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Determination of Crystal Structures01:29

Determination of Crystal Structures

In the late 1800s, the revelation that light extended beyond visible wavelengths led to the discovery of X-rays by Wilhelm Roentgen. Recognized as high-energy electromagnetic radiation with short wavelengths, X-rays prompted exploration into their interaction with crystals. Max von Laue proposed in 1912 that the periodic arrangement of atoms, ions, or molecules in crystals would cause them to diffract X-rays, a hypothesis confirmed through experiments with copper sulfate and zinc sulfide...

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Crystallization of Proteins on Chip by Microdialysis for In Situ X-ray Diffraction Studies
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In situ system for X-ray absorption spectroscopy experiments to investigate nanoparticle crystallization.

C T Meneses1, W H Flores, A P Sotero

  • 1Departamento de Física, Universidade Federal do Ceará, Campus do Pici, CP 6030, 60455-760 Fortaleza, CE, Brazil. cristiano@fisica.ufc.br

Journal of Synchrotron Radiation
|October 24, 2006
PubMed
Summary

A novel furnace enables in situ X-ray absorption spectroscopy for studying nanoparticle formation during thermal treatments. This system successfully monitored the crystallization of nickel oxide (NiO) nanoparticles synthesized via the sol-gel method.

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Microfluidic Chips for In Situ Crystal X-ray Diffraction and In Situ Dynamic Light Scattering for Serial Crystallography

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Area of Science:

  • Materials Science
  • Nanotechnology
  • Spectroscopy

Background:

  • In situ studies are crucial for understanding dynamic processes during material synthesis.
  • X-ray absorption spectroscopy (XAS) provides element-specific electronic and structural information.
  • Controlled thermal treatment is key for nanoparticle crystallization.

Purpose of the Study:

  • To design and construct a new halogen lamp-based furnace for in situ XAS experiments.
  • To demonstrate the furnace's capability in studying nanoparticle formation under controlled thermal conditions.
  • To showcase the furnace performance in dispersive mode using nickel oxide (NiO) nanoparticle synthesis.

Main Methods:

  • Development of a specialized furnace and sample cell for in situ XAS.
  • Utilizing sol-gel (gelatin) method for NiO nanoparticle synthesis.
  • Performing in situ Ni K-edge X-ray absorption near-edge structure (XANES) measurements during heating.

Main Results:

  • The designed furnace and sample cell effectively supported in situ XAS experiments in both conventional and dispersive modes.
  • Successful synthesis of NiO nanoparticles was achieved using the sol-gel method.
  • In situ Ni K-edge XANES measurements revealed the evolution of the Ni environment during heating, confirming complete NiO nanoparticle crystallization.

Conclusions:

  • The new furnace is a valuable tool for in situ thermal treatment studies of materials.
  • The apparatus allows for real-time monitoring of dynamic structural changes during nanoparticle formation.
  • The demonstrated application highlights the furnace's effectiveness in dispersive mode XAS experiments.