A new method for in situ structural investigations of nano-sized amorphous and crystalline materials using mixed-flow reactors

Hoeher, Alexandria; Mergelsberg, Sebastian; Borkiewicz, Olaf J.; Dove, Patricia M.; Michel, F. Marc

doi:10.1107/S2053273319008623

Title: A new method for in situ structural investigations of nano-sized amorphous and crystalline materials using mixed-flow reactors

Journal Article · Fri Aug 23 00:00:00 EDT 2019 · Acta Crystallographica. Section A, Foundations and Advances (Online)

DOI:https://doi.org/10.1107/S2053273319008623· OSTI ID:1617945

; Mergelsberg, Sebastian; Borkiewicz, Olaf J.; Dove, Patricia M.; Michel, F. Marc

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.

View Journal Article

Cite

Export

Save

Research Organization:: Argonne National Laboratory (ANL), Argonne, IL (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: BES-FG02-00ER15112; AC02-06CH11357

OSTI ID:: 1617945

Alternate ID(s):: OSTI ID: 1575251

Journal Information:: Acta Crystallographica. Section A, Foundations and Advances (Online), Journal Name: Acta Crystallographica. Section A, Foundations and Advances (Online) Vol. 75 Journal Issue: 5; ISSN 2053-2733

Publisher:: International Union of Crystallography (IUCr)Copyright Statement

Country of Publication:: Denmark

Language:: English

Citation Metrics:

Cited by: 20 works

Citation information provided by
Web of Science

References (31)

Area detector corrections for high quality synchrotron X-ray structure factor measurements Skinner, Lawrie B.; Benmore, Chris J.; Parise, John B. Nuclear Instruments and Methods in Physics Research Section A: Accelerators, Spectrometers, Detectors and Associated Equipment, Vol. 662, Issue 1 https://doi.org/10.1016/j.nima.2011.09.031	journal	January 2012
Structure of Clusters and Formation of Amorphous Calcium Phosphate and Hydroxyapatite: From the Perspective of Coordination Chemistry Du, Lin-Wei; Bian, Sha; Gou, Bao-Di Crystal Growth & Design, Vol. 13, Issue 7 https://doi.org/10.1021/cg400498j	journal	May 2013
Characterization of Structure in Biogenic Amorphous Calcium Carbonate: Pair Distribution Function and Nuclear Magnetic Resonance Studies of Lobster Gastrolith Reeder, Richard J.; Tang, Yuanzhi; Schmidt, Millicent P. Crystal Growth & Design, Vol. 13, Issue 5 https://doi.org/10.1021/cg301653s	journal	April 2013
Crystallographic properties of the calcium phosphate mineral, brushite, by means of First Principles calculations Sainz-Díaz, C. Ignacio; Villacampa, Ana; Otálora, Fermín American Mineralogist, Vol. 89, Issue 2-3 https://doi.org/10.2138/am-2004-2-308	journal	February 2004
Synthetic amorphous calcium phosphate and its relation to bone mineral structure Posner, Aaron S.; Betts, Foster Accounts of Chemical Research, Vol. 8, Issue 8 https://doi.org/10.1021/ar50092a003	journal	August 1975
Crystallization by particle attachment in synthetic, biogenic, and geologic environments De Yoreo, J. J.; Gilbert, P. U. P. A.; Sommerdijk, N. A. J. M. Science, Vol. 349, Issue 6247 https://doi.org/10.1126/science.aaa6760	journal	July 2015
PDFgetX3 : a rapid and highly automatable program for processing powder diffraction data into total scattering pair distribution functions Juhás, P.; Davis, T.; Farrow, C. L. Journal of Applied Crystallography, Vol. 46, Issue 2 https://doi.org/10.1107/S0021889813005190	journal	March 2013
Antimonate and arsenate speciation on reactive soil minerals studied by differential pair distribution function analysis van Genuchten, Case M.; Peña, Jasquelin Chemical Geology, Vol. 429 https://doi.org/10.1016/j.chemgeo.2016.03.001	journal	July 2016
A thermodynamic analysis of the amorphous to crystalline calcium phosphate transformation Meyer, J. L.; Eanes, E. D. Calcified Tissue Research, Vol. 25, Issue 1 https://doi.org/10.1007/BF02010752	journal	December 1978
Investigation of Surface Structures by Powder Diffraction: A Differential Pair Distribution Function Study on Arsenate Sorption on Ferrihydrite Harrington, Richard; Hausner, Douglas B.; Bhandari, Narayan Inorganic Chemistry, Vol. 49, Issue 1 https://doi.org/10.1021/ic9022695	journal	January 2010
Structural analysis of complex materials using the atomic pair distribution function — a practical guide Proffen, Th.; Billinge, S. J. L.; Egami, T. Zeitschrift für Kristallographie - Crystalline Materials, Vol. 218, Issue 2 https://doi.org/10.1524/zkri.218.2.132.20664	journal	January 2003
Prenucleation clusters and non-classical nucleation Gebauer, Denis; Cölfen, Helmut Nano Today, Vol. 6, Issue 6 https://doi.org/10.1016/j.nantod.2011.10.005	journal	December 2011
Atomic pair distribution function analysis of materials containing crystalline and amorphous phases Proffen, Thomas; Page, Katharine L.; McLain, Sylvia E. Zeitschrift für Kristallographie, Vol. 220, Issue 12/2005 https://doi.org/10.1524/zkri.2005.220.12_2005.1002	journal	January 2005
PDFfit2 and PDFgui: computer programs for studying nanostructure in crystals Farrow, C. L.; Juhas, P.; Liu, J. W. Journal of Physics: Condensed Matter, Vol. 19, Issue 33 https://doi.org/10.1088/0953-8984/19/33/335219	journal	July 2007
Nanoporous Structure and Medium-Range Order in Synthetic Amorphous Calcium Carbonate Goodwin, Andrew L.; Michel, F. Marc; Phillips, Brian L. Chemistry of Materials, Vol. 22, Issue 10 https://doi.org/10.1021/cm100294d	journal	May 2010
Structural Changes upon Dehydration of Amorphous Calcium Carbonate Schmidt, Millicent P.; Ilott, Andrew J.; Phillips, Brian L. Crystal Growth & Design, Vol. 14, Issue 3 https://doi.org/10.1021/cg401073n	journal	January 2014
Structure of Sulfate Adsorption Complexes on Ferrihydrite Zhu, Mengqiang; Northrup, Paul; Shi, Chenyang Environmental Science & Technology Letters, Vol. 1, Issue 1 https://doi.org/10.1021/ez400052r	journal	October 2013
Extracting differential pair distribution functions using MIXSCAT Wurden, Caroline; Page, Katharine; Llobet, Anna Journal of Applied Crystallography, Vol. 43, Issue 3 https://doi.org/10.1107/S0021889810009155	journal	April 2010
Time-resolved in situ studies of apatite formation in aqueous solutions Borkiewicz, O.; Rakovan, J.; Cahill, C. L. American Mineralogist, Vol. 95, Issue 8-9 https://doi.org/10.2138/am.2010.3168	journal	August 2010
Specific Characteristics of Wet Nanocrystalline Apatites. Consequences on Biomaterials and Bone Tissue Eichert, Diane; Sfihi, Hocine; Combes, Christèle Key Engineering Materials, Vol. 254-256 https://doi.org/10.4028/www.scientific.net/KEM.254-256.927	journal	December 2003
Atomic structure of intracellular amorphous calcium phosphate deposits. Betts, F.; Blumenthal, N. C.; Posner, A. S. Proceedings of the National Academy of Sciences, Vol. 72, Issue 6 https://doi.org/10.1073/pnas.72.6.2088	journal	June 1975
PDFgetX2: a GUI-driven program to obtain the pair distribution function from X-ray powder diffraction data Qiu, Xiangyun; Thompson, Jeroen W.; Billinge, Simon J. L. Journal of Applied Crystallography, Vol. 37, Issue 4, p. 678-678 https://doi.org/10.1107/S0021889804011744	journal	July 2004
In Situ Detection of Calcium Phosphate Clusters in Solution and Wet Amorphous Phase by Synchrotron X-ray Absorption Near-Edge Spectroscopy at Calcium K-Edge Zhang, Qun; Jiang, Yun; Gou, Bao-Di Crystal Growth & Design, Vol. 15, Issue 5 https://doi.org/10.1021/cg5018505	journal	March 2015
Chemical and physical controls on the transformation of amorphous calcium carbonate into crystalline CaCO3 polymorphs Blue, C. R.; Giuffre, A.; Mergelsberg, S. Geochimica et Cosmochimica Acta, Vol. 196 https://doi.org/10.1016/j.gca.2016.09.004	journal	January 2017
Structural Characteristics of Synthetic Amorphous Calcium Carbonate Michel, F. Marc; MacDonald, Jason; Feng, Jian Chemistry of Materials, Vol. 20, Issue 14 https://doi.org/10.1021/cm800324v	journal	July 2008
Biological calcium phosphates and Posner’s cluster Yin, Xilin; Stott, Malcolm J. The Journal of Chemical Physics, Vol. 118, Issue 8 https://doi.org/10.1063/1.1539093	journal	February 2003
Applications of an amorphous silicon-based area detector for high-resolution, high-sensitivity and fast time-resolved pair distribution function measurements Chupas, Peter J.; Chapman, Karena W.; Lee, Peter L. Journal of Applied Crystallography, Vol. 40, Issue 3 https://doi.org/10.1107/S0021889807007856	journal	May 2007
Ion-association complexes unite classical and non-classical theories for the biomimetic nucleation of calcium phosphate Habraken, Wouter J. E. M.; Tao, Jinhui; Brylka, Laura J. Nature Communications, Vol. 4, Issue 1 https://doi.org/10.1038/ncomms2490	journal	February 2013
Approach to Steady State in Completely Mixed Flow Reactors Jensen, James N. Journal of Environmental Engineering, Vol. 127, Issue 1 https://doi.org/10.1061/(ASCE)0733-9372(2001)127:1(13)	journal	January 2001
Two-dimensional detector software: From real detector to idealised image or two-theta scan Hammersley, A. P.; Svensson, S. O.; Hanfland, M. High Pressure Research, Vol. 14, Issue 4-6, p. 235-248 https://doi.org/10.1080/08957959608201408	journal	January 1996
3D printed mixed flow reactor for geochemical rate measurements Michel, F. Marc; Rimstidt, J. Donald; Kletetschka, Karel Applied Geochemistry, Vol. 89 https://doi.org/10.1016/j.apgeochem.2017.11.008	journal	February 2018

Similar Records

Composition Systematics in the Exoskeleton of the American Lobster, Homarus americanus and Implications for Malacostraca

Journal Article · Fri Apr 05 00:00:00 EDT 2019 · Frontiers in Earth Science · OSTI ID:1617945

Mergelsberg, Sebastian T.; Ulrich, Robert N.; Xiao, Shuhai; +1 more

Final Scientific/Technical Report

Technical Report · Wed Oct 18 00:00:00 EDT 2017 · OSTI ID:1617945

Reeder, Richard; Phillips, Brian

Application of high-energy x-rays and pair-distribution-function analysis to nano-scale structural studies in catalysis.

Journal Article · Thu Jul 30 00:00:00 EDT 2009 · Catal.Today · OSTI ID:1617945

Chupas, P J; Chapman, K W; Chen, H; +1 more

Related Subjects

36 MATERIALS SCIENCE
in situ X-ray total scattering
crystallization
amorphous calcium phosphate
amorphous calcium carbonate
pair distribution function analysis

Title: A new method for in situ structural investigations of nano-sized amorphous and crystalline materials using mixed-flow reactors

Citation Formats

References (31)

Similar Records

Related Subjects