Crystal Growth Cell Incorporating Automated Image Analysis Enabling Measurement of Facet Specific Crystal Growth Rates

Offiler, Caroline A.; Cruz‐Cabeza, Aurora J.; Davey, Roger J.; Vetter, Thomas

doi:10.1021/acs.cgd.1c01019

Cited by 9 publications

(15 citation statements)

References 65 publications

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“…Growth rate experiments on BZM-I in both pure solutions and in the presence of additives were carried out in a growth cell under flow conditions (flow cell, FC). The FC setup and image analysis algorithms used in data extraction have been described in detail elsewhere . Briefly, at its core sits a small quartz flow cell through which solution at a controlled concentration can flow.…”

Section: Methodsmentioning

confidence: 89%

“…The FC setup and image analysis algorithms used in data extraction have been described in detail elsewhere. 11 Briefly, at its core sits a small quartz flow cell through which solution at a controlled concentration can flow. The cell is immersed in a water bath set to 15 ± 0.01 °C.…”

Section: Slow Cooling Crystallizationsmentioning

confidence: 99%

“…In this context, the present work seeks to utilize crystal growth rate data along with morphological observations to understand further the growth behavior of the historically important BZM-I system. Here, our newly developed automated method was used to study the facet-specific growth rates 11 of BZM-I pure as well as in the presence of the additives shown in Figure 1. The technique combines a crystal growth flow cell with image processing allowing for efficient retrieval of facet-specific growth rates.…”

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Complex Growth of Benzamide Form I: Effect of Additives, Solution Flow, and Surface Rugosity

Offiler

Fonte

Kras

et al. 2022

Crystal Growth & Design

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Understanding crystal growth kinetics is of great importance for the development and manufacturing of crystalline molecular materials. In this work, the impact of additives on the growth kinetics of benzamide form I (BZM-I) crystals has been studied. Using our newly developed crystal growth setup for the measurement of facetspecific crystal growth rates under flow, BZM-I growth rates were measured in the presence of various additives previously reported to induce morphological changes. The additives did not have a significant impact on the growth rates of BZM-I at low concentrations. By comparison to other systems, these additives could not be described as "effective" since BZM-I showed a high tolerance of the additives' presence during growth, which may be a consequence of the type of growth mechanisms at play. Growth of pure BZM-I was found to be extremely defected, and perhaps those defects allow the accommodation of impurities. An alternative explanation is that at low additive concentrations, solid solutions are formed, which was indeed confirmed for a few of the additives. Additionally, the growth of BZM-I was found to be significantly affected by solution dynamics. Changes in some facet growth rates were observed with changes in the orientation of the BZM-I single crystals relative to the solution flow. Of the two sets of facets involved in the growth of the width and length of the crystal, the {10l̅ } facets were found to be greatly affected by the solution flow while the {011} facets were not affected at all. Computational fluid dynamics simulations showed that solute concentration has higher gradients at the edges of the leading edge {10l̅ } facets, which can explain the appearance of satellite crystals. {10l̅ } facets were found to show significant structural rugosity at the molecular level, which may play a role in their mechanism of growth. The work highlights the complexities of measuring crystal growth data of even simple systems such as BZM-I, specifically addressing the effect of additives and fluid dynamics.

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Section: Methodsmentioning

confidence: 89%

Section: Slow Cooling Crystallizationsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Complex Growth of Benzamide Form I: Effect of Additives, Solution Flow, and Surface Rugosity

Offiler

Fonte

Kras

et al. 2022

Crystal Growth & Design

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“…Roger had been among the first to employ the rotating disc method in an earlier investigation of crystal growth of HMT . Recently, more than 40 years later, the method has seen a revival in the literature (with some adaptations). , Roger’s quest for reliable growth rate data for individual crystal surfaces has continued and is reflected in the description here by Offiler et al of a new experimental setup . This contribution includes a succinct overview of crystal growth rate measurement techniques over the last 50 years.…”

Section: Crystal Morphology and Crystal Growthmentioning

confidence: 99%

Professor Roger Davey: Master ofAllCrystal Trades

Cruz‐Cabeza¹,

Sadiq²,

Vetter³

et al. 2022

Crystal Growth & Design

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“…This has enabled a better fundamental understanding of processes in particle technology. [34][35][36][37][38] By contrast, an experimentally validated methodology enabling the rapid and online measurement of cuboidal or plate-like particles has yet to be developed. Full 3D characterization is possible through µCT, but this comes with several downsides, such as extended scanning times and, in the case of powders, difficulties in particle segmentation.…”

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confidence: 99%

Online 3D Characterization of Micrometer‐Sized Cuboidal Particles in Suspension

et al. 2022

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materials (e.g., metal-organic frameworks) and catalysts, and the production of pharmaceutical, agrochemical, and food compounds. In all situations, particle sizing plays a key role in the design and control of particle properties and particle size and shape manipulation.Conventionally, a single characteristic length is used to describe particles, assuming a spherical geometry, or taking advantage of the concept of equivalent diameter. This assumption may be acceptable for irregular yet compact shapes, and is an established simplification functional to the description of various physical phenomena. [1] However, it is clearly incorrect when analyzing elongated or plate-like particles, i.e., with low sphericity, which are common crystalline products. [2] This leads to particle size and shape estimates that poorly match physical reality. [3][4][5] To describe both size and shape, at least two characteristic lengths are needed, which can be obtained through a number of 2D or 3D characterization techniques. [6][7][8][9] Such (offline and online) techniques, including micro-computed tomography (µCT), [10][11][12][13][14][15][16][17] holography, [18][19][20] structural light, [21] machine vision, [13,[22][23][24][25][26][27][28][29][30][31] confocal microscopy, [32] and surface imaging [33] have varying degrees of accuracy and complexity. Machine vision through image analysis (IA) has become an increasingly powerful tool, due to experimental simplicity, hardware improvements, and continual increases in available computational power. [8] For the online measurement of elongated, needle-like particles on the microscale, effective IA algorithms have been proposed and successfully used to track particle length and width distributions. This has enabled a better fundamental understanding of processes in particle technology. [34][35][36][37][38] By contrast, an experimentally validated methodology enabling the rapid and online measurement of cuboidal or plate-like particles has yet to be developed. Full 3D characterization is possible through µCT, but this comes with several downsides, such as extended scanning times and, in the case of powders, difficulties in particle segmentation. [14] 2D characterization by single projection imaging can be fast, but does not provide sufficient information to reliably extract characteristic lengths and shapes, whilst the accuracy of multiple projection imaging is compromised by particle orientation. [6,8] Other techniques, such as holography or surface imaging, are yet to be applied to, or are unsuited for online measurement purposes.Characterization of particle size and shape is central to the study of particulate matter in its broadest sense. Whilst 1D characterization defines the state of the art, the development of 2D and 3D characterization methods has attracted increasing attention, due to a common need to measure particle shape alongside size. Herein, ensembles of micrometer-sized cuboidal particles are studied, for which reliable sizing techniques are currently missing. Such particle...

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Crystal Growth Cell Incorporating Automated Image Analysis Enabling Measurement of Facet Specific Crystal Growth Rates

Cited by 9 publications

References 65 publications

Complex Growth of Benzamide Form I: Effect of Additives, Solution Flow, and Surface Rugosity

Complex Growth of Benzamide Form I: Effect of Additives, Solution Flow, and Surface Rugosity

Professor Roger Davey: Master ofAllCrystal Trades

Online 3D Characterization of Micrometer‐Sized Cuboidal Particles in Suspension

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