Microfluidic screening of potassium nitrate polymorphism

Laval, Pierre-François; Giroux, Céline; Leng, Jacques; Salmon, Jean‐Baptiste

doi:10.1016/j.jcrysgro.2008.03.009

Cited by 39 publications

(52 citation statements)

References 26 publications

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“…5 One highly effective method for obtaining reproducible data is to perform crystallisation within droplets. 6 These not only provide the opportunity to perform hundreds of experiments very quickly, but the small reaction volume is such that the majority of droplets do not contain impurities; those that do generate outlying data points and can in principle be excluded. To this end, levitated droplets 7,8 and droplets created using automated dispensing systems 9-11 have previously been used to study homogeneous nucleation and to facilitate rapid screening of crystallisation conditions.…”

Section: Introductionmentioning

confidence: 99%

“…The volume contained within each droplet provides a well-defined and confined environment where homogeneous nucleation of crystals can be studied. 14,15 The potential of this approach has been established in the generation of high quality protein crystals for subsequent XRD analysis, [16][17][18] the screening of potassium nitrate polymorphism, 6 the investigation of nucleation phenomena, 1,19 and the screening of solubility diagrams. 20 Herein, we describe the use of droplet-based microfluidics to investigate the precipitation of calcium carbonate under highly controlled conditions.…”

Section: Introductionmentioning

confidence: 99%

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Calcium carbonate polymorph control using droplet-based microfluidics

2012

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Calcium carbonate (CaCO 3 ) is one of the most abundant minerals and of high importance in many areas of science including global CO 2 exchange, industrial water treatment energy storage, and the formation of shells and skeletons. Industrially, calcium carbonate is also used in the production of cement, glasses, paints, plastics, rubbers, ceramics, and steel, as well as being a key material in oil refining and iron ore purification. CaCO 3 displays a complex polymorphic behaviour which, despite numerous experiments, remains poorly characterised. In this paper, we report the use of a segmented-flow microfluidic reactor for the controlled precipitation of calcium carbonate and compare the resulting crystal properties with those obtained using both continuous flow microfluidic reactors and conventional bulk methods. Through combination of equal volumes of equimolar aqueous solutions of calcium chloride and sodium carbonate on the picoliter scale, it was possible to achieve excellent definition of both crystal size and size distribution. Furthermore, highly reproducible control over crystal polymorph could be realised, such that pure calcite, pure vaterite, or a mixture of calcite and vaterite could be precipitated depending on the reaction conditions and dropletvolumes employed. In contrast, the crystals precipitated in the continuous flow and bulk systems comprised of a mixture of calcite and vaterite and exhibited a broad distribution of sizes for all reaction conditions investigated.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Calcium carbonate polymorph control using droplet-based microfluidics

2012

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“…However, measurements of nucleation kinetics in traditional emulsion crystallizations [54] have severe limitations due to the polydispersity of emulsions and the existence of surfactants. Thus, besides the synthesis of crystals, nucleation kinetics has become one of the focuses of study of crystallization in monodisperse droplets generated in microfluidic devices [55][56][57][58][59][60].…”

Section: Nucleation Kineticsmentioning

confidence: 99%

“…Laval et al [57][58][59][60] fabricated a new microfluidic device consisting of a droplets-generation section by flowfocusing and a droplets-storage section composed of several parallel channels to assist the study of crystallization. Hundreds of nanolitre droplets of a given solution can be stored in the device and can be manipulated as independent microreactors.…”

Section: Nucleation Kineticsmentioning

confidence: 99%

“…By building a two-dimensional array of droplets with both concentration and temperature gradients, the solubility curve of adipic acid solution was measured as an application for the screening technology of solubility diagrams [57]. In the study of crystallization and dissolution of potassium nitrate (KNO 3 ) in water [58], they observed independent and mononuclear crystallization and the existence of two concomitant polymorphic forms. They measured the solubility curves and metastable zones of both polymorphs.…”

Section: Nucleation Kineticsmentioning

confidence: 99%

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Synthesis of crystals and particles by crystallization and polymerization in droplet-based microfluidic devices

Wang

Zhang

Han

2010

Front. Chem. Eng. China

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The recent advances in crystallization and polymerization assisted by droplet-based microfluidics to synthesize micro-particles and micro-crystals are reviewed in this paper. Droplet-based microfluidic devices are powerful tools to execute some precise controls and operations on the flow inside microchannels by adjusting fluid dynamics parameters to produce monodisperse emulsions or multiple-emulsions of various materials. Major features of this technique are producing particles of monodispersity to control the shape of particles in a new level, and to generate droplets of diverse materials including aqueous solutions, gels and polymers. Numerous microfluidic devices have been employed to generate monodisperse droplets of range from nm to μm, such as T junctions, flow-focusing devices and co-flow or cross-flow capillaries. These discrete, independently controllable droplets are ideal microreactors to be manipulated in the channels to synthesize the nanocrystals, protein crystals, polymer particles and microcapsules. The generated monodisperse particles or crystals are to meet different technical demands in many fields, such as crystal engineering, encapsulation and drug delivery systems. Microfluidic devices are promising tools in the synthesis of micron polymer particles that have diverse applications such as the photonic materials, ion-exchange and chromatography columns, and field-responsive rheological fluids. Processes assisted by microfluidic devices are able to produce the polymer particles (including Janus particles) with precise control over their sizes, size distribution, morphology and compositions. The technology of microfluidics has also been employed to generate core-shell microcapsules and solid microgels with precise controlled sizes and inner structures. The chosen "smart" materials are sensitive to an external stimulus such as the change of the pH, electric field and temperature. These complex particles are also able to be functionalized by encapsulating nanoparticles of special functions and by attaching some special groups like targeting ligands. The nucleation kinetics of some crystals like KNO 3 was investigated in different microfluidic devices. Because of the elimination of the interactions among crystallites in bulk systems, using independent droplets may help to measure the nucleation rate more accurately. In structural biology, the droplets produced in microfluidic devices provide ideal platforms for protein crystallization on the nanoliter scale. Therefore, they become one of the promising tools to screen the optimal conditions of protein crystallization.

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Crystallization in Confinement

2020

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Many crystallization processes of great importance, including frost heave, biomineralization, the synthesis of nanomaterials, and scale formation, occur in small volumes rather than bulk solution. Here, the influence of confinement on crystallization processes is described, drawing together information from fields as diverse as bioinspired mineralization, templating, pharmaceuticals, colloidal crystallization, and geochemistry. Experiments are principally conducted within confining systems that offer well‐defined environments, varying from droplets in microfluidic devices, to cylindrical pores in filtration membranes, to nanoporous glasses and carbon nanotubes. Dramatic effects are observed, including a stabilization of metastable polymorphs, a depression of freezing points, and the formation of crystals with preferred orientations, modified morphologies, and even structures not seen in bulk. Confinement is also shown to influence crystallization processes over length scales ranging from the atomic to hundreds of micrometers, and to originate from a wide range of mechanisms. The development of an enhanced understanding of the influence of confinement on crystal nucleation and growth will not only provide superior insight into crystallization processes in many real‐world environments, but will also enable this phenomenon to be used to control crystallization in applications including nanomaterial synthesis, heavy metal remediation, and the prevention of weathering.

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Microfluidic screening of potassium nitrate polymorphism

Cited by 39 publications

References 26 publications

Calcium carbonate polymorph control using droplet-based microfluidics

Calcium carbonate polymorph control using droplet-based microfluidics

Synthesis of crystals and particles by crystallization and polymerization in droplet-based microfluidic devices

Crystallization in Confinement

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