Profound Effect of the Milling Assembly on Polymorphism in Mechanochemical Cocrystallization

10.26434/chemrxiv.11829414 ◽

2020 ◽

Author(s):

Luzia S. Germann ◽

Mihails Arhangelskis ◽

Robin Stein ◽

Martin Etter ◽

Robert E. Dinnebier ◽

...

Keyword(s):

Real Time ◽

Adipic Acid ◽

Direct Impact ◽

X Ray Diffraction ◽

Organic Solids ◽

X Ray ◽

Related Form ◽

Highly Efficient

Mechanochemistry provides a highly efficient, but still poorly understood route to synthesize and screen for polymorphs of organic solids. We present a hitherto unexplored approach to control the mechanism and outcome of mechanochemical cocrystallization through changes to the milling assembly, <i>i.e. </i>milling jar and balls. Whereas polymorph control of mechanochemical cocrystallization is typically discussed in terms of liquid additives, real-time synchrotron X-ray diffraction studies reveal a direct impact of the choice of milling media on the rate of formation and interconversion of cocrystal polymorphs. This effect enabled the discovery of a new polymorph of a cocrystal of nicotinamide and adipic acid, whose formation and conversion to the previously known, enantiotropically-related form, was readily controlled by milling in jars made of different materials.

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Real-time X-ray diffraction using synchrotron radiation: System characterization and applications

Nuclear Instruments and Methods in Physics Research ◽

10.1016/0167-5087(83)91173-0 ◽

1983 ◽

Vol 208 (1-3) ◽

pp. 495-510 ◽

Cited By ~ 35

Author(s):

Martin Caffrey ◽

Donald H. Bilderback

Keyword(s):

Synchrotron Radiation ◽

Real Time ◽

X Ray Diffraction ◽

X Ray ◽

System Characterization

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Real-Time Composition And Thickness Control Techniques In A Metalorganic Chemical Vapor Deposition Process

MRS Proceedings ◽

10.1557/proc-406-133 ◽

1995 ◽

Vol 406 ◽

Author(s):

M. S. Gaffneyt ◽

C. M. Reavesl ◽

A. L Holmes ◽

R. S. Smith ◽

S. P. DenBaars

Keyword(s):

Chemical Vapor Deposition ◽

Real Time ◽

Vapor Deposition ◽

Metalorganic Chemical Vapor Deposition ◽

Chemical Vapor ◽

Normal Operation ◽

Growth Monitoring ◽

X Ray Diffraction ◽

X Ray ◽

Metalorganic Chemical

AbstractMetalorganic chemical vapor deposition (MOCVD) is a process used to manufacture electronic and optoelectronic devices that has traditionally lacked real-time growth monitoring and control. We have developed control strategies that incorporate monitors as real-time control sensors to improve MOCVD growth. An analog control system with an ultrasonic concentration monitor was used to reject bubbler concentration disturbances which exist under normal operation, during the growth of a four-period GaInAs/InP superlattice. Using X-ray diffraction, it was determined that the normally occurring concentration variations led to a wider GaInAs peak in the uncompensated growths as compared to the compensated growths, indicating that closed loop control improved GaInAs composition regulation. In further analysis of the X-ray diffraction curves, superlattice peaks were used as a measure of high crystalline quality. The compensated curve clearly displayed eight orders of satellite peaks, whereas the uncompensated curve shows little evidence of satellite peaks.

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A Characterization of the Phase Transitions in Saturated Monogalactosyldiacylglycerol-Water Systems Using Real-Time X-Ray Diffraction Methods

Molecular Crystals and Liquid Crystals Incorporating Nonlinear Optics ◽

10.1080/00268948908037167 ◽

1989 ◽

Vol 167 (1) ◽

pp. 109-121

Author(s):

P. J. Quinn ◽

L. J. Lis

Keyword(s):

Phase Transitions ◽

Real Time ◽

Water Systems ◽

X Ray Diffraction ◽

X Ray

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Real‐time wide‐angle X‐ray diffraction during polyethylene blown film extrusion

Polymer Engineering & Science ◽

10.1002/pen.21111 ◽

2008 ◽

Vol 48 (8) ◽

pp. 1487-1494 ◽

Cited By ~ 13

Author(s):

Giri Gururajan ◽

H. Shan ◽

G. Lickfield ◽

A.A. Ogale

Keyword(s):

Real Time ◽

Wide Angle ◽

X Ray Diffraction ◽

X Ray ◽

Film Extrusion ◽

Blown Film ◽

Blown Film Extrusion

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Dynamics of the nanocrystal structure and composition in growth solutions monitored by in situ lab-scale X-ray diffraction

Nanoscale ◽

10.1039/d1nr05371j ◽

2021 ◽

Author(s):

Helena Fridman ◽

Michael Volokh ◽

Taleb Mokari

Keyword(s):

Real Time ◽

Growth Dynamics ◽

X Ray Diffraction ◽

X Ray ◽

Nanocrystal Growth ◽

Novel Approach ◽

Phase Size ◽

Time Observation ◽

Real Time Observation

Nanocrystal growth dynamics are investigated by a novel approach: real-time observation of nanocrystals in growth solutions using lab-scale in situ X-ray diffraction. The method reveals the evolution of crystal phase, size, shape, and composition.

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Non-Isothermal Crystallization Behavior of PEEK/Graphene Nanoplatelets Composites from Melt and Glass States

Polymers ◽

10.3390/polym11010124 ◽

2019 ◽

Vol 11 (1) ◽

pp. 124 ◽

Cited By ~ 6

Author(s):

Ángel Alvaredo ◽

María Martín ◽

Pere Castell ◽

Roberto Guzmán de Villoria ◽

Juan Fernández-Blázquez

Keyword(s):

Real Time ◽

Orthorhombic Phase ◽

Complex Viscosity ◽

Crystallization Time ◽

X Ray Diffraction ◽

Scanning Calorimetry ◽

X Ray ◽

Chain Mobility ◽

Peek Composite ◽

Poly Ether Ether Ketone

The effect of the graphene nanoplateletets (GNP), at concentration of 1, 5 and 10 wt %, in Poly ether ether ketone (PEEK) composite crystallization from melt and during cold crystallization were investigated by differential scanning calorimetry (DSC) and real time X-ray diffraction experiments. DSC results revealed a double effect of GNP: (a) nucleating effect crystallization from melt started at higher temperatures and (b) longer global crystallization time due to the restriction in the polymer chain mobility. This hindered mobility were proved by rheological behavior of nanocomposites, because to the increase of complex viscosity, G′, G″ with the GNP content, as well as the non-Newtonian behavior found in composites with high GNP content. Finally, real time wide and small angle synchrotron X-ray radiation (WAXS/SAXS) X-ray measurements showed that GNP has not affected the orthorhombic phase of PEEK nor the evolution of the crystal phase during the crystallization processes. However, the correlation length of the crystal obtained by WAXS and the long period (L) by SAXS varied depending on the GNP content.

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