Acta Crystallographica A - Foundations and Advances

Autor: Patricia M. Dove, Alexandria J. Hoeher, Olaf J. Borkiewicz, F. M. Michel, Sebastian T. Mergelsberg
Jazyk: angličtina
Rok vydání: 2019
Předmět:
pair distribution function analysis
Materials science
CALCIUM-PHOSPHATE
crystallization
PAIR DISTRIBUTION FUNCTION
Chemistry
Multidisciplinary
Crystal growth
02 engineering and technology
7. Clean energy
Biochemistry
law.invention
Inorganic Chemistry
03 medical and health sciences
chemistry.chemical_compound
Structural Biology
law
FLOW REACTOR
General Materials Science
CARBONATE
Amorphous calcium phosphate
Physical and Theoretical Chemistry
Crystallization
030304 developmental biology
0303 health sciences
Crystallography
Pair distribution function
in situ X-ray total scattering
021001 nanoscience & nanotechnology
Condensed Matter Physics
Research Papers
Amorphous calcium carbonate
Nanocrystalline material
Amorphous solid
Volumetric flow rate
Chemistry
AREA DETECTOR
Chemical engineering
chemistry
amorphous calcium carbonate
Physical Sciences
0210 nano-technology
CLUSTERS
amorphous calcium phosphate
Zdroj: Acta Crystallographica. Section A, Foundations and Advances
ISSN: 2053-2733
Popis: A novel method is introduced for in situ X-ray total scattering experiments. Two examples of the method as applied to non-classical nucleation and crystal growth studies are discussed.
Structural investigations of amorphous and nanocrystalline phases forming in solution are historically challenging. Few methods are capable of in situ atomic structural analysis and rigorous control of the system. A mixed-flow reactor (MFR) is used for total X-ray scattering experiments to examine the short- and long-range structure of phases in situ with pair distribution function (PDF) analysis. The adaptable experimental setup enables data collection for a range of different system chemistries, initial supersaturations and residence times. The age of the sample during analysis is controlled by adjusting the flow rate. Faster rates allow for younger samples to be examined, but if flow is too fast not enough data are acquired to average out excess signal noise. Slower flow rates form older samples, but at very slow speeds particles settle and block flow, clogging the system. Proper background collection and subtraction is critical for data optimization. Overall, this MFR method is an ideal scheme for analyzing the in situ structures of phases that form during crystal growth in solution. As a proof of concept, high-resolution total X-ray scattering data of amorphous and crystalline calcium phosphates and amorphous calcium carbonate were collected for PDF analysis.
Databáze: OpenAIRE
Externí odkaz: