File Name: progress in crystal growth and characterization of materials .zip
The scope of Materials Technology Materials especially crystalline materials provide the foundation of our modern technologically driven world. The domination of materials is achieved through detailed scientific research.
This chapter covers the field of bulk single crystals of materials used in electronics and optoelectronics. Single-crystal material usually provides superior properties to polycrystalline or amorphous equivalents. The various bulk growth techniques are outlined, together with specific critical features, and examples are given of the types of materials, and their current typical sizes, grown by these techniques. Neither does this chapter cover the more fundamental aspects of the growth of the particular materials covered; again the reader is referred to relevant chapters within the handbook, or to other sources of information in the general literature.
Studies of proton conductivity in crystalline porous materials CPMs , mainly metal—organic frameworks MOFs and coordination polymers CPs , have received enormous attention due to their potential application in fuel cell membranes. These materials have well-defined structural features, easy synthetic routes, and functionalizable channels. These factors provide an added advantage of their targeted synthesis and control of framework—carrier interactions that eventually determine the orderly arrangement, mobility, and density of the proton carriers.
The nature of framework—carrier interactions depends on a few characteristic features such as the choice of metal ions to build the framework, the nature of the ligands, the flexibility of the framework, and the polarity of the guest molecules. This Perspective focuses on understanding the fundamental principles of proton conduction, implicates various design strategies, and discusses the role of host—guest interactions in proton conductivity, a factor largely overlooked so far.
Mineralization in living organisms is highly regulated by the synergistic action of many macromolecules, where distinctive proteins play the role of direct modulators of the crystal growth. The number of methods for in vitro biomineralization studies in the presence of proteins is limited due to the influence of the environment on their functionality. We focus on a counter-diffusion system in the biomineralization of calcium carbonate that is based on the diffusion of salt solutions through a gel-matrix supplemented with the protein of interest.
This article discusses the background of the system, physical principles, matrices commonly in use, advantages, limitations, variations, and our own experience. Special attention is paid to the overview of already published studies that applied the counter-diffusion system as a model for investigation of the biomineralization of calcium carbonate. The system has great potential to be widely used in the analysis of biomineralization-associated proteins in vitro and the biomineralization process itself.
This perspective recalls the most important theoretical basis as well as practical application of the system for specialists in various fields of biomineralization.
Most notably, the detonation properties of the cocrystal are better than that of the hypothetical physical mixture and also higher than the theoretically predicted salt, making this a rare example of a cocrystal in which the detonation properties are synergistic.
The facile and rapid microwave-assisted method has been demonstrated to be effective in synthesizing manganese fluoride MnF2 nanoparticles in binary mixtures of ethylene glycol and imidazolium-based ionic liquid containing fluorine, within a minute, without any surfactant and stabilizer. The effect of volume ratio of an ionic liquid in the binary mixtures with ethylene glycol and the length of the alkyl chain of imidazolium on the morphologies and crystalline structures of MnF2 was investigated.
The morphologies of rutile MnF2 clearly varied depending on what kind of ionic liquid was used in the synthesis. Clear room temperature photoluminescence PL spectra of MnF2 nanoparticles were observed at ambient pressure. The change of PL spectra depending on the crystalline phase was also observed. In this study, we report that the microwave-assisted method using ethylene glycol—ionic liquid binary mixtures is proper for synthesizing high-quality MnF2 nanoparticles with controllable crystalline phase and morphology.
The self-assembly of nickel II nitrate hexahydrate and a rigid tetraphosphonic acid H8L under hydrothermal conditions has resulted in the formation of a NiII phosphonate 1. The cycloaddition reaction of CO2 and epoxides was carried out under ambient conditions to investigate the catalytic activity of 1, and the results show its excellent performance in the catalysis.
Moreover, compound 1 can be easily separated and reused without significant reduction in the catalytic ability. The heterogeneous nature along with good catalytic performance entitles 1 as an excellent catalyst for CO2 transformation. A new cocrystal of Vitamin D3 Cholecalciferol and resorcinol has been discovered and characterized through experimental cocrystal screening. Its high stability has been studied against light, heat, and chemicals present in animal food premixes in order to develop a novel and alternative formulation to current microencapsulation approaches to protect Vitamin D3 from oxidation.
Our results show that the new cocrystal is extremely stable and it can become the basis for very efficient formulations of Vitamin D3 which fulfills the stability requirements of industrial applications. Water-soluble, anionic calix[n]arenes are useful receptors for protein recognition and assembly.
For example, sulfonato-calixarene sclx8 can encapsulate proteins and direct their assembly into porous frameworks. A cocrystal structure of p-benzyl-sulfonato-calixarene b-sclx8 and cytochrome c cyt c revealed a surprising assembly. A pseudorotaxane comprising a stack of three b-sclx8 molecules threaded by polyethylene glycol PEG was bound to the protein.
The trimeric b-sclx8 stack, a tubelike structure with a highly charged surface, mediated assembly via a new mode of protein recognition. This unprecedented binding mode suggests new possibilities for supramolecular protein chemistry.
Thermal expansion of an organic salt, prepared by solvent-drop grinding of terephthalic acid and imidazole in a ratio, has been studied over a wide range of temperature — K. Restricted motion of the components in the hydrogen-bonded network resembles a fence-like structure led to a uniaxial negative thermal expansion NTE. Large transverse vibration of atoms involved in the hydrogen bonding plays an unprecedented role to keep the distances constant.
Diphenylamine reacts with benzophenone in the solid state through the formation of a eutectic liquid intermediate, from which the final product, in the form of a hydrogen-bonded cocrystal, is finally formed.
Accompanied by isothermal and nonisothermal spectroscopic monitoring of the system, this provides additional details of the mechanistic pathway of the process of cocrystal formation through a metastable liquid intermediate phase. The initialization of barite deposition is believed to be mineral nucleation.
The induction times characterizing the kinetics of nucleation have been widely studied to investigate the precipitation kinetics of barium sulfate and to estimate the risk of mineral deposition in the flowing tube. However, recent research shows that barium sulfate still deposits inside the flowing tube even though the predicted induction time is longer than the travel time.
The results correlate to the field observations that the mineral scale deposition is found in the production well even at the condition that is predicted to be kinetically stable. The contradiction suggests that there is a missing step of mineral deposition in the flow. In this work, a hypothesis of nucleation in the boundary layer is proposed to explain the contradiction: the barium sulfate can nucleate inside the boundary layer at the surface where the linear flow velocity approaches zero.
This slow-flow region offers enough time for the crystals to form without being flushed away. A series of experiments were conducted in the flowing tube and the microfluidic channels to support the hypothesis. The amounts of deposited barium sulfate in the pipes were measured and compared with the induction time prediction. On the other hand, the observed nucleation time in the microfluidic channels matches the previously reported nucleation time in the kinetic turbidity tests in beakers.
This implies that the barium sulfate can stay and nucleate in the boundary layer at the surface, which further supports the proposed mechanism. To conclude, we combine the ideas of induction times, boundary layer, and precipitation kinetics to describe a new mechanism of barium sulfate deposition.
Once the solution in the boundary layer reaches its induction time, the deposition begins. Syntheses of transition-metal dichalcogenides TMDs using colloidal-chemistry approaches are gaining significant interest in recent years, as these methods enable the morphology and properties of the nanocrystals to be tuned for targeted applications.
Surface chemistry analyses of the synthesized nanocrystals by solution NMR establish that neither of the ligands bind strongly to the surface of nanocrystals but are in a dynamic coordination with the WSe2 surface. A further examination of the coordination of tungsten hexacarbonyl W CO 6 with the respective ligands confirms that W CO 6 decomposes in OA, losing its octahedral symmetry, which leads to fast reactivity in the flask.
These insights into the influence of precursor-ligand chemistry on reaction outcome and the peculiar surface chemistry of colloidal TMD nanocrystals will be instrumental in developing future colloidal TMD nanocrystals. The present work reports two Zn II based metal—organic frameworks that show excellent proton conductivity with potential application in proton exchange membrane fuel cell development.
Structural studies show some intriguing crystallographic phenomena including the occurrence of different conformations in the same crystal lattice. Furthermore, the compounds exhibit excellent chemical and thermal stability. Both compounds show some important structural features that make them highly suitable candidates for proton conductivity. The above features indicate that both MOFs are suitable for fuel cell development, while further support comes from the corroborating variable temperature proton conductivity data.
Multicomponent crystal forms for drugs with poor solubility, such as orotic acid OA , can potentially promote dissolution behavior and bioavailability. Herein an affinity prediction was carried out to predict the formation of multicomponent crystal forms between OA and 41 coformers.
Amino acids were selected as coformers to solve the solid-state solubility problem of OA. Six new multicomponent crystal forms, including five salts and one salt hydrate, were characterized and confirmed by powder X-ray diffraction, differential scanning calorimetry, and thermogravimetric analysis.
Finally, a powder dissolution study was conducted. The powder dissolution of all salts presented a higher apparent solubility 1. This study investigates the effect of solid-state intermolecular binding energies on the dissolution rates of single faceted-crystals.
In vitro dissolution of the ibuprofen crystals is quantified by capturing images during the dissolution process at fixed time intervals using a camera mounted on an inverted optical microscope.
The regression rate of crystal faces with time is measured by an image analysis. VisualHabit software is used for a prediction of the crystal morphology and to characterize the intermolecular binding energies in the solid-state structure of the ibuprofen crystals to predict relative, face-specific dissolution rates. The relative face-specific dissolution rates of ibuprofen crystal calculated based on binding energies suggest that the face dissolves faster than face The experimental results on face-specific dissolution rates of single ibuprofen crystals reveal that the dissolution rates of faces and change nonlinearly as a function of undersaturation.
The binding energy model is critically evaluated for performance as confronted with the experimental measurements. The binding energy model suggests a pathway to understand dissolution at the microscopic level and to design a crystal morphology for regulating bioavailability optimally during dissolution processes.
We demonstrate that the use of suspension temperature cycling in combination with tailor-made additives alleviates such extreme needle-like morphologies and increases the average particle size of this cocrystal material. Temperature cycling of the cocrystal suspensions in ethanol alone reduces the mean aspect ratio from 10 to 3. The further addition of low concentrations of benzamide or nicotinamide suppresses the growth rate at the tip of the needle even more, resulting in a more favorable equant morphology.
An iterative mechanism in which additives are incorporated in the lattice structure and released during the temperature increase in each cycle is proposed.
Thus, the incorporation of an additive at the normally fast growing and potential needle tips and its release during the temperature increase part of the cycle effectively makes an additive action catalytic. The simultaneous use of temperature cycling and tailor-made additives offers a new and effective approach for the elimination of unsatisfactory needle-like crystal morphologies and a small crystal size during the production of a pharmaceutical cocrystal material.
Trimethoprim TMP is an active pharmaceutical ingredient with poor aqueous solubility. Here, we describe the cocrystallization of TMP with five co-formers, three bipyridines and two monopyridines. Cocrystallization of TMP with the bipyridines yields neutral cocrystals, and while both components are present in the lattice, they do not interact with each other via any strong intermolecular forces. Conversely, cocrystallization of TMP with the monopyridines yields salts, and included water or solvent molecules that play a key role in supramolecular assembly.
Moreover, the salts exhibit significantly higher aqueous solubility than that of TMP. Two solids feature a compound on the Generally Recognized as Safe list, making them promising as ionic pharmaceutical cocrystals.
Layered double hydroxides LDHs are a class of cationic-layered solids that can be synthetically designed for a variety of advanced functions. Facile thin film growth of LDHs is an important requisite for a variety of applications including functional coatings, displays, and sensing.
In this work we demonstrate, for the first time, an in situ and patternable thin film synthesis of interconnected Zn—Cr LDH particles from a transparent conducting oxide precursor, aluminum-doped zinc oxide, at room temperature within minutes.
Synthetic parameters such as chromium III nitrate concentration, solvent composition, and reaction time were found to significantly affect the thickness and morphology of the resulting LDH films.
These LDH thin films can undergo interlayer anion exchange, which modulates the interlayer distance of the LDH sheets and surface energy of the thin film. Replacement of the interlayer anion with perfluorooctanoate increases the interlayer sheet distance from 0. The synthetic method and structural analysis of the LDH thin films introduced in this work opens new avenues of application for LDH films. This work reports on uniformly mingled nanostructures of Co3O4 and MnO2 deposited on a well-aligned electrospun carbon nanofiber WA-ECNF mat for rapid glucose electrooxidation and sensing.
These results are discussed with mechanisms of glucose absorption to the nanostructure surfaces followed by a fast glucose oxidation reaction. Molecular shape is observed to greatly determine the properties of energetic materials EMs ; that is, the spherical molecules generally have high energy while the planar molecules have low sensitivity in common.
Nevertheless, how the molecular shapes along with their packing modes affect the crystal packing features, such as crystal density and packing coefficient PC , that are crucial factors describing the energy and sensitivity properties of EMs, is still unclear.
Herein, this issue was addressed via a statistical analysis of more than available energetic crystals. Despite crystal density having an overall increasing trend with PC, high crystal density and high PC are dominated by spherical and planar molecules, respectively. Intra- and intermolecular hydrogen bonds are important factors that affect molecular shapes and packing features of EMs, respectively.
Scientific Research An Academic Publisher. Liu, F. Yun and H. Muranaka, Y. Kikuchi, T.
Studies of proton conductivity in crystalline porous materials CPMs , mainly metal—organic frameworks MOFs and coordination polymers CPs , have received enormous attention due to their potential application in fuel cell membranes. These materials have well-defined structural features, easy synthetic routes, and functionalizable channels. These factors provide an added advantage of their targeted synthesis and control of framework—carrier interactions that eventually determine the orderly arrangement, mobility, and density of the proton carriers. The nature of framework—carrier interactions depends on a few characteristic features such as the choice of metal ions to build the framework, the nature of the ligands, the flexibility of the framework, and the polarity of the guest molecules. This Perspective focuses on understanding the fundamental principles of proton conduction, implicates various design strategies, and discusses the role of host—guest interactions in proton conductivity, a factor largely overlooked so far. Mineralization in living organisms is highly regulated by the synergistic action of many macromolecules, where distinctive proteins play the role of direct modulators of the crystal growth.
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Materials genome is a subversive frontier technology emerging in the field of international materials in recent years and also a propeller for the development of new materials. It brings fundamental changes to the traditional material research mode, aiming to accelerate the research and development of new materials and reduce costs, so as to support the development of electronic information, energy and environmental protection, aerospace, and other industries. In this paper, we introduce the strategic significance, national layout, and methods of materials genome technology and emphatically introduce the design idea and development status of materials database method. Then we summarize the development trends of materials genome and put forward suggestions for its future research, aiming to provide references for the development direction of materials genome technology in various countries, especially in developing countries. New materials, such as new energy materials, information materials, and intelligent materials, are the core of subversive technology revolution and also the strategic highland of fierce competition among countries around the world.
Help expand a public dataset of research that support the SDGs. The scope of Materials Technology Materials especially crystalline materials provide the foundation of our modern technologically driven world.
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