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Crystal Growth

Crystal growth is the process of forming solid crystalline materials from a solution, melt, or vapor.
This process involves the nucleation and growth of crystals, which can be influenced by factors such as temperature, pressure, and the presence of impurities.
Crystal growth research is essential for the development of materials with desired properties, such as semiconductors, ceramics, and pharmaceuticals.
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Most cited protocols related to «Crystal Growth»

Crystal growth procedures are available as supplementary information. All X-ray diffraction experiments were carried out at the Caltech Molecular Observatory. Crystals were removed from wells and incubated in a cryoprotectant solution consisting of 30% ethylene glycol, 25% PEG 4000, 100 mM lithium nitrate, 10 mM copper sulfate, and 100 mM tris pH 7.0 for several minutes. During this time the large crystals under a 100 K nitrogen cryostream. 1.54 Å X-rays were generated using a Rigaku rotating anode source. Oscillation images were recorded following determination of crystal parameters in a manner to maximize completeness of the data sets. Images were recorded on a Rigaku Raxis IV++ detector operated with CRYSTALCLEAR.
Reflections were integrated and processed using iMOSFLM29 . Data were scaled and merged using SCALA30 (link). Structures were solved by the method of molecular replacement as implemented in program MOLREP12 (link) using the 2.4 Å structure of azurin C112D (PDBID: 1AG0) as a search model. The MOLREP output was then used for model building with ARP/wARP31 (link), with a single coordinate randomization included to alleviate any possible model bias. Maximum likelihood restrained refinement was carried out using program REFMAC512 (link).
Publication 2009
Azurin Cryoprotective Agents Crystal Growth Glycol, Ethylene Lithium Nitrates Nitrogen Reflex Roentgen Rays Sulfate, Copper Tromethamine X-Ray Diffraction
The crystal structure of epidermal growth factor receptor (EGFR) cocrystallized with Lapatinib was downloaded from protein data bank (PDB file: 1XKK) [35 (link)]. The MOE 2010 program was used for carrying out molecular docking for the target derivatives 29 inside the EGFR active site. The cocrystallized ligand was redocked inside the dynamic site in order to ensure the veracity of the docking study and the RMSD was determined. The 3D structures of the prepared compounds were built by the MOE molecular builder, then protonated, followed by energy minimization, then saved in an mdb file to be docked inside the active site of EGFR. Hydrogen bonds, interacting groups, and docking scores are listed in Table 2.
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Publication 2021
Crystal Growth derivatives Epidermal Growth Factor Receptor Epidermis Hydrogen Bonds Lapatinib Ligands
Setting up an in meso crystallization trial is straightforward (Fig. 4). Typically, it involves combining two parts protein solution with three parts lipid at 20°C (Caffrey & Cherezov, 2009 ▶ ; Caffrey & Porter, 2010 ▶ ). The most commonly used lipid is the monoacylglycerol (MAG) monoolein. According to the monoolein–water temperature–composition phase diagram (Fig. 5; Qiu & Caffrey, 2000 ▶ ), and assuming there is no major influence on the phase behaviour of the protein-solution components, this mixing process should generate, by spontaneous self-assembly, the cubic mesophase at or close to full hydration. The original method for mixing lipid and protein solution involved multiple, cumbersome centrifugations in small glass tubes. Harvesting crystals required cutting the tubes and searching for small crystals through curved glass, which was not easy, very inefficient and required experience, time and patience.
The cubic phase is sticky and viscous in the manner of thick toothpaste (Fig. 6). As such, it is not easy to handle. In the course of earlier lipid-phase science work carried out in the Membrane Structural and Functional Biology (MS&FB) group, we had developed tools and procedures for manipulating such refractory materials. One of these, the coupled-syringe mixing device (Fig. 4; Cheng et al., 1998 ▶ ), was ideally suited to the task of combining microlitre volumes of monoolein with membrane-protein solution in a way that produces protein-laden mesophase for direct use in crystallization trials with minimal waste. The mixer consists of two, positive-displacement Hamilton micro-syringes connected by a narrow-bore coupler. Lipid is placed in one syringe and protein solution in the other. Mixing is achieved by repeatedly moving the contents of the two syringes back and forth through the coupler (Caffrey & Porter, 2010 ▶ ). The coupler is replaced by a needle for convenient dispensing of the homogenous mesophase into wells of custom-designed, glass sandwich crystallization plates (Cherezov & Caffrey, 2003 ▶ ; Cherezov et al., 2004 ▶ ). Precipitant solutions of varying compositions are placed over the mesophase and the wells are sealed with a cover glass. For initial screening, the plates are incubated at 20°C and monitored for crystal growth. The optical quality is the best it can be given that the mesophase is held between two glass plates and the mesophase itself is transparent (Fig. 7). This means that crystals of just a few micrometres in size can readily be seen by microscope whether the proteins are coloured or not. The use of cross-polarizers can enhance the visibility of small crystals, which usually appear birefringent on a dark background; the cubic phase itself is optically isotropic and non-birefringent. An added feature of the glass sandwich plates is that the double-sided tape used to create the wells provides almost hermetic sealing, ensuring minimal change in well composition during the course of trials that can last for months. Step-by-step instructions, complete with an open-access online video demonstration of the entire in meso crystallization process, have been published (Caffrey & Cherezov, 2009 ▶ ; Caffrey & Porter, 2010 ▶ ; Li, Boland, Aragão et al., 2012 ▶ ; Li, Boland, Walsh et al., 2012 ▶ ).
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Publication 2015
ARID1A protein, human Birefringence Centrifugation Crystal Growth Crystallization Cuboid Bone Hermetic Homozygote Lipids Membrane Proteins Microscopy Monoglycerides monoolein Needles Proteins Syringes Tissue, Membrane Toothpaste Viscosity Vision
Crystallization trials began with the reconstitution of the protein into the bilayer of the lipidic cubic mesophase following a standard protocol32 (link). The protein solution at 12 mg/mL was homogenized with 7.9 MAG in equal parts by volume using a coupled syringe device at room temperature (20–22 °C). Approximately 20 μL of protein-laden mesophase was transferred into a 0.5 mL Hamilton syringe containing 0.4 mL precipitant solution (0.2 % (v/v) MPD, 0.1 M sodium chloride, 0.1 M sodium citrate pH 5.6) using a narrow bore coupler32 (link), as described above for GPCR crystallization. The syringe was incubated for 21 d at 20 °C for crystal growth. After separating the bathing solution from the crystal-laden LCP, excess precipitant was absorbed by mixing in 3–5 μL molten 7.9 MAG. This procedure produced optically clear LCP in which microcrystals were dispersed ready for loading into the reservoir of the LCP injector, as described above.
Publication 2014
Crystal Growth Crystallization Cuboid Bone Lipid Bilayers Proteins Sodium Chloride Sodium Citrate Syringes
Purified SOSIP.664 gp140 trimers were tested for crystallizability either alone or as complexes with one or more ligands from the following list: soluble CD4, Fabs: PGT121, PGT122, PGT123, PGT127, PGT128, PGT135, PG9, PG16, PGT145, PGV04, 17b. In addition, purified trimers and complexes were in some cases treated with the following glycosidases, alone or in combination, for 3 h at temperatures ranging between 20-37°C: EndoH (New England Biolabs), EndoD (VWR), Endo F1 (EMD Chemicals) or α1,2,3,6 mannosidase (QA-Bio). The monodispersity of the resulting samples was measured by SDS-PAGE, BN-PAGE and SEC coupled in-line with multi-angle light scattering (SEC-MALS) using the following layout: a Superose 6 10/30 SEC column (GE Healthcare) operated on an AKTA Avant FPLC system (GE Healthcare) with the following calibrated detectors: 1) HP1 1050 Hewlett-Packard UV detector (Norwalk, CT); 2) MiniDawn Treos multi-angle light scattering (MALS) detector (Wyatt Corporation, CA); 3) quasi-elastic light scattering (QELS) detector (Wyatt Corporation, CA); and 4) Optilab T-reX refractive index (RI) detector (Wyatt Corporation, CA). The purified complexes were concentrated to approximately 2-6 mg/ml and subjected to extensive crystallization trials using either: 1) the Oryx8 crystallization robot (Douglas Instruments) with 96 different crystallization conditions at 16°C; or 2) the automated IAVI/JCSG/TRSI CrystalMation robotic system (Rigaku) at the Joint Center for Structural Genomics (www.jcsg.org), where 384 different crystallization conditions were tested at 4°C and 22°C.
In the above trials, only the partially deglycosylated SOSIP.664 gp140 trimers from various isolates in complex with antibodies of the PGT121-family (PGT121, PGT122 and PGT123) resulted in crystal hits. Surprisingly, for these complexes, hits were obtained from approximately 10% of the crystallization conditions, but the majority of crystals tested (>600) only diffracted to 8 Å or worse at various synchrotron sources (APS, SSRL, and CLS). Several pre- and post-crystallization strategies were explored in an effort to improve the x-ray diffraction properties of these crystals: however, the use of single-chain Fv instead of Fab, limited in-situ proteolysis, varying temperature of crystal growth, additives screening, crystal cross-linking, dehydration, and annealing all met with limited success. In addition, we attempted use of a SOSIP construct further truncated to gp41 position 650. Although crystals could be obtained with the trimer in complex with PGT122 Fab, these did not show improved diffraction properties compared to the majority of SOSIP.664-containing crystals.
Publication 2013
Antibodies Crystal Growth Crystallization Dehydration Endometriosis Glycoside Hydrolases GP 140 Joints Ligands Light Mannosidase Phytolacca dodecandra Proteolysis recombinant soluble CD4 SDS-PAGE Single-Chain Antibodies X-Ray Diffraction

Most recents protocols related to «Crystal Growth»

Example 3

To evaluate the crystal morphology of the example iPP/CNF composites, a ME520 Series polarized light microscope (PLM) (AmScope, USA) was utilized. Sections that were 3 μm-thick were obtained from cross sections of injection molded specimens using a Sorvall MT2-B Ultramicrotome. Each section was placed between a glass slide and a cover slip then transferred to a hot plate (Thermo Scientific) at 200° C. for 2 min before it was cooled at room temperature.

FIG. 5 shows the crystal morphology of iPP and iPP/CNF composites obtained by a polarized light microscope. Because no cold-crystallization peaks were observed in the DSC scans for all specimens, the crystal morphology caused by the micrograph preparation was negligible. As the CNF content was increased in the iPP matrix, the nucleation density increased, but spherulite size decreased. Typical crystal diameters of iPP, iPP/MA, and the iPP/CNF3%, iPP/CNF10%, iPP/CNF30% and iPP/MA/CNF10% composites were about 33 μm, 27 μm, 21 μm, 12 μm, 8 μm, and 10 μm, respectively. These results suggested that CNF restricted the folding motion of polymer chains during crystallization and made the re-entry of polymer chains into the crystal face more difficult, resulting in smaller crystals. Hence, steric hindrance attributed to a large concentration of CNF resulted in the high values of ΔE for iPP, as shown in Table 5. Meanwhile, MAPP allowed the PP to mix more effectively with CNF. MAPP may also have facilitated transcrystallization, a process in which spherulites grow perpendicularly to a surface. Transcrystallization can improve the attachment of polymer segments to the crystal surface and reduce ΔE. However, the method used in this example to prepare sections for PLM observation involved fairly rapid cooling (˜80° C./min), which may have created thin transcrystalline layers. Thin crystal layers are not readily seen in PLM at high magnification because of their weak light intensity. A possible site of CNF transcrystallization was identified in the iPP/MA/CNF10% composite shown in FIG. 5. As a comparison, the morphology of the PP spherulites on the CNF surfaces in the PP/CNF3% composite is also shown and was almost identical to that of the iPP matrix. These results suggest that MAPP caused a transcrystalline layer formation. The PLM micrographs also confirmed kinetic results obtain in previous sections.

The overall crystallization rate may be dependent on nucleation rate and crystal growth rate. For iPP/CNF3%, the presence of CNF increased the nucleation density without affecting the crystal growth. Therefore, iPP/CNF3% had an accelerated crystallization rate. For iPP/CNF10%, the nucleation density pf iPP was increased by the CNF. At the same time, crystal growth was impeded by CNF. Overall, CNF reduced iPP's crystallization rate when present at 10 wt. %. After MAPP was introduced to iPP/CNF10%, the nucleation density of the composite furthered increased because of a coupling effect. Moreover, the formation of transcrystalline layers facilitated crystal growth.

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Patent 2024
Cold Temperature Crystal Growth Crystallization Debility Face Kinetics Light Microscopy Microscopy, Polarization Polymers Radionuclide Imaging Ultramicrotomy Vision

Example 9

Single Crystal Growth and Sample Preparation

Form 1 was analyzed by single crystal X-ray diffraction. The crystal was obtained from a DMF solution of Form 1 followed by slow evaporation. The crystal structure was determined at 100(2) K.

Results

The crystal is monoclinic, space group P21/c with the final R1 [I>2σ(I)]=4.37%. The structure was identified as depicted in FIG. 27 and the asymmetric unit found to contain 1 molecule of Compound 1. The structure of Compound 1 is a coordination polymer where the potassium cation is coordinated by four ligands (FIG. 28). Table 11 summarizes sample and crystal data for Form 1. Simulated XRPD pattern at 100K is shown in FIG. 29.

TABLE 11
Sample and crystal data for Form 1.
Empirical formulaC21H17FKN5O5S
Formula weight509.55
Temperature100(2)K
Wavelength1.54184
Crystal size0.140 × 0.120 × 0.010 mm
Crystal habitcolorless plate
Crystal systemMonoclinic
Space groupP21/c
Unit cell dimensionsa = 19.5421(9) Å a = 90°
b = 15.1329(6) Å b = 90.579(4)°
c = 6.9265(3) Å g = 90°
Volume2048.27(15) Å3
Z4
Density (calculated)1.652Mg/m3
Absorption coefficient3.740mm−1
F(000)1048

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Patent 2024
Cells Crystal Growth Crystallography, X-Ray Ligands Polymers Potassium Radiography
Reagent precursors metals Bi, Sb, Te, Se were ordered from Sigma-Aldrich Co., purity 5N grade. Quartz tubes were ordered from Technical Glass Products, Inc. with an outer diameter of 14 mm, inner diameter of 12 mm, and wall thickness of 2 mm for the ampoule. The raw materials were prepared with a Bi:Sb:Te:Se ratio of 1:1:1:2. The material total weight was 3 g mixed and crushed for 30 min, producing mixed fine powder. The powder was then loaded into the quartz tube to prepare for sealing. The inner tube wall was carbon-coated, preventing any possible reaction of the materials to the tube wall. Afterward, the tube was flushed with argon gas four times, displacing air, followed by vacuum pumping to reach a pressure below 10−6 torr to allow crystal growth in a vacuumed atmosphere. Finally, the tube was sealed by a hydrogen gas torch to a length of 6–8 cm.
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Publication 2023
Argon Atmosphere Carbon Crystal Growth Hydrogen Metals Powder Pressure Quartz
After BSTS crystal growth, the ampoule was gently broken and the material was cleaved via razor blade and exfoliated to produce a thin layer for elemental composition detection using energy-dispersive X-ray spectroscopy (EDS, HITACHI S-4800 High Resolution Field Emission Scanning Electron Microscopy (SEM)) operating at an acceleration voltage of 20 to 30 kV. Both solid and powder samples were prepared for both crystal plane and powder X-ray diffraction (XRD, Philips PANalytical X’Pert, Cu Kα wavelength). For peak identification and crystal structure Rigaku data analysis software (PDXL—version 2) was used. Part of the crystal was prepared via fracturing for Thermo-gravimetric analysis (TGA, TA Instruments Discovery SDT 650).
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Publication 2023
Acceleration Crystal Growth Energy Dispersive X Ray Spectroscopy Powder Scanning Electron Microscopy Thermogravimetry X-Ray Diffraction
The manufacture of PV modules involves several stages, from quartz mining to PV module production, as shown in Fig. 2. The system starts with silica sand acquisition, of which only heat and sand are added to the first stage to obtain silica sand61 . Metallurgical grade silicon, a crucial stepping stone in the refining process of silicon metals, is then yielded by a carbothermic reduction reaction from silica sand with other material inputted, including petroleum coke, wet wood chips, etc., into the second stage62 (link). After metallurgical grade silicon is obtained, electronics grade silicon is produced through the Siemens process, which involves the deposition of silicon from a mixture of purified silane with an excess of liquid hydrogen onto high purity metallurgical grade silicon. Solar grade silicon is produced through a modified Siemens process, which involves additional processing to separate the toxic and corrosive gas from the reduction process of metallurgical grade silicon63 (link),64 (link). These procedures to obtain all these types of silicons are homogeneous regardless of c-Si technology type, although the quantities needed to produce the same functional unit of three types of c-Si PV modules are different. After solar grade and electronics grade silicon are obtained, the manufacturing configurations of PV systems start to differ by the type of c-Si selected as the semiconductor material to form cells and modules. When sc-Si is the semiconductor material, the Czochralski crystal growth technique is implemented to form sc-Si crystal blocks in an inert atmosphere, such as argon in this study65 (link). These crystals then go through the wafer sawing process in that individual silicon chips are mechanically separated from each other for cell manufacturing66 (link). When r-Si is the semiconductor material, solar grade silicon and electronics grade silicon are used directly for r-Si wafer production, of which carbon-based strings are pulled upward through holes with molten silicon, and sawing loss is avoided67 (link), leading to relatively low energy required to manufacture r-Si PV module compared with sc-Si and mc-Si technologies. When mc-Si is picked as the semiconductor material, solar grade silicon and electronics grade silicon are melted and cast into quartz crucibles to form mc-Si ingots68 (link). Similar to sc-Si crystals, mc-Si ingots then go through the process of wafer sawing69 (link). Processing of silicon wafers into solar cells involves texturing, acid cleaning, diffusion, etching, etc., while electrical contacts are placed between the cells and then wired and arrayed to form modules. Despite the differences in wafer types, the cell manufacturing and module assembly processes are similar for all three types of c-Si technologies70 (link).
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Publication 2023
Acids Argon Atmosphere Calculi Carbon Cardiac Arrest CD3EAP protein, human Cells Cocaine Corrosives Crystal Growth Diffusion DNA Chips Edema Electricity Hydrogen Metals Petroleum Place Cells Quartz Silanes Silicon Silicon Dioxide

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