Nano- to micro-pore characterization by synchrotron radiation SAXS and nano-CT for bituminous coals
Yixin ZHAO, Chujian HAN, Yingfeng SUN, Nima Noraei DANESH, Tong LIU, Yirui GAO
Nano- to micro-pore characterization by synchrotron radiation SAXS and nano-CT for bituminous coals
Considering the complementarity of synchrotron radiation SAXS and nano-CT in the pore structure detection range, synchrotron radiation SAXS and nano-CT methods were combined to characterize the nano- to micro-pore structure of two bituminous coal samples. In mesopores, the pore size distribution curves exhibit unimodal distribution and the average pore diameters are similar due to the affinity of metamorphic grades of the two samples. In macropores, the sample with higher mineral matter content, especially clay mineral content, has a much higher number of pores. The fractal dimensions representing the pore surface irregularity and the pore structure heterogeneity were also characterized by synchrotron radiation SAXS and nano-CT. The fractal dimensions estimated by both methods for different pore sizes show consistency and the sample with smaller average pore diameters has a more complex pore structure within the full tested range.
synchrotron radiation / SAXS / nano-CT / pore size distribution / fractal / coal
[1] |
Bale H D, Schmidt P W (1984). Small-angle X-ray-scattering investigation of submicroscopic porosity with fractal properties. Phys Rev Lett, 53(6): 596–599
CrossRef
Google scholar
|
[2] |
Baradez M O, Mcguckin C P, Forraz N, Pettengell R, Hoppe A (2004). Robust and automated unimodal histogram thresholding and potential applications. Pattern Recognit, 37(6): 1131–1148
CrossRef
Google scholar
|
[3] |
Beaucage G, Kammler H K, Pratsinis S E (2004). Particle size distributions from small-angle scattering using global scattering functions. J Appl Cryst, 37(4): 523–535
CrossRef
Google scholar
|
[4] |
Benedetti A, Ciccariello S (1996). Coal rank and shape of the small-angle X-ray intensity. J Phys III, 6(11): 1479–1487
CrossRef
Google scholar
|
[5] |
Coutinho J, Kräutner H, Sassi F, Schmid R, Sen S (2007). Recommendations by the IUGS subcommission on the systematics of metamorphic rocks: Web version 01.02.07, 16–23
|
[6] |
Gallagher N, Wise G (1981). A theoretical analysis of the properties of median filters. IEEE Trans Acoust, 29(6): 1136–1141
CrossRef
Google scholar
|
[7] |
Giffin S, Littke R, Klaver J, Urai J L (2013). Application of BIB-SEM technology to characterize macropore morphology in coal. Int J Coal Geol, 114: 85–95
CrossRef
Google scholar
|
[8] |
Guinier A, Fournet G (1955). Small-angle Scattering of X-rays. Hoboken: Wiley
|
[9] |
Jellinek M H, Soloman E, Fankuchen I (1946). Measurement and analysis of small-angle X-Ray scattering. Ind Eng Chem Anal Ed, 18(3): 172–175
CrossRef
Google scholar
|
[10] |
Jiang L M, Sun J M, Liu X F, Wang H T (2012). Numerical study of the effect of natural gas saturation of the reservoir rock’s elastic parameters. Well Logging Technol, 36: 239–243 (in Chinese)
|
[11] |
Li P P, Zhang X D, Zhang S (2018). Structures and fractal characteristics of pores in low volatile bituminous deformed coals by low-temperature N2 adsorption after different solvents treatments. Fuel, 224: 661–675
CrossRef
Google scholar
|
[12] |
Luo L, Liu J X, Zhang Y C, Zhang H, Ma J F, You Y L, Jiang X M (2016). Application of small angle X-ray scattering in evaluation of pore structure of superfine pulverized coal/char. Fuel, 185: 190–198
CrossRef
Google scholar
|
[13] |
Li Z H, Gong Y J, Wu D, Sun Y H, Wang J, Liu Y, Dong B Z (2001). A negative deviation from Porod’s law in SAXS of organo-MSU-X. Microporous Mesoporous Mater, 46(1): 75–80
CrossRef
Google scholar
|
[14] |
Li Z H, Sun J H, Wu D, Sun Y H, Liu Y, Sheng W J, Dong B Z (2000). Determination of specific surfaces of silica xerogets by SAXS. Chin Sci Bull, 45(15): 1386–1390
CrossRef
Google scholar
|
[15] |
Li Z T (2018). Evolution of pore-fractures of coal reservoir and its impact on CBM microcosmic flow. Dissertation for the Doctoral Degree. Beijing: China University of Geosciences (in Chinese)
|
[16] |
Li Z T, Liu D M, Cai Y D, Ranjith P G, Yao Y B (2017). Multi-scale quantitative characterization of 3-D pore-fracture networks in bituminous and anthracite coals using FIB-SEM tomography and X-ray m-CT. Fuel, 209: 43–53
CrossRef
Google scholar
|
[17] |
Mahamud M, Novo M (2008). The use of fractal analysis in the textural characterization of coals. Fuel, 87(2): 222–231
CrossRef
Google scholar
|
[18] |
Mares T E, Radliński A P, Moore T A, Cookson D, Thiyagarajan P, Ilavsky J, Klepp J (2009). Assessing the potential for CO2 adsorption in a subbituminous coal, Huntly Coalfield, New Zealand, using small angle scattering techniques. Int J Coal Geol, 77(1–2): 54–68
CrossRef
Google scholar
|
[19] |
Mastalerz M, He L, Melnichenko Y B, Rupp J A (2012). Porosity of coal and shale: insights from gas adsorption and SANS/USANS techniques. Energy Fuels, 26(8): 5109–5120
CrossRef
Google scholar
|
[20] |
Nakagawa T, Komaki I, Sakawa M, Nishikawa K (2000). Small angle X-ray scattering study on change of fractal property of Witbank coal with heat treatment. Fuel, 79(11): 1341–1346
CrossRef
Google scholar
|
[21] |
Pan J N, Niu Q H, Wang K, Shi X H, Li M (2016). The closed pores of tectonically deformed coal studied by small-angle X-ray scattering and liquid nitrogen adsorption. Micropor Mesopor Mater, 224: 245–252
CrossRef
Google scholar
|
[22] |
Potton J A, Daniell G J, Rainford B D (1988). A new method for the determination of particle size distributions from small-angle neutron scattering measurements. J Appl Cryst, 21(6): 891–897
CrossRef
Google scholar
|
[23] |
Radlinski A P, Mastalerz M, Hinde A L, Hainbuchner M, Rauch H, Baron M, Lin J S, Fan L, Thiyagarajan P (2004). Application of SAXS and SANS in evaluation of porosity, pore size distribution and surface area of coal. Int J Coal Geol, 59(3-4): 245–271
CrossRef
Google scholar
|
[24] |
Reich M H, Snook I K, Wagenfeld H K (1992). A fractal interpretation of the effect of drying on the pore structure of Victorian brown coal. Fuel, 71(6): 669–672
CrossRef
Google scholar
|
[25] |
Rodrigues C F, Lemos de Sousa M J (2002). The measurement of coal porosity with different gases. Int J Coal Geol, 48(3-4): 245–251
CrossRef
Google scholar
|
[26] |
Roess L C, Shull C G (1947). X-Ray scattering at small angles by finely-divided solids. Part II: exact theory for random distributions of spheroidal particles. J Appl Phys, 18(3): 308–313
CrossRef
Google scholar
|
[27] |
Rootare H M, Prenzlow C F (1967). Surface areas from mercury porosimeter measurements. J Phys Chem, 71(8): 2733–2736
CrossRef
Google scholar
|
[28] |
Rouquerol J K K, Avnir D, Fairbridge C W, Everett D H, Haynes J M, Pernicone N, Ramsay J D F, Sing K S W, Unger K K (1994). Recommendations for the characterization of porous solids (Technical Report). Pure Appl Chem, 66(8): 1739–1758
CrossRef
Google scholar
|
[29] |
Song X X, Tang Y G, Li W, Ceng F G, Xiang J H (2014). Pore structure in tectonically deformed coals by small angle X-ray scattering. J China Coal Soc, 39: 719–724 (in Chinese)
|
[30] |
Suggate R P, Dickinson W W (2004). Carbon NMR of coals: the effects of coal type and rank. Int J Coal Geol, 57(1): 1–22
CrossRef
Google scholar
|
[31] |
Sun Y F, Zhao Y X, Wang X, Peng L, Sun Q (2019). Synchrotron radiation facility-based quantitative evaluation of pore structure heterogeneity and anisotropy in coal. Pet Explor Dev, 46(6): 1195–1205
CrossRef
Google scholar
|
[32] |
Sun Y F, Zhao Y X, Yuan L (2018a). Quantifying nano-pore heterogeneity and anisotropy in gas shale by synchrotron radiation nano-CT. Micropor Mesopor Mater, 258: 8–16
CrossRef
Google scholar
|
[33] |
Sun Y F (2018b). Investigation of gas adsorption and diffusion behavior based on three-dimensional pore structure of coal. Dissertation for the Doctoral Degree. Beijing: China University of Mining and Technology (in Chinese)
|
[34] |
Syed R, Sen D, Mani Krishna K V, Ghosh S K (2018). Fabrication of highly ordered nanoporous alumina membranes: probing microstructures by SAXS, FESEM and AFM. Microporous Mesoporous Mater, 264: 13–21
CrossRef
Google scholar
|
[35] |
Wang H, Liu Y, Song Y, Zhao Y, Zhao J (2012). Fractal dimension analysis on pore structure of artificial cores using magnetic resonance imaging. In: 2nd International Conference on Consumer Electronics, Communications and Networks, 2593–2596
CrossRef
Google scholar
|
[36] |
Wang Y, Wang L H, Wang J Q, Zheng J G, Wang C C, Fu Y A, Song Y F, Wang Y F, Liu D Z, Jin C (2019). Multiscale characterization of three-dimensional pore structures in a shale gas reservoir: a case study of the Longmaxi shale in Sichuan basin, China. J Nat Gas Sci Eng, 66: 207–216
CrossRef
Google scholar
|
[37] |
Xie H P (1993). Fractals in Rock Mechanics. Boca Raton: CRC Press
|
[38] |
Zhang R, Liu S, Wang Y (2017). Fractal evolution under in situ pressure and sorption conditions for coal and shale. Sci Rep, 7(1): 8971
CrossRef
Pubmed
Google scholar
|
[39] |
Zhang S H, Tang D Z, Tang S H, Xu H, Lin W J, Zhang B (2008). The characters of coal beds micropores and its influence factors in the eastern margin of Ordos Basin. Acta Geol Sin, 82: 1341–1349 (in Chinese)
|
[40] |
Zhao Y X, Liu S M, Elsworth D, Jiang Y D, Zhu J (2014). Pore structure characterization of coal by synchrotron small-angle X-ray scattering and transmission electron microscopy. Energy Fuels, 28(6): 3704–3711
CrossRef
Google scholar
|
[41] |
Zhao Y X, Peng L, Liu S M, Cao B, Sun Y F, Hou B F (2019). Pore structure characterization of shales using synchrotron SAXS and NMR cryoporometry. Mar Pet Geol, 102: 116–125
CrossRef
Google scholar
|
[42] |
Zhao Y X, Sun Y F, Liu S M, Chen Z W, Yuan L (2018). Pore structure characterization of coal by synchrotron radiation nano-CT. Fuel, 215: 102–110
CrossRef
Google scholar
|
[43] |
Zhao Y X, Zhu G P, Dong Y H, Danesh N N, Chen Z W, Zhang T (2017). Comparison of low-field NMR and microfocus X-ray computed tomography in fractal characterization of pores in artificial cores. Fuel, 210: 217–226
CrossRef
Google scholar
|
[44] |
Zheng S J, Yao Y B, Liu D M, Cai Y D, Liu Y (2018). Characterizations of full-scale pore size distribution, porosity and permeability of coals: a novel methodology by nuclear magnetic resonance and fractal analysis theory. Int J Coal Geol, 196: 148–158
CrossRef
Google scholar
|
/
〈 | 〉 |