Reactor design for in situ X-ray scattering studies of nanoparticle formation in supercritical water syntheses

被引:40
作者
Breraholm, Martin [1 ,2 ]
Jensen, Henrik [3 ]
Iversen, Steen Brummerstedt [3 ]
Iversen, Bo Brummerstedt [1 ,2 ]
机构
[1] Aarhus Univ, Dept Chem, DK-8000 Aarhus C, Denmark
[2] Aarhus Univ, Interdisciplinary Nanosci Ctr iNANO, DK-8000 Aarhus C, Denmark
[3] SCF Technol AS, DK-2730 Herlev, Denmark
关键词
Supercritical synthesis; nanoparticles; In situ X-ray scattering; reactor design;
D O I
10.1016/j.supflu.2007.09.029
中图分类号
O64 [物理化学(理论化学)、化学物理学];
学科分类号
070304 ; 081704 ;
摘要
In situ X-ray studies have been widely used in both solid-state chemistry and wet-chemistry to study a variety of reactions and processes, but so far studies of syntheses in the supercritical phase are few and mainly limited to static experiments. Here the design of reactor cells for time-resolved in situ X-ray studies of synthesis in supercritical water is discussed and examples of the information that can be obtained are given for both batch and continuous flow reactors. It is shown that highly useful information on process kinetics can be obtained despite the considerable experimental challenges. (C) 2007 Elsevier B.V. All rights reserved.
引用
收藏
页码:385 / 390
页数:6
相关论文
共 27 条
[1]   Hydrothermal synthesis of metal oxide nanoparticles at supercritical conditions [J].
Adschiri, T ;
Hakuta, Y ;
Sue, K ;
Arai, K .
JOURNAL OF NANOPARTICLE RESEARCH, 2001, 3 (2-3) :227-235
[2]   Hydrothermal synthesis of metal oxide fine particles at supercritical conditions [J].
Adschiri, T ;
Hakuta, Y ;
Arai, K .
INDUSTRIAL & ENGINEERING CHEMISTRY RESEARCH, 2000, 39 (12) :4901-4907
[3]  
[Anonymous], 2004, CRYSTALLIZATION
[4]  
[Anonymous], INT TABLES CRYSTALLO
[5]   Review of supercritical fluids in inorganic materials science [J].
Aymonier, Cyril ;
Loppinet-Serani, Anne ;
Reveron, Helen ;
Garrabos, Yves ;
Cansell, Francois .
JOURNAL OF SUPERCRITICAL FLUIDS, 2006, 38 (02) :242-251
[6]   A combined SAXS/WAXS/XAFS setup capable of observing concurrent changes across the nano-to-micrometer size range in inorganic solid crystallization processes [J].
Beale, Andrew M. ;
van der Eerden, Ad M. J. ;
Jacques, Simon D. M. ;
Leynaud, Olivier ;
O'Brien, Matthew G. ;
Meneau, Florian ;
Nikitenko, Sergei ;
Bras, Wim ;
Weckhuysen, Bert M. .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2006, 128 (38) :12386-12387
[7]  
BECKER J, UNPUB CRITICAL SIZE
[8]   Small-angle scattering in materials science - a short review of applications in alloys, ceramics and composite materials [J].
Fratzl, P .
JOURNAL OF APPLIED CRYSTALLOGRAPHY, 2003, 36 (01) :397-404
[9]   Probing active sites during palladium-catalyzed alcohol oxidation in "supercritical'' carbon dioxide [J].
Grunwaldt, JD ;
Caravati, M ;
Ramin, M ;
Baiker, A .
CATALYSIS LETTERS, 2003, 90 (3-4) :221-229
[10]   Supercritical propanol-water synthesis and comprehensive size characterisation of highly crystalline anatase TiO2 nanoparticles [J].
Hald, Peter ;
Becker, Jacob ;
Bremholm, Martin ;
Pedersen, Jan S. ;
Chevallier, Jacques ;
Iversen, Steen B. ;
Iversen, Bo B. .
JOURNAL OF SOLID STATE CHEMISTRY, 2006, 179 (08) :2674-2680