In situ nanoscale visualization of solvent effects on molecular crystal surfaces

CrystEngComm ◽  
2021 ◽  
Author(s):  
Mikkel Herzberg ◽  
Anders Støttrup Larsen ◽  
Tue Hassenkam ◽  
Anders Østergaard Madsen ◽  
Jukka Rantanen
Keyword(s):  
Solid Solution ◽  
Solvent Effects ◽  
Molecular Crystal ◽  
Rational Design ◽  
Molecular Level ◽  
Molecular Crystals ◽  
Crystal Surfaces ◽  
Solution Interface ◽  
Atomic Force

Solvents can dramatically affect molecular crystals. Obtaining favorable properties for these crystals requires rational design based on molecular level understanding of the solid-solution interface. Here we show how atomic force...

Use of In Situ Atomic Force Microscopy to Follow Phase Changes at Crystal Surfaces in Real Time

2013 ◽  
Vol 52 (40) ◽  
pp. 10541-10544 ◽  
Author(s):  
Ranjit Thakuria ◽  
Mark D. Eddleston ◽  
Ernest H. H. Chow ◽  
Gareth O. Lloyd ◽  
Barry J. Aldous ◽  
...  
Keyword(s):  
Atomic Force Microscopy ◽  
Real Time ◽  
Phase Changes ◽  
Crystal Surfaces ◽  
Force Microscopy ◽  
Atomic Force

scholarly journals In situ imaging of two-dimensional surface growth reveals the prevalence and role of defects in zeolite crystallization

2020 ◽  
Vol 117 (46) ◽  
pp. 28632-28639
Author(s):  
Madhuresh K. Choudhary ◽  
Rishabh Jain ◽  
Jeffrey D. Rimer
Keyword(s):  
Silica Nanoparticles ◽  
Rational Design ◽  
Surface Defects ◽  
Surface Growth ◽  
Two Dimensional ◽  
Crystal Surfaces ◽  
Structure Directing Agent ◽  
Layered Growth

Zeolite crystallization predominantly occurs by nonclassical pathways involving the attachment of complex (alumino)silicate precursors to crystal surfaces, yet recurrent images of fully crystalline materials with layered surfaces are evidence of classical growth by molecule attachment. Here we use in situ atomic force microscopy to monitor three distinct mechanisms of two-dimensional (2D) growth of zeolite A where we show that layer nucleation from surface defects is the most common pathway. Direct observation of defects was made possible by the identification of conditions promoting layered growth, which correlates to the use of sodium as an inorganic structure-directing agent, whereas its replacement with an organic results in a nonclassical mode of growth that obscures 2D layers and markedly slows the rate of crystallization. In situ measurements of layered growth reveal that undissolved silica nanoparticles in the synthesis medium can incorporate into advancing steps on crystal surfaces to generate defects (i.e., amorphous silica occlusions) that largely go undetected in literature. Nanoparticle occlusion in natural and synthetic crystals is a topic of wide-ranging interest owing to its relevance in fields spanning from biomineralization to the rational design of functional nanocomposites. In this study, we provide unprecedented insight into zeolite surface growth by molecule addition through time-resolved microscopy that directly captures the occlusion of silica nanoparticles and highlights the prevalent role of defects in zeolite crystallization.

scholarly journals Infrared spectroscopy of bare single crystal and nano-particle covered surfaces

2006 ◽  
Vol 71 (8-9) ◽  
pp. 945-948 ◽  
Author(s):  
Nebojsa Marinkovic ◽  
Radoslav Adzic
Keyword(s):  
Single Crystal ◽  
Noble Metals ◽  
Nano Particle ◽  
Oxidation Of Co ◽  
Crystal Surfaces ◽  
Adsorbed Species ◽  
Single Crystal Surfaces ◽  
Solution Interface ◽  
In Situ Investigation

Infrared spectroelectrochemistry is the leading technique for in situ investigation of electrode - solution interfaces because it can both identify the species adsorbed at the metal/solution interface, and quantitatively follow their reaction and kinetic behavior. The unique capabilities of the method have been demonstrated by selective examples, including the identification of preferentially adsorbed species on single crystal surfaces of noble metals with hexagonal symmetry, and electrochemical oxidation of CO on bare and Pt-decorated single crystal Ru surfaces.

Use of In Situ Atomic Force Microscopy to Follow Phase Changes at Crystal Surfaces in Real Time

2013 ◽  
Vol 125 (40) ◽  
pp. 10735-10738 ◽  
Author(s):  
Ranjit Thakuria ◽  
Mark D. Eddleston ◽  
Ernest H. H. Chow ◽  
Gareth O. Lloyd ◽  
Barry J. Aldous ◽  
...  
Keyword(s):  
Atomic Force Microscopy ◽  
Real Time ◽  
Phase Changes ◽  
Crystal Surfaces ◽  
Force Microscopy ◽  
Atomic Force

In-situ X-ray Studies of Clean Catalytic Technologies

2011 ◽  
Vol 1351 ◽  
Author(s):  
Adam F. Lee ◽  
Christine V. Ellis ◽  
Mark A. Newton ◽  
Christopher M. Parlett ◽  
Karen Wilson
Keyword(s):  
Rational Design ◽  
Heterogeneous Catalysts ◽  
Molecular Level ◽  
Aerobic Oxidation ◽  
Allylic Alcohols ◽  
Time Resolved ◽  
X Ray ◽  
Adsorbed Layers ◽  
Insight Into

ABSTRACTThe rational design of new heterogeneous catalysts for clean chemical technologies can be accelerated by molecular level insight into surface chemical processes. In-situ methodologies, able to provide time-resolved and/or pressure dependent information on the evolution of reacting adsorbed layers over catalytically relevant surfaces, are therefore of especial interest. Here we discuss the application of in-situ XPS and in-situ, synchronous DRIFTS/MS/XAS methodologies to elucidate the active site in Pd-catalyzed, selective aerobic oxidation of allylic alcohols.

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