced supacapacitive performance. Nano Energy 2014, 5, 28-35.
Choi, H.-J.; Jung, S.-M.; Seo, J.-M.; Chang, D. W.; Dai, L.; Baek, J.- B., Graphene for energy conversion and storage in fuel cells and supercapacitors. Nano Energy 2012, 1 (4), 534-551. 17. Granadeiro, C. M.; Cruz, S. M. A.; Goncalves, G.; Marques, P. A. A. P.; Costa, P. M. F. J.; Ferreira, R. A. S.; Carlos, L. D.; Nogueira, H. I. S., Photoluminescent bimetallic-3-hydroxypicolinate/graphene oxide nanocomposite. RSC Advances 2012, 2 (25), 9443-9447. 18. Ma, X.; Tao, H.; Yang, K.; Feng, L.; Cheng, L.; Shi, X.; Li, Y.; Guo, L.; Liu, Z., A functionalized graphene oxide-iron oxide nanocomposite for magnetically targeted drug delivery, photothermal therapy, and magnetic resonance imaging. Nano Res. 2012, 5 (3), 199-212. 19. Zhao, C.; Chou, S.-L.; Wang, Y.; Zhou, C.; Liu, H.-K.; Dou, S.-X., A facile route to synthesize transition metal oxide/reduced graphene oxide composites and their lithium storage performance. RSC Advances 2013, 3 (37), 16597-16603.
Du, M.; Sun, J.; Chang, J.; Yang, F.; Shi, L.; Gao, L., Synthesis of nitrogen-doped reduced graphene oxide directly from nitrogen-doped graphene oxide as a high-performance lithium ion battery anode. RSC Advances 2014, 4 (80), 42412-42417. 21. Vermisoglou, E. C.; Giannakopoulou, T.; Romanos, G.; Giannouri, M.; Boukos, N.; Lei, C.; Lekakou, C.; Trapalis, C., Effect of hydrothermal reaction time and alkaline conditions on the electrochemical properties of reduced graphene oxide. Applied surface Science 2015, 358, Part A, 100- 109.
Park, S.; An, J.; Potts, J. R.; Velamakanni, A.; Murali, S.; Ruoff, R. S., Hydrazine-reduction of graphite- and graphene oxide. Carbon 2011, 49 (9), 3019-3023.
Wong, C. P. P.; Lai, C. W.; Lee, K. M.; Hamid, S. B. A., Advanced Chemical Reduction of Reduced Graphene Oxide and I ts Photocatalytic Activity in Degrading Reactive Black 5. Materials 2015, 8 (10), 7118-7128.
Xu, C.; Shi, X.; Ji, A.; Shi, L.; Zhou, C.; C ui, Y., Fabrication and Characteristics of Reduced Graphene Oxide Produced with Different Green Reductants. P lo S one 2015, 10 (12), e01 44 842.
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Kumar, N. A.; Choi, H.-J.; Shin, Y. R.; Chang, D. W.; Dai, L.; Baek, J.-B., Polyaniline-Grafted Reduced Graphene Oxide for Efficient Electrochemical Supercapacitors. ACS Nano 2012, 6 (2), 1715-1723. 43. Lim, H. N.; Huang, N. M.; Lim, S. S.; Harrison, I.; Chia, C. H., Fabrication and characterization of graphene hydrogel via hydrothermal approach as a scaffold for preliminary study of cell growth. International Journal of Nanomedicine 2011, 6, 1817-1823. 44. Kumar, N. A.; Gambarelli, S.; Duclairoir, F.; Bidan, G.; Dubois, L., Synthesis of high quality reduced graphene oxide nanosheets free of paramagnetic metallic impurities. Journal of Materials Chemistry A 2013, 1 (8), 2789-2794. EMBODIMENTS FOR CARBON DIOXIDE CAPTURE Another application for the compositions and materials (and methods of making them) described herein is carbon dioxide capture. See, in particular, Figures 16-19. The effective capture of C 0 2 emitted by fossil-fuel-based power plants and other large industrial facilities is a top global priority to reduce the impact of global climate change and energy crisis (Chowdhury, S.; Balasubramanian, R., Highly efficient, rapid and selective C 0 2 capture by thermally treated graphene nanosheets. Jou rn al of C 0 2 Utilization 2016, 13, 50-60). As a result, several adsorbent materials have been studied for separation and storage of C 0 2 from fuel gases and other industrial exhaust streams. Recently, graphite and graphene have received a great deal of attention for gas adsorption, however, there has been little work carried out on graphene oxide (GO) for gas adsorption (Table I V) (Burress, J. W.; Gadipelli, S.; Ford, J.; Simmons, J. M.; Zhou, W.; Yildirim, T., G r aphene Oxide Framework Materials: Theoretical Predictions and Experimental Results. Angewandte Chemie International Edition 2010, 49 (47), 8902- 8904). Moreover, while GO with different degrees of oxidation and functionalization have been studied, the characterization of their porosity and/or gas adsorption properties is still overlooked. The most common GO production process is the so-called Hummer's method (or an adaptation of this). Not surprisingly, the few studies that have delved into C O 2 capture using GO have been based in GO derived from the Hummer's method without serious concerns on the steps involved. One such step, that is key is the drying methodology used after the GO product is obtained. The reported specific surface area of GO materials are less than or about 100 m 2 g-(Table V), possibly due to the GO pore network collapse and sheet re-aggregation taking place during the drying step. In this study, we illustrate that GO can be turned into a potentially relevant gas storage material by using an adapted ("Improved") Hummer's method that results in a material (improved GO, or IGO) with a higher degree of oxidation (A. Alazmi et al., Polyhedron, DOI: 10.1016/j.poly.20 1 6.04.044). Depending on the post-synthesis drying method employed, it is possible to partially tune the pore width/volume and specific surface area of the GO material. In line with this, the effect of employing vacuum, freeze and critical point drying (CPD) on the morphology, specific surface area, porosity and gas adsorption properties of I GO can be and has been determined. Our findings demonstrate for the first time that the CPD process can have a positive influence on the characteristic of GO materials, and it represents an effective strategy in the design and development of GO-based solid adsorbents for C₀ 2 capture. Overall, GO-vacuum dried material and GO-freeze-dried material are exclusively made up of micro-pores in the material. On the other hand, the GO-CPD dried material comprises micro, meso and macro pores. At the range of pressure of 0-1 bar, the micro pores are filled, while the meso and macro pores will only be filled at higher pressures (>10 bar). From the t-plot, the micro pore volume of the GO-CPD is comparable with the micro pore volume of GO-Vacuum and GO-freeze (Table 4). This can explain the comparable C₀ 2-uptake values for GO- vacuum dried, GO-freeze dried, and GO-CPD dried materials. On the other hand, our observation demonstrated that the GO prepared using Improved-Hummers' method has higher C 0 2-uptake than the GO prepared using Hummers' method (Figure 17). The filling of the meso/macro pores of GO-CPD at higher pressure (>10 bar) canimprove the C₀ SVG 16313726.12-27-2018.JQ₇ERIIURXEAPX0.SPEC.27.25.697.2595.775.2639.svg 0.147 0.26 Chemistry Black and white uptake value of these materials. Table IV. Comparison o f C O₂ adsorption by GO Adsorbent Synthesis method Drying method Porosity Temperature CO 2 Uptake at 1 bar References SVG 16313726.12-27-2018.JQ₇ERIIURXEAPX0.SPEC.28.4.358.539.2255.679.svg 0.467 6.323 Chemistry Black and white GO GO by modified Under vacuum at 50 Micropores 273 0.93 Xueta l.NanoscaleResearch t ette Hummers' method a C rs (2015)10:318 GO GO by I mproved CPD Micro/macro 273 1.8 Our work Hummer s' pores Table V. Comparison of specific surface area of GO SVG 16313726.12-27-2018.JQ₇ERIIURXEAPX0.SPEC.28.13.357.1479.2198.1582.svg 0.343 6.137 Chemistry Black and white GO from porous graphite (355 GO by Hummers' method I n vacuum 161 Ad v. Fu n ct, Mater. 2010,20,1670-1679 m z/g),+ GO from graphite (14.36 m 2/g) GO by modified Hummer's freeze-dried 102.29 Journal of S olid State Electrochem i stry, 2014. 19(2): p. 361-380 GO GO by modified Stau-denma l er's Dried at room 5.7 E. C. Vermisoglou et al./Applied surface method [temperature Sci ence 358 358 (2015) (2015) 100-109 Claims What is claimed is:
Layer stacks claimed or described, ordered top of device to substrate.
supercapacitor electrode
Materials described outside the worked examples.
graphene oxide (GO)
reduced graphene oxide (rGO)
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
BET specific surface area of rGO/CPD | 364 m2/g | reduced graphene oxide (rGO) |
supercapacitance of rGO/CPD electrode |
improved graphene oxide (IGO)
| 441 F/g |
reduced graphene oxide (rGO) |
CO2 uptake at 1 bar, 273 K, GO by Improved Hummers' + CPD drying | 1.8 mmol/g | improved graphene oxide (IGO) |
CO2 uptake at 1 bar, 273 K, GO by modified Hummers' + vacuum drying (prior art reference) | 0.93 mmol/g | graphene oxide (GO) |
Thickness | 50–250 µm | — |
Thickness | 50–150 µm | — |
Thickness | 100–150 µm | — |
Thickness | 1–2 mm | — |
Voltage | 0.3–0.4 V | — |
Thickness | ≤ 2 nm | — |
Thickness | ≥ 75 nm | — |
Pressure | 0–1 bar | — |
Pressure | ≥ 10 bar | — |
improved graphene oxide (IGO)
| 441 F/g |
reduced graphene oxide (rGO) |
CO2 uptake at 1 bar, 273 K, GO by Improved Hummers' + CPD drying | 1.8 mmol/g | improved graphene oxide (IGO) |
CO2 uptake at 1 bar, 273 K, GO by modified Hummers' + vacuum drying (prior art reference) | 0.93 mmol/g | graphene oxide (GO) |
Thickness | 50–250 µm | — |
Thickness | 50–150 µm | — |
Thickness | 100–150 µm | — |
Thickness | 1–2 mm | — |
Voltage | 0.3–0.4 V | — |
Thickness | ≤ 2 nm | — |
Thickness | ≥ 75 nm | — |
Pressure | 0–1 bar | — |
Pressure | ≥ 10 bar | — |
improved graphene oxide (IGO)
| 441 F/g |
reduced graphene oxide (rGO) |
CO2 uptake at 1 bar, 273 K, GO by Improved Hummers' + CPD drying | 1.8 mmol/g | improved graphene oxide (IGO) |
CO2 uptake at 1 bar, 273 K, GO by modified Hummers' + vacuum drying (prior art reference) | 0.93 mmol/g | graphene oxide (GO) |
Thickness | 50–250 µm | — |
Thickness | 50–150 µm | — |
Thickness | 100–150 µm | — |
Thickness | 1–2 mm | — |
Voltage | 0.3–0.4 V | — |
Thickness | ≤ 2 nm | — |
Thickness | ≥ 75 nm | — |
Pressure | 0–1 bar | — |
Pressure | ≥ 10 bar | — |
improved graphene oxide (IGO)
| 441 F/g |
reduced graphene oxide (rGO) |
CO2 uptake at 1 bar, 273 K, GO by Improved Hummers' + CPD drying | 1.8 mmol/g | improved graphene oxide (IGO) |
CO2 uptake at 1 bar, 273 K, GO by modified Hummers' + vacuum drying (prior art reference) | 0.93 mmol/g | graphene oxide (GO) |
Thickness | 50–250 µm | — |
Thickness | 50–150 µm | — |
Thickness | 100–150 µm | — |
Thickness | 1–2 mm | — |
Voltage | 0.3–0.4 V | — |
Thickness | ≤ 2 nm | — |
Thickness | ≥ 75 nm | — |
Pressure | 0–1 bar | — |
Pressure | ≥ 10 bar | — |
