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Cryogenic-scanning electron microscopy as a technique to image sol-to-gel transformation in chelated alkoxide systems

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Title Cryogenic-scanning electron microscopy as a technique to image sol-to-gel transformation in chelated alkoxide systems
 
Creator HARIDAS, MM
MENON, A
GOYAL, N
CHANDRAN, S
BELLARE, JR
 
Subject aluminum alkoxides
chemistry
 
Description Direct imaging of wet sol-to-gel microstructures in chelated alkoxide systems is reported for the first time by using fast-freeze and freeze-fracture techniques for sample fixing. The system chosen for microstructural imaging is that of a chelated alkoxide, in an effort to observe sol-to-gel transformation. The batch composition corresponds to a 1:1 molar ratio of aluminum sec-butoxide and ethyl acetoacetate made using isopropyl alcohol as a mutual solvent. About 100 mu l of samples in varying stages of sonogelation, at a water addition rate of 0.4 ml per hour per gram of alkoxide, were injected between two 300-mesh TEM grids mounted on 0.1 mm copper plates and plunged into melting Freon to bring about a rapid solidification. The sample was cryo-transferred into an SEM, equipped with a cold stage maintained at -170 degrees C, using liquid N-2. The specimen was fractured and imaged for microstructural detail under the electron beam. The direct imaging techniques developed here have been applied to chelated alkoxides for the first time, showing the morphology and microstructure in unhydrolysed as well as fully hydrolysed sols, which were found to indicate complex shapes that were not previously known to exist in such systems. Thus, more microstructural information could be directly gained as a result of this cryo-SEM technique.
 
Publisher ELSEVIER SCI LTD
 
Date 2011-07-21T22:57:16Z
2011-12-26T12:52:12Z
2011-12-27T05:39:15Z
2011-07-21T22:57:16Z
2011-12-26T12:52:12Z
2011-12-27T05:39:15Z
1996
 
Type Article
 
Identifier CERAMICS INTERNATIONAL, 22(2), 155-159
0272-8842
http://dx.doi.org/10.1016/0272-8842(95)00073-9
http://dspace.library.iitb.ac.in/xmlui/handle/10054/6024
http://hdl.handle.net/10054/6024
 
Language en