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Calcination of ZSM-5. An in situ synchrotron powder diffraction study.
Materials Science Forum (2004), 443-444, (EPDIC 8), 319-322. Publisher: (Trans Tech Publications Ltd., ) CODEN:MSFOEP ISSN:0255-5476.
Bibliographic Information

Calcination of ZSM-5. An in situ synchrotron powder diffraction study.     Stahl, Kenny; Gustavsson, Ester; Jacobsen, Claus J. H.; Schmidt, Iver.    Department of Chemistry,  Technical University of Denmark,  Lyngby,  Den.    Materials Science Forum  (2004),  443-444(EPDIC 8),  319-322.  Publisher: Trans Tech Publications Ltd.,  CODEN: MSFOEP  ISSN: 0255-5476.  Journal  written in English.    CAN 141:286051    AN 2004:163481    CAPLUS  

Abstract

The calcination of the zeolite ZSM-5 was studied by in situ x-ray synchrotron powder diffraction.  Two samples were studied: one conventionally synthesized (CONV) and one synthesized in a charcoal matrix according to the confined space synthesis method (CSS).  The powder diffraction data were collected between 375-975 K in steps of 8 K/5 min. and evaluated by Rietveld refinements.  Both sets of powder diffraction patterns displayed the characteristic intensity changes for calcination, but neither of them showed the expected orthorhombic to monoclinic phase transition.  Refinements of the extra-framework occupancy showed that the calcination starts at 475 K and is essentially completed at 675 K for CSS, while the CONV calcination starts at 525 K and ends at 650 K.  The refinement results agree very well with the TGA results.  The C matrix of the CSS sample is combusted between 700-850 K.  The unit cell dimensions continuously decrease from 475-975 K.  An initial slow 1.2% redn. between 375-875 K is followed by a fast 1.2% redn. between 875-950 K for the CSS sample.  This 2nd unit cell redn. step is unrelated to the calcination process and does not involve any wt. loss.  It is suggested that this step is a recrystn./annealing process reducing the amt. of defects and strain.  

Indexing -- Section 75-1  (Crystallography and Liquid Crystals)   

Calcination  
Recrystallization  
    (calcination of ZSM-5 studied in situ by synchrotron powder diffractometry)  

Zeolite ZSM-5  
Role: PEP (Physical, engineering or chemical process); PRP (Properties); PYP (Physical process); PROC (Process)  
    (calcination of ZSM-5 studied in situ by synchrotron powder diffractometry)  

Combustion  
    (calcination of ZSM-5 with combustion of its C matrix)   

7440-44-0, Carbon, processes  
Role: CPS (Chemical process); PEP (Physical, engineering or chemical process); PROC (Process)  
    (calcination of ZSM-5 with combustion of its C matrix)  

Supplementary Terms

zeolite ZSM 5 calcination recrystn  

Citations

1) Madsen, C; Chem Commun 1999, 673
2) Jacobsen, C; J Am Chem Soc 2000, 122, 7116
3) Cerenius, Y; J Synchr Rad 2000, 7, 203
4) Stahl, K; J Appl Crystallogr 2000, 33, 394
5) Koningsveld, H; Acta Crystallogr B 1987, 43, 127
6) Koningsveld, H; Zeolites 1990, 10, 235
3Â¥2011-07-22 15:46:42
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wenhui15

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Originally posted by duyuhai at 2011-07-22 15:46:42:
Calcination of ZSM-5. An in situ synchrotron powder diffraction study.
Materials Science Forum (2004), 443-444, (EPDIC 8), 319-322. Publisher: (Trans Tech Publications Ltd., ) CODEN:MSFOEP ISSN:02 ...

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