In situ system for X-ray absorption spectroscopy experiments to investigate nanoparticle crystallization.
A new furnace, based on a halogen lamp, and a sample cell have been designed and constructed for in situ X-ray absorption spectroscopy experiments in conventional and dispersive mode (transmission and fluorescence geometries). The main application of the apparatus is thermal treatment studies under controlled conditions for dynamical processes. The sol-gel (gelatin) method has been utilized to synthesize NiO nanoparticles. During this heating process, in situ Ni K-edge X-ray absorption near-edge structural measurements provided evidence of the evolution of a Ni environment until complete NiO nanoparticle crystallization. This case is reported in order to show the furnace performance in dispersive mode.
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Departamento de Física, Universidade Federal do Ceará, Campus do Pici, CP 6030, 60455-760 Fortaleza, CE, Brazil. cristiano@fisica.ufc.br
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Sotero
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Tamura
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Garcia
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Sasaki
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D003460:Crystallization / Q000379:methods*; D018360:Crystallography, X-Ray / Q000295:instrumentation* / Q000379:methods; D004867:Equipment Design; D019544:Equipment Failure Analysis; D008422:Materials Testing / Q000379:methods; D053758:Nanoparticles / Q000737:chemistry* / Q000648:ultrastructure*; D013052:Spectrometry, X-Ray Emission / Q000295:instrumentation* / Q000379:methods