Surface Degradation during Separation of Crystals from Solution: Minimizing the Shut-off Effect

Bruele, Fieke J. van den; Marks, Kess; Harmsen, Bram; Alfring, Alinda; Sprong, Hannah; Enckevort, W.J.P. van; Vlieg, E.

doi:10.1021/cg201506y

Cited by 5 publications

(6 citation statements)

References 27 publications

(49 reference statements)

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“…Figure a shows crystals grown from a small scale experiment using brine containing 20% (w/w) formamide. The crystals show clearly developed {111} faces, which is in accordance with the findings of Radenovic et al The surface of these NaCl crystals were further examined at a higher resolution to determine the crystallization pattern on the surface. Figure b shows a SEM image of the {111} surface of a crystal grown from a large scale solution experiment in the presence of 25% (w/w) formamide.…”

Section: Resultssupporting

confidence: 87%

“…It was observed by SEM that the {100} surface is much flatter than the {111} surface. The {100} surface shows evidence of the shut off effect, which occurs when a crystal is removed from solution and a thin-film of supersaturated solution remains on the surface and evaporates quickly giving rise to extra structures . However, there is no ordered nucleation pattern, but the {111} surface is more rough and displays trigonally shaped islands, which were not evident on the {100} surface.…”

Section: Resultsmentioning

confidence: 99%

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Polymer versus Monomer Action on the Growth and Habit Modification of Sodium Chloride Crystals

Townsend

Enckevort

Meijer

et al. 2015

Crystal Growth & Design

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We have investigated the use of polymers and monomers as habit modifiers and anticaking agents for sodium chloride. We show that amide functional groups cause the {111} faces to propagate on sodium chloride crystals and that polymer amides give a 1−2 orders of magnitude greater effect than the corresponding monomers on the habit modification of sodium chloride. We have also shown that the alcohol functional group does not have an effect on the surface or habit modification but that, when in a polymer form, leads to macrostep formation and acts as a nucleation inhibitor. The latter also holds true for other polymers that we have also tested. We have also found that there is no evidence of these polymers having anticaking abilities. Finally, we found that no amino acids, apart from glycine, have an effect on the morphology of NaCl crystals.

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Section: Resultssupporting

confidence: 87%

Section: Resultsmentioning

confidence: 99%

Polymer versus Monomer Action on the Growth and Habit Modification of Sodium Chloride Crystals

Townsend

Enckevort

Meijer

et al. 2015

Crystal Growth & Design

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“…The growth runs were stopped by venting the cell with air, which nearly completely blocks the transport of anthraquinone. This prevents a shut-off effect by which the substrate becomes covered by unwanted anthraquinone material …”

Section: Methodsmentioning

confidence: 99%

“…This prevents a shut-off effect by which the substrate becomes covered by unwanted anthraquinone material. 35 2.4. Characterization Methods.…”

Section: Methodsmentioning

confidence: 99%

Epitaxy of Anthraquinone on (100) NaCl: A Quantitative Approach

Enckevort¹,

Noorduin²,

Graswinckel³

et al. 2018

Crystal Growth & Design

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A growth cell suitable for microscopic in situ observation of well-controlled crystal growth from the vapor phase is used to study the heteroepitaxial growth of anthraquinone crystals on a (100) NaCl substrate. In this, the morphology, orientation, nucleation, and growth rate of the crystals is studied as a function of driving force, Δμ/kT. At the lowest Δμ/kT, the crystals are block-shaped and show no preferential orientation with respect to the substrate. Increasing the driving force leads to the growth of oriented block- and needle-shaped crystals, which nucleate from macrosteps on the substrate. At the highest Δμ/kT, crystals nucleate on the flat surface areas or at monatomic steps on the substrate, resulting in a dramatic increase in epitaxial needle density. Growth rate measurements show an exponential behavior as a function of Δμ/kT. In all cases, the supply of growth units proceeds via surface diffusion over the NaCl substrate surface toward the anthraquinone crystals. At the lowest Δμ/kT, growth is partly limited by integration of the growth units at the crystal surfaces. At intermediate driving force, kinetic roughening sets in, leading to rounded needle tips. At the highest supersaturation, growth is completely governed by the supply of growth units via surface diffusion, leading to tip splitting as a consequence of morphological instability.

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“…4 Experimental access to the buried interface during the growth is challenging. In situ observations are required because the grown structures are often prone to oxidation or because of the so-called shut-off effect, 5 which occurs as unwanted surface crystallization during the removal of a crystal from the solution. So far, in situ experiments have focused on microscopy 6 or on the growth from saturated solutions.…”

Section: ■ Introductionmentioning

confidence: 99%

Observation of Ultrathin Precursor Film Formation during Ge–Si Liquid-Phase Epitaxy from an Undersaturated Solution

et al. 2017

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Our in situ X-ray study shows that a silicon substrate in contact with an undersaturated In(Ge) solution is wetted by an approximately 1 nm thin germanium film, which does not grow any thicker. The results can be understood by the use of thickness-dependent correlated interfacial energies. This near-equilibrium heterogeneous interface structure marks the initial stage of crystal growth before the formation of bulk material, which can only form under conditions of supersaturation. This finding uncovers a fundamental aspect of the thermodynamics at solid-liquid interfaces relevant for understanding the transition from equilibrium to supersaturation and is of importance for nanoscale solution growth methods.

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Surface Degradation during Separation of Crystals from Solution: Minimizing the Shut-off Effect

Cited by 5 publications

References 27 publications

Polymer versus Monomer Action on the Growth and Habit Modification of Sodium Chloride Crystals

Polymer versus Monomer Action on the Growth and Habit Modification of Sodium Chloride Crystals

Epitaxy of Anthraquinone on (100) NaCl: A Quantitative Approach

Observation of Ultrathin Precursor Film Formation during Ge–Si Liquid-Phase Epitaxy from an Undersaturated Solution

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