ISSN 1000-6818CN 11-1892/O6CODEN WHXUEU
Acta Phys Chim Sin >> 0,Vol.>> Issue()>> 0-0     doi: 10.3866/PKU.WHXB201704142         中文摘要
Accepted manuscript
Nuclear Magnetic Resonance Characterization of Nano Self-Assembly γ-Al2O3 Pore Structure
WANG Lin, XIAO Li-Zhi, GUO Long, LIAO Guang-Zhi, ZHANG Yan, GE Ge
State Key Laboratory of Petroleum Resources and Prospecting, China University of Petroleum, Beijing 102249, P. R. China
Full text: PDF (1578KB) Export: BibTeX | EndNote (RIS)

Nano self-assembled γ-Al2O3, having two kinds of nano-scale pore structures, which can be used as a catalyst carrier suitable for large molecule diffusion and shale gas reservoir models. Characterization of the pore structures in nanomaterials are scanning electron microscopy, nitrogen adsorption method, mercury injection method, etc. These characterization techniques have their own limitations. This paper utilized nuclear magnetic resonance (NMR) relaxation measurements to study and quantitatively characterize the pore structures of nano self-assembled γ-Al2O3. Random walker simulation and error function analysis were used to explore the surface relaxation strength and pore size distribution of nano self-assembled γ-Al2O3. The random walker simulation results show that the main apertures of nano self-assembled γ-Al2O3 are 5-7 nm and 30-42 nm; NMR experiments through error function analysis show that the main apertures of the nano self-assembled material are 5-9 nm and 29-47 nm. Nitrogen adsorption only characterized the microporous, mesoporous, and part of the macroporous structures. The pore diameters greater than 100 nm cannot be detected by the nitrogen adsorption method. The mercury injection method characterizes apertures of size less than 10 nm relatively inaccurately. Nuclear magnetic relaxation can comprehensively characterize bimodal pore system of nano self-assembled γ-Al2O3 of size 2.8-315 nm. As one of the NMR measurements, the T2 spectrum signal amplitude ratio of three samples, S-1, S-2 and S-3 are 0.603, 1.15, 1.84, directly reflect the variety of their micropores and mesopores chemical Al2O3 material ratio 0.85, 1.38, 1.7 respectively. The suggested method can be applied to the investigation for shale gas pore structure and associated mechanisms.

Keywords: Pore distribution   Nuclear magnetic relaxation   Radom walker   Error function analysis   Nano self-assambly  
Received: 2017-03-01 Accepted: 2017-04-05 Publication Date (Web): 2017-04-14
Corresponding Authors: XIAO Li-Zhi Email:,

Fund: The project was supported by the National Natural Science Foundation of China (21427812) and the "111 Project" Discipline Innovative Engineering Plan, China (B13010).

Cite this article: WANG Lin, XIAO Li-Zhi, GUO Long, LIAO Guang-Zhi, ZHANG Yan, GE Ge. Nuclear Magnetic Resonance Characterization of Nano Self-Assembly γ-Al2O3 Pore Structure[J]. Acta Phys. -Chim. Sin., 0, (): 0-0.    doi: 10.3866/PKU.WHXB201704142

(1) Vartuli, J. C.; Kresge, C. T.; Leonowicz, M. E.; Chu, A. S.; McCullen, S. B.; Johnson, I. D.; Sheppard, E. W. Chem. Mater. 1994, 6, 2070. doi: 10.1021/cm00047a029
(2) Beck, J. S.; Vartuli, J. C.; Roth, W. J.; Leonowicz, M. E.; Kresge, C. T.; Schmitt, K. D.; Chu, C. T-W.; Olson, D. H.; Sheppard, E. W.; McCullen, S. B.; Higgins, J. B.; Schlenker, J. L. J. Am. Chem. Soc. 1992, 114, 10834. doi: 10.1021/ja00053a020
(3) Imhof, A.; Pine, D. J. Nature. 1997, 389, 948. doi: 10.1038/40105
(4) Kresge, C. T.; Leonowicz, M. E.; Roth, W. J.; Vartuli, J. C.; Beck, J. S. Nature 1992, 356, 710. doi: 10.1038/359710a0
(5) Zeng, S. Petrol. Refin. Eng. 2011 , 41, 39. [曾松. 炼油技术与工程, 2011, 41, 39.] doi: 10.3969/j.issn.1002-106x.2011.09.011
(6) Javadpour, F. J. Can. Pet. Technol. 2009, 48, 16. doi: 10.2118/09-08-16-DA
(7) Javadpour, F.; Fisher, D.; Unsworth, M. J. Can. Pet. Technol. 2007, 46, 55. doi: 10.2118/07-10-06
(8) Zolfaghari, A.; Dehghanpour, H. A Comparative Study of Pore Size Distribution in Gas Shales. In Society of Petroleum Engineers, SPE Asia Pacific Unconventional Resources Conference and Exhibition, Brisbane, Australia, November 9-11, 1-14
(9) Elgmati, M. Shale Gas Rock Characterization and 3D Submicron Pore Network Reconstruction. M. S. Dissertation, Missouri University of Science and Technology, Missouri, 2011.
(10) Loucks, R. G.; Reed, R. M.; Ruppel, S. C.; Jarvie, D. M. J. Sediment. Res. 2009, 79, 848. doi: 10.2110/jsr.2009.092
(11) Chen, S. B.; Zhu, Y. M.; Wang, H. Y.; Liu, H. L.; Wei W.; Fang, J. H. J. China. Coal. Soc. 2012, 3, 438. [陈尚斌, 朱炎铭, 王红岩, 刘洪林, 魏伟, 方俊华. 煤炭学报, 2012, 3, 438.] doi: 10.13225/j.cnki.jccs.2012.03.007
(12) Chalmers, G. R.; Bustin, R. M.; Power, I. M. AAPG Bull. 2012, 96, 1099. doi: 10.1306/10171111052
(13) Rouquerol, J.; Avnir, D.; Fairbridge, C. W.; Everett, D. H.; Haynes, J. H.; Pernicone, N.; Ramsay, J. D. F.; Sing, K. S. W.; Unger, K. K. Pure Appl. Chem. 1994, 66, 1739. doi: 10.1351/pac199466081739
(14) Li, J. X.; Zhang, L. X.; Yang, L. Mineralogy and Petrology. The University of Electronic Science and Technology Press: Chengdu, 2014; pp 50-170. [李景霞, 张立新, 杨丽. 矿物岩石学. 成都: 电子科技大学出版社, 2014: 50-170.]
(15) Xiao, L. Z.; Coates, G. R.; Prammer, M. G. NMR Logging Principles and Applications. Gulf Publishing Company: Houston, 1999; pp 10-200.
(16) Tiumer, A. J. Pet. Technol. 1969, 21, 775. doi: 10.2118/2045-PA
(17) Kenyon, W. E.; Day, P. I.; Straley, C.; Willemsen, J. F. SPE Form. Eval. 1988, 3, 622. doi: 10.2118/15643-PA
(18) Gallegos, D. P.; Smith, D. M. J. Colloid Interface Sci. 1988, 122, 143. doi: 10.1016/0021-9797(88)90297-4
(19) Straley, C.; Morriss, C. E.; Kenyon, W. E.; Howard, J. J. NMR in Partially Saturated Rocks: Laboratory Insights on Free Fluid Index and Comparison with Borehole Logs. In Society of Petrophysicists and Well-Log Analysts, SPWLA 32nd Annual Logging Symposium, Midland, Texas, June 16-19, 1991, 143-153
(20) Sigal, R. F.; Odusina, E. Petrophysics. 2010, 52, 32
(21) Hinai, A. A.; Rezaee, R.; Esteban, L.; Labani, M. J. Unconvent. Oil Gas Resources 2014, 8, 13. doi: 10.1016/j.juogr.2014.06.002
(22) Wang, D. C. Sci. China Ser. B-Chem. 2009, 52, 2114. doi: 10.1007/s11426-009-0290-x
(23) Straley, C.; Rossini, D.; Vinegar, H.; Tutunjian, P.; Morriss, C. Log Anal. 1997, 38, 84.
(24) Kleinberg, R. L.; Vinegar, H. J. Log Anal. 1996, 37, 6, 20
(25) Liu, T. Y.; Xiao, L. Z.; Fu, R. S. Chin. J. Geophys.-Chin. Ed. 2004, 47, 663. [刘堂晏, 肖立志, 傅容珊. 地球物理学报, 2004, 47, 663.] doi: 10.3321/j.issn:0001-5733.2004.04.017
(26) Martin, P.; Dacy, J. Effective Qv by NMR Core Tests. In Society of Petrophysicists and Well-Log Analysts, SPWLA 45th Annual Logging Symposium, Noordwijk, Netherlands, June 6-9, 2004, 1-14
(27) Toumelin, E.; Torres-Verdin, C.; Sun, B. Q.; Dunn, K J. J. Magn. Reson. 2007 , 188, 83. doi: 10.1016/j.jmr.2007.05.024
(28) Toumelin, E.; Torres-Verdin, C.; Chen, S. SPE Reserv. Eval. Eng. 2003, 6, 234. doi: 10.2118/85635-PA
(29) Carneiro, G.; Souza, A.; Boyd, A.; Schwartz, L.; Song, Y. Q.; Azeredo, R.; Trevizan, W.; Santos, B.; Rios, E.; Machado, V. Evaluating Pore Space Connectivity by NMR Diffusive Coupling. In Society of Petrophysicists and Well-Log Analysts, SPWLA 55th Annual Logging Symposium, Abu Dhabi, United Arab Emirates, May 18-22, 2014, 1-7.

1. DU Xue-Lian, CONG Ye, JIANG Lu, LI Xuan-Ke, CUI Zheng-Wei, DONG Zhi-Jun, YUAN Guan-Ming, ZHANG Jiang.Preparation and Structure Regulation of Silicon Carbide-Derived Carbon/ Spherical Natural Graphite Composites[J]. Acta Phys. -Chim. Sin., 2015,31(3): 583-588
2. SUN Gang-Wei, SONG Wen-Hua, LIU Xiao-Jun, QIAO Wen-Ming, LING Li-Cheng.Asymmetric Capacitance Behavior Based on the Relationship between Ion Dimension and Pore Size[J]. Acta Phys. -Chim. Sin., 2011,27(02): 449-454
3. WU Jian, WANG Yu, HUANG Feng, YANG Yang, MENG Chang-Gong.Thermal Diffusion Synthesis and Characterization of SnO2 Clusters within ZSM-5 Crystals[J]. Acta Phys. -Chim. Sin., 2010,26(06): 1705-1710
4. Le Yuan; Chen Jian-Feng; Wang Wen-Chuan.Determination of Pore Size Distribution of Silica Hollow Microspheres by Experiment and Simulation[J]. Acta Phys. -Chim. Sin., 2004,20(11): 1303-1307
5. Shao Xiao-Hong;Zhang Xian-Ren;Wang Wen-Chuan.Comparison of Density Functional Theory and Molecular Simulation Methods for Pore Size Distribution of Mesoporous Materials[J]. Acta Phys. -Chim. Sin., 2003,19(06): 538-542
6. Dong Song-Tao;Li Xuan-Wen;Li Da-Dong;Shi Ya-Hua;Nie Hong;Kang Xiao-Hong.Study on the Formation of Mesopore during Hydrothermal Dealumination of Y Zeolite[J]. Acta Phys. -Chim. Sin., 2002,18(03): 201-206
7. Liu Zhen-Yu;Zheng Jing-Tang;Wang Mao-Zhang;Zhang Bi-Jiang.Study for Nitrogen Adsorption of PAN-based Activated Carbon Fibers[J]. Acta Phys. -Chim. Sin., 2001,17(07): 594-599
8. Wang Wen-Tao,Zhong Bang-Ke.The Preparation and Characterization of Alumina Membranes Supported by Porous Titanium Plate[J]. Acta Phys. -Chim. Sin., 1996,12(01): 85-90
Copyright © 2006-2016 Editorial office of Acta Physico-Chimica Sinica
Address: College of Chemistry and Molecular Engineering, Peking University, Beijing 100871, P.R.China
Service Tel: +8610-62751724 Fax: +8610-62756388
^ Top