Ex situ transmission electron microscopy: A fixed-bed reactor approach

Microscopy and Microanalysis

Volumn 12, Issue 2, 2006, Pages 135-144

  Kliewer, Chris E ^a   Kiss, Gabor ^a   DeMartin, Gregory J ^a  

^a EXXONMOBIL UPSTREAM RESEARCH COMPANY   (United States)

Author keywords

ex situ transmission electron microscopy; Oxidation

Indexed keywords

COPPER;

ARTICLE; CHEMISTRY; ELECTRON MICROSCOPY; EQUIPMENT DESIGN; INDUSTRY; INSTRUMENTATION; METHODOLOGY; OXIDATION REDUCTION REACTION; REPRODUCIBILITY; SENSITIVITY AND SPECIFICITY;

COPPER; EQUIPMENT DESIGN; INDUSTRY; MICROSCOPY, ELECTRON; OXIDATION-REDUCTION; REPRODUCIBILITY OF RESULTS; SENSITIVITY AND SPECIFICITY;

EID: 33644849143     PISSN: 14319276     EISSN: 14358115     Source Type: Journal    
DOI: 10.1017/S1431927606060077     Document Type: Article

References (117)

1. ABRAMS, I.M. & MCBAIN, J.W. (1944a). A closed cell for electron microscopy. J Appl Phys 15, 607-609.
2. ABRAMS, I.M. & MCBAIN, J.W. (1944b). A closed cell for electron microscopy. Science 100, 273-274.
3. ALANI, P. & PAN, M. (2000). "In-situ" TEM studies and "real-time" digital imaging. Microsc Microanal 6(Suppl. 2), 1018-1019.
4. ALLARD, L.F., AILEY, K.S., DAYTE, A.K. & BIGELOW, W.C. (1997). An ex situ reactor with anaerobic specimen transfer capabilities for TEM studies of reactive (catalyst) systems. Microsc Microanal 3(Suppl. 2), 595-596.
5. BELLARE, J.R. (1988). Cryo-electron and optical microscopy of surfactant microstructures. Ph.D. Thesis, University of Minnesota.
6. BHARADWAJ, M.D., TROPIA, L., GIBSON, M. & YANG, J.C. (2000). Initial kinetics of copper oxidation in different oxidizing atmospheres as studied by in situ UHV-TEM. Microsc Microanal 6(Suppl. 2), 42-43.
7. BOYES, E.D. (1997). Controlled environment (ECELL) HREM. Microsc Microanal 3(Suppl. 2), 589-599.
8. BOYES, E.D. (2004). ETEM issues and opportunities for dynamic in situ experiments. Microsc Microanal 10(Suppl. 2), 130-131.
9. BOYES, E.D. & GAI, P.L. (1997). Environmental high resolution electron microscopy and applications to chemical science. Ultramicroscopy 6, 219-212.
10. BOYES, E.D. & GAI, P.L. (2004). ETEM issues and opportunities for dynamic in situ experiments. Microsc Today 12, 24-27.
11. BUTLER, E.P. & HALE, K.F. (1981). Dynamic Experiments in the Electron Microscope. Amsterdam: North-Holland.
12. CASTNER, D.G. & CHAN, I. (1986). Controlled atmosphere catalyst characterization by X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XAS), and analytical electron microscopy (AEM). In Microbeam Analysis Proceedings, Romig, Jr., A.D., and Chambers, W.F. (Eds.), pp. 617-619. San Francisco: San Francisco Press, Inc.
13. CASTNER, D.G., WATSON, P.R. & CHAN, I. (1989). X-ray absorption spectroscopy, X-ray photoelectron spectroscopy, and analytical electron microscopy studies in cobalt catalysts 1. Characterization of calcined catalysts. J Phys Chem 93, 3188-3194.
14. CHAN, I. (1985). A controlled atmosphere specimen holder for transmission electron microscopy. J Electron Microsc Tech 2, 525-532.
15. CHEN, J.J. & RUCKENSTEIN, E. (1981). Role of interfacial phenomena in the behavior of alumina-supported palladium crystallites in oxygen. J Phys Chem 85, 1606-1612.
16. CHIOU, W.A. & MITRA, R. (2000). In situ TEM study of straining of free standing nickel thin films. Microsc Microanal 6(Suppl. 2), 464-465.
17. 2. Microsc Microanal 1(Suppl. 2), 252-253.
18. CRONIN, S.B., LIN, Y.M., RABIN, O., BLACK, M.R., GAI, P.L., DRESSELHAUS, G. & DRESSELHAUS, M. (2001). Bismuth nanowires for potential applications in nanoscale electronics technology. Microsc Microanal 7(Suppl. 2), 418-419.
19. CROZIER, P.A. (2001). In situ characterization of dynamic changes in the microstructure and chemistry of catalysts. Microsc Microanal 7(Suppl 2), 1058-1059.
20. CROZIER, P.A. & DAYTE, A.K. (1999). In-situ HREM observation of reduction of PdO to Pd metal. Microsc Microanal 5(Suppl. 2), 336-337.
21. CROZIER, P.A. & SHARMA, R. (1998). In situ oxidation and reduction of small Pd particles on silica. Microsc Microanal 4(Suppl. 2), 748-749.
22. DAHMEN, U., RADETIC, T., HAGEGE, S., ZHANG, L. & JOHNSON, E. (2003). TEM observations on the role of defects in melting, migration and transformation of Pb-rich precipitates in Al. Microsc Microanal 9(Suppl. 2), 54-55.
23. EDINGTON, J.W. (1976). Practical Electron Microscopy in Materials Science. Princeton, NJ: Van Nostrand Reinhold Company.
24. FONTANA, M.G. & GREENE, N.D. (1978). Corrosion Engineering, 2nd ed. New York: McGraw-Hill Inc.
25. 3. Phil Mag A 43, 841-855.
26. GAI, P.L. (1997a). A new structural transformation mechanism in catalytic oxides. Acta Cryst B 53, 346-352.
27. GAI, P.L. (1997b). Unveiling novel reaction processes in catalysis by environmental HREM (EHREM). Microsc Microanal 3(Suppl. 2), 617-618.
28. GAI, P.L. (1998). Direct probing of gas molecule-solid catalyst interactions on the atomic scale. Adv Mater 10, 1259-1263.
29. GAI, P.L. (1999). Designer nanostructures of catalysts in the environmental-HREM. Microsc Microanal 5(Suppl. 2), 686-687.
30. GAI, P.L. (2002). In situ molecular imaging of heterogeneous catalytic processes in liquid environments. Microsc Microanal 8(Suppl. 2), 412-413.
31. GAI, P.L. (2004). In situ environmental TEM (ETEM) of n-butane oxidation: Advances and challenges in the catalyst microstructural design. Microsc Microanal 10(Suppl. 2), 38-39.
32. GAI, P.L., BOYES, E.D. & BART, J.C.J. (1982). Electron microscopy of industrial catalysts. Phil Mag A 45, 531-547.
33. GAI, P.L. & KOURTAKIS, K. (1995). Solid-state defect mechanism in vanadyl pyrophosphate catalysts: Implications for selective oxidation. Science 267, 661-663.
34. GAI, P.L. & KOURTAKIS, K. (1998). Effects of cation promoters in selective catalyzation of n-butane. Microsc Microanal 4(Suppl. 2), 742-743.
35. GAI, P.L., KOURTAKIS, K., COULSON, D.R. & SONNICHSEN, G.C. (1997). HREM microstructural studies on the effect of steam exposure and cation promoters on vanadium phosphorous oxides: New correlations with n-butane oxidation reaction chemistry. J Phys Chem B 101, 9916-9925.
36. GAI, P.L., KURTAKIS, K. & ZIEMECKI, S. (2000). In situ environmental high resolution electron microscopy of adiponitrile hydrogenation. Microsc Microanal 6(Suppl. 2), 6-7.
37. GAI, P.L., KOURTAKIS, K. & ZIEMECKI, S. (2001). In situ nanoscale studies of liquid polymerization reactions in the manufacture of polyamides and combinatorial catalysts. Microsc Microanal 7(Suppl. 2), 1060-1061.
38. GAI, P.L., SMITH, B.C. & OWEN, G. (1990). Bulk diffusion of metal particles on ceramic substrates. Nature 348, 430-432.
39. GAI-BOYES, P.L. (1992). Defects in oxide catalysts: Fundamental studies of catalyst in action. Catal Rev Sci Eng 34, 1-54.
40. GAI-BOYES, P.L., SALTZBERG, M.A. & VEGA, A. (1993). Structures and stabilization mechanisms in chemically stabilized ceramics. J Sol State Chem 106, 35-47.
41. GE, D., DOMNICH, V. & GOGOTSI, Y. (2003). In situ TEM study of thermal stabilities of metastable silicon phases. Microsc Microanal 9(Suppl. 2), 484CD-485CD.
42. HANSEN, T.W., WAGNER, J.B., HANSEN, P.L., DAHL, S., TOPSOE, H. & JACOBSEN, C.J.H. (2001). Atomic-resolution in situ transmission electron microscopy of a promoter of a heterogeneous catalyst. Science 294, 1508-1510.
43. HAQUE, M.A., SAIF, M.T.A., ROBACH, J.S. & ROBERTSON, M. (2003). Correlating deformation mechanisms with mechanical properties in free stranding thin metallic films. Microsc Microanal 9(Suppl. 2), 898CD-899CD.
44. HATTAR, K., HAN, J., SAIF, T. & ROBERTSON, I.M. (2004). Development and application of a MEMS-based in situ TEM straining device for ultra-fine grained metallic systems. Microsc Microanal 10(Suppl. 2), 50-51.
45. HELVEG, S., LOPEZ-CARTES, C., SEHESTED, J., HANSEN, P.L., CLAUSEN, B.S., ROSTRUP NIELSEN, J.R., ABILD-PEDERSEN, F. & NORSKOV, J.K. (2004). Atomic-scale imaging of carbon nanofiber growth. Nature 27, 426-429.
46. HIRSCH, P., HOWIE, A., NICHOLSON, R.B., PASHLEY, D.W. & WHELAN, M.J. (1965). Electron Microscopy of Thin Crystals. New York: Robert E. Krieger Publishing Company.
47. HOWE, J.M. (1995). In situ hot stage high-resolution transmission electron microscope studies of the mechanisms and kinetics of precipitation reactions. Microsc Microanal 1, 228-229.
48. KAMINO, T., YAGUCHI, T. & HASHIMOTO, T. (2003). High temperature in situ electron microscopy using a dedicated scanning transmission electron microscope. Microsc Microanal 9(Suppl. 2), 922CD-923CD.
49. KLIE, R.F., BROWNING, N.D. & ZHU, Y. (2002). Atomic scale characterization of oxygen vacancy dynamics by in situ reduction and analytical atomic resolution STEM. Microsc Microanal 8(Suppl. 2), 1396CD-1370CD.
50. KLIEWER, C.E., DISKO, M.M., SOLED, S.L. & DEMARTIN, G.J. (1999). A reactor for "ex-situ" TEM catalyst characterization. Microsc Microanal 5(Suppl. 2), 926-927.
51. KLIEWER, C.E., DISKO, M.M., SOLED, S.L., DEMARTIN, G.J., BAUMGARTNER, J.E. & MISEO, S. (2000). Copper oxidation via "ex-situ" TEM. Microsc Microanal 6(Suppl. 2), 378-379.
52. KONNO, T.J. & SINCLAIR, R. (1992). Crystallization of silicon in aluminum/amorphous silicon multilayers. Phil Mag B 66, 749-765.
53. KONNO, T.J. & SINCLAIR, R. (1995). Metal-mediated crystallization of amorphous silicon in silicon-silver layered systems. Phil Mag B 71, 163-178.
54. LIAN, J., WANG, L.M. & EWING, R.C. (2002). In situ TEM study of order-disorder transition in murataite ceramics. Microsc Microanal 8(Suppl. 2), 1424CD-1425CD.
55. LIAN, J., WANG, L.M. & EWING, R.C. (2004). Phase decomposition- induced nanocrystal formation and structural disordering in murataite structure. Microsc Microanal 10(Suppl. 2), 586-587.
56. LIU, R.J., CROZIER, P.A., SMITH, C.M., HUCUL, D.A., BLACKSON, J. & SALAITA, G. (2003). In situ TEM studies of sintering of Pd.alumina catalysts. Microsc Microanal 9(Suppl. 2), 1024CD-1025CD.
57. 3 catalysts. Microsc Microanal 10(Suppl. 2), 488CD-489CD.
58. 7 (x = 0.5-0.6). Microsc Microanal 7(Suppl. 2), 410-411.
59. MCCABE, R.J., MISRA, A. & MITCHELL, T.E. (2002). The use of stereomicroscopy in conjunction with in situ straining TEM for studying dislocation behavior. Microsc Microanal 8(Suppl. 2), 1382CD-1383CD.
60. MEDLIN, D.L. (2001). In situ TEM analysis of facet motion in gold ∑ = 3 {112} boundaries. Microsc Microanal 7(Suppl. 2), 324-325.
61. MEDLIN, D.L. (2002). Morphological evolution and junction dynamics at faceted grain boundaries. Microsc Microanal 8(Suppl. 2), 1400CD-1401CD.
62. MINOR, A.M., LILLEODDEN, E.T., JIN, M., STACH, E.A., CHRZAN, D., MORRIS, J.W., JR., FRIEDMANN, T.A., XIAO, X., AUCIELLO, O.H. & CARLISLE, J.A. (2003). In-situ nanoindentation - A unique probe of deformation response in materials. Microsc Microanal 9(Suppl. 2), 900-901.
63. MINOR, A.M., MORRIS, J.W., JR. & STACH, E.A. (2001a. Quantitative in situ nanoindentation in an electron microscope. Appl Phys Lett 79, 1625-1627.
64. MINOR, A.M., STACH, E.A. & MORRIS, J.W., JR. (2001b). Quantitative in situ nanoindentation of thin films in a transmission electron microscope. Microsc Microanal 7(Suppl. 2), 912-913.
65. NAKAYAMA, T., ARAI, M. & NISHIYAMA, Y. (1983). Formation of pitted particles and redispersion in supported nickel catalysts during heating in oxygen and hydrogen. J Catal 79, 497-500.
66. NAKAYAMA, T., ARAI, M. & NISHIYAMA, Y. (1984). Dispersion of nickel particles supported on alumina and silica in oxygen and hydrogen. J Catal 87, 108-115.
67. NORTON, M.G., BENTLEY, J. & BIGGERS, R.R. (1995). In situ electron microscope observations of structural transformations in single crystal lanthanum aluminate. Microsc Microanal 1(Suppl. 2), 238-239.
68. OH, S.G., RODRIGUEZ, N.M. & BAKER, R.T.K. (1992). In-situ electron microscopy studies of surface segregation in bimetallic catalyst particles. J Catal 136, 584-597.
69. OLESHKO, V.P. & HOWE, J.M. (2004). In situ EFTEM/PEELS investigation of melting behavior of industrial Al-Si alloy small particles. Microsc Microanal 10(Suppl. 2), 350-351.
70. PARKINSON, G.M. (1991). Controlled environment transmission electron microscopy (CETEM) of catalysts. In Proceedings of the Institute of Physics Electron Microscopy and Analysis Group Conference, University of Bristol, UK, Institute of Physics Conference Series No. 119: Section 4. Humphreys, F.J. (Ed.), pp. 151-156. New York: Institute of Physics.
71. PARKINSON, G.M. & WHITE, D. (1986). The application of a controlled atmosphere reaction cell for studying electroactive polymers by TEM. In Proceedings of the XI International Congress on Electron Microscopy, Koyoto, Japan, pp. 331-332.
72. PARSONS, D.F. (1974). Structure of wet specimens in electron microscopy. Science 186, 407-414.
73. PASHLEY, D.W., STOWELL, M.J., JACOBS, M.H. & LAW, T.J. (1964). The growth and structure of gold and silver deposits formed by evaporation inside an electron microscope. Phil Mag 10, 127-158.
74. 2 catalyst. Appl Catal A: General 175, 113-120.
75. POTOCZNA-PETRU, D. & KEPINSKI, L. (1991). Effect of oxidation-reduction treatment on the behavior of model silica supported cobalt catalysts. Catal Lett 9, 355-362.
76. POTOCZNA-PETRU, D. & KRAJCZYK, L. (1995). Microstructure evolution of Co particles supported on carbon induced by oxidation-reduction treatment. J Mater Sci Lett 14, 1294-1297.
77. 2 in oxygen. J Catal 157, 676-686.
78. ROSS, F.M. & SEARSON, P.C. (1995). In situ microscopy of the anodic etching of silicon. Microsc Microanal 1(Suppl. 2), 232-233.
79. ROSS, F.M., WILLIAMSON, M.J., TROMP, R.M., HULL, R. & VEREECKEN, P.M. (2002). In situ transmission electron microscopy of copper electrodeposition. Microsc Microanal 8(Suppl. 2), 420-421.
80. 2 of supported metal crystallites. J Colloid Interface Sci 86, 1-11.
81. RUCKENSTEIN, E. & LEE, S.H. (1984). Redispersion and migration of nickel supported on alumina. J Catal 86, 457-464.
82. SAWYER, L.C. & GRUBB, D.T. (1987). Polymer Microscopy. New York: Chapman and Hall.
83. SHARMA, R. (2003). In situ observations of carbon nanotube formation and growth process. Microsc Microanal 9(Suppl. 2), 302CD-302CD.
84. SHARMA, R. (2004). Understanding the carbon nanotube growth mechanism by in situ microscopy. Microsc Microanal 10(Suppl. 2), 368-369.
85. SHARMA, R. & CROZIER, P.A. (2000). Quantification of CeO reduction by in situ electron energy-loss spectroscopy. Microsc Microanal 6(Suppl. 2), 12-13.
86. SHARMA, R. & CROZIER, P. (2002). In situ determination of local Ce oxidation states during redox reactions. Microsc Microanal 8(Suppl. 2), 600CD-601CD.
87. SHARMA, R. & IQBAL, Z. (2004). In situ observations of carbon nanotube formation using environmental transmission electron microscopy. Appl Phys Lett 84, 990-992.
88. SHARMA, R., MCKELVY, M.J., BEARAT, H., CHIZMESHYA, A.V.G. & CARPENTER, R.W. (2001). In situ observation of nanocrystal formation via dehydroxylation. Microsc Microanal 7(Suppl. 2), 438-439.
89. 2 mineral sequestration process for power plants. Microsc Microanal 8(Suppl. 2), 796CD-797CD.
90. SHEWMON, P.G. (1969). Transformations in Metals. New York: McGraw-Hill Inc.
91. SINCLAIR, R. & KONNO, T.J. (1994). In situ HREM: Application to metal-mediated crystallization. Ultramicroscopy 56, 225-232.
92. SINCLAIR, R. & MIN, K.H. (2002). In situ HREM of crystallization reactions. Microsc Microanal 8(Suppl. 2), 416-417.
93. SINCLAIR, R. & PARKER, M.A. (1986). High-resolution transmission electron microscopy of silicon re-growth at controlled elevated temperatures. Nature 322, 531-533.
94. SMITH, D.A., MEHTA, S.C. & ERB, U. (1995). In situ grain growth in electrodeposited nanocrystalline Ni-1.2wt%P alloy. Microsc Microanal 1(Suppl 2), 250-251.
95. STACH, E.A., DAHMEN, U. & NIX, W.D. (2000a). Real time observations of dislocation mediated plasticity in the epitaxial aluminum (110)/silicon (001) thin film system. Microsc Microanal 6(Suppl. 2), 438-439.
96. STACH, E.A., HULL, R., TROMP, R.M., ROSS, F.M., REUTER, M.C. & BEAM, J.C. (1999). In situ TEM studies of the interaction between dislocations in SiGe heterostructures. Microsc Microanal 5(Suppl. 2), 728-729.
97. STACH, E.A., KISIELOWSKI, C.F., WONG, W.S., SANDS, T. & CHEUNG, N.W. (2000b). Real time observations of nanopipe formation, dislocation motion, and nitrogen desorption in GaN. Microsc Microanal 6(Suppl 2), 1096-1097.
98. STORASKA, G.A. & HOWE, J.M. (2000). In situ TEM investigation of the liquid/solid interface in Al-Si Alloys. Microsc Microanal 6(Suppl. 2), 1068-1069.
99. SUN, H.P., TIAN, W., CHEN, Y.B., YU, J.H., YEADON, M., BOOTHROYD, C.B., LUKASZEW, R.A., CLARK, R. & PAN, X.Q. (2004). Growth and structural evolution of nanosized Ni on (001) MgO by in situ TEM. Microsc Microanal 10(Suppl. 2), 272-273.
100. SUSHMNA, I. & RUCKENSTEIN, E. (1984). Oscillations in crystallite shape during heating in hydrogen of model iron/alumina catalysts. J Catal 90, 241-255.
101. SUSHMNA, I. & RUCKENSTEIN, E. (1985). Role of physical and chemical interactions in the behavior of supported metal catalysts: Iron on alumina - A case study. J Catal 94, 239-288.
102. THOMAS, G. & GORINGE, M.J. (1979). Transmission Electron Microscopy of Materials. New York: John Wiley and Sons.
103. 3 at low temperatures. Phil Mag 33, 639-662.
104. WALL, M.A. & DAHMEN, U. (1997). Development of an in situ nanoindentation specimen holder for the high voltage electron microscope. Microsc Microanal 3(Suppl. 2), 593-594.
105. WANG, L. & YANG, J.C. (2004). Nano-oxidation dynamics of (001) Cu50at%Au thin film by in situ UHV-TEM. Microsc Microanal 10(Suppl. 2), 382CD-383CD.
106. WANG, Z.L., PETROSKI, J.M., GREEN, T.C. & EL-SAYED, M.A. (1998). Shape transformation and surface melting of cubic and tetragonal platinum nanocrystals. J Phys Chem B 102, 6145-6151.
107. YAGI, K., KOBAYASHI, K., TANISHIRO, Y. & TAKAYANAGI, K. (1985). In situ electron microscope of the initial stage of metal growth on metals. Thin Solid Films 126, 95-105.
108. 2O growth on Cu(001) thin films. Appl Phys Lett 70, 3522-3524.
109. YANG, J.C., KOLASA, B., GIBSON, J.M. & YEADON, M. (1998). Self-limiting oxidation of copper. Appl Phys Lett 73, 2841-2843.
110. YANG, J.C., YEADON, M., KOLASA, B. & GIBSON, M. (1999). In situ UHV-TEM oxidation and reduction of metals. Microsc Microanal 5(Suppl. 2), 132-133.
111. YANG, J.C. & ZHOU, G. (2003). Nano-oxide formation by in situ oxidation of copper thin films. Microsc Microanal 9(Suppl. 2), 296CD-297CD.
112. YEADON, M., LIN, M., BOOTHROYD, C.B., ZHENG, H. & LOH, K.P. (2003). In situ growth of BN nanocages. Microsc Microanal 9(Suppl. 2), 914CD-915CD.
113. ZHOU, G.W., BHARADWAJ, M.D. & YANG, J.C. (2001). Initial oxidation kinetics of copper (110) thin films as investigated by in situ UHV-TEM. Microsc Microanal 7(Suppl 2), 1274-1275.
114. ZHOU, G.W. & YANG, J.C. (2002). Initial oxidation kinetics of copper films investigated by in situ UHV-TEM. Microsc Microanal 8(Suppl. 2), 1406CD-1407CD.
115. ZHOU, G.W. & YANG, J.C. (2003a). Surface modifications: Evaporation of oxide islands on metal surfaces investigated by in situ TEM. Microsc Microanal 9(Suppl. 2), 298CD-299CD.
116. 2O oxide morphology created by oxidation of Cu (001) as investigated by in situ TEM. Appl Surf Sci 210, 165-170.
117. 4. Microsc Microanal 1(Suppl. 2), 230-231.