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Synthesis, Characterization, and Properties of Rivaroxaban New Crystalline Forms 利伐沙班新晶型的合成、表征和性质
IF 1.5 4区 材料科学 Pub Date : 2021-06-19 DOI: 10.1002/crat.202000243
L. Zhai, Zhaohua Zhang, Lihong Guo, Zhiying Zhu, Changkai Hu, Guimin Zhang
In this paper, two new Rivaroxaban crystalline forms are reported and characterized by the single‐crystal X‐ray diffraction (SXRD), powder X‐ray diffraction (PXRD), thermogravimetric analysis, and differential scanning calorimetry (TGA/DSC), which are synthesized with formic acid and acetic acid, named as forms F and G, respectively. The intermolecular forces for forms F and G are analyzed by Hirshfeld surface analysis method, showing that the force of O···H is significantly stronger than that of H···H. Furthermore, the stability, solubility, and bioavailability of the two crystal forms are also studied. The clinical experiments show that form F is more effective than other reported crystal forms in inhibiting the activity of thrombin and thrombosis, which is expected to replace the marketed crystalline forms in clinical application.
本文报道了两种新的利伐沙班结晶形式,并通过单晶X射线衍射(SXRD)、粉末X射线衍射(PXRD)、热重分析和差示扫描量热法(TGA/DSC)对其进行了表征,它们分别由甲酸和乙酸合成,命名为F型和G型。采用Hirshfeld表面分析方法对F和G的分子间作用力进行了分析,结果表明O··H的作用力明显强于H··H。此外,还研究了两种晶型的稳定性、溶解度和生物利用度。临床实验表明,F型在抑制凝血酶活性和血栓形成方面比其他已报道的晶体形式更有效,有望在临床应用中取代已上市的晶体形式。
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引用次数: 3
Analysis on Dielectric, Thermal, and Mechanical Characteristics of Nickel Boro Phthalate NLO Crystal for Optoelectronic Applications 光电用邻苯二甲酸镍NLO晶体介电、热、力学特性分析
IF 1.5 4区 材料科学 Pub Date : 2021-06-19 DOI: 10.1002/crat.202000247
M. Divya, P. Malliga, P. Sagayaraj, A. Joseph Arul Pragasam
Dielectric, thermal, and mechanical behavior of an efficient nonlinear crystal, nickel boro phthalate (NBP), grown by a slow evaporation solution growth technique, is characterized for optoelectronic applications. Ultraviolet absorption study identifies the lower cutoff wavelength as 281 nm. This low value along with transparency in the visible and infrared regions establishes that NBP is a probable nonlinear material. The frequency and the temperature dependency of dielectric constant and dielectric loss are probed. AC conductivity and activation energy are computed, to examine the semiconducting ability of the crystal. Thermal gravimetric analysis and differential thermal analysis are carried out to determine the decomposition temperature. Mechanical characterization is performed by the Vickers microhardness test. The study reveals that NBP comes under the category of soft material. Mechanical properties such as the elastic stiffness constant, brittleness index, yield strength, and fracture toughness are explored.
通过缓慢蒸发溶液生长技术生长的高效非线性晶体邻苯二甲酸镍(NBP)的介电、热学和力学行为具有光电子应用的特点。紫外吸收研究确定其下限截止波长为281 nm。这个低值以及可见光和红外区的透明度确定NBP可能是一种非线性材料。探讨了介电常数和介电损耗与频率和温度的关系。计算了晶体的交流电导率和活化能,考察了晶体的半导体性能。通过热重分析和差热分析确定了分解温度。力学特性是通过维氏显微硬度测试来完成的。研究表明,NBP属于软质材料。研究了弹性刚度常数、脆性指数、屈服强度和断裂韧性等力学性能。
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引用次数: 3
Various Molecular Arrangements Leading to Different Desolvation Rates: Research on the Stability of 2,7‐Dibromo‐9H‐carbazole Solvates 不同分子排列导致不同的脱溶速率:2,7 -二溴- 9H -咔唑溶剂化物的稳定性研究
IF 1.5 4区 材料科学 Pub Date : 2021-06-17 DOI: 10.1002/crat.202100059
Xuran Guo, Wei Chen, Rongli Wei, Jingchen Sui, Xin Huang, Na Wang, Songqiang Liu, Ting Wang, H. Hao
The stability of solvates is very important in the field of crystal engineering. Molecular interaction and packing mode are important factors affecting the stability of solvates. In this study, 2,7‐dibromo‐9H‐carbazole is selected as the model compound to investigate the influence of molecular stacking mode on the stability of solvates. An anhydrous form and five solvates of 2,7‐dibromo‐9H‐carbazole are obtained by recrystallization. The desolvation phenomena of the five solvates are studied by thermogravimetric analysis, hot stage microscope, and infrared spectroscopy and it is found that the stability of the solvates is N,N‐dimethylacetamide solvate > dimethyl sulfoxide solvate > N,N‐dimethylformamide solvate > dioxane solvate > acetonitrile solvate. Crystal structures are analyzed by single crystal X‐ray diffraction and Hirshfeld surface analysis is also applied to analyze the intermolecular interactions in the crystals. The results show that the stability of the five solvates is related to the packing modes of the molecules in the crystal. It is suggested that the solute molecules and solvent molecules in the unstable solvates are arranged in the interlayer mode, while they are arranged in a staggered mode in stable solvates.
溶剂化物的稳定性在晶体工程领域具有重要意义。分子间的相互作用和堆积方式是影响溶剂化物稳定性的重要因素。本研究选择2,7 -二溴- 9H -咔唑作为模型化合物,研究分子堆积方式对溶剂化物稳定性的影响。通过重结晶得到了2,7 -二溴- 9H -咔唑的无水形态和5种溶剂化物。通过热重分析、热级显微镜和红外光谱研究了5种溶剂化物的脱溶现象,发现溶剂化物的稳定性为N,N‐二甲基乙酰胺溶剂化物>二甲基亚砜溶剂化物> N,N‐二甲基甲酰胺溶剂化物>二氧环溶剂化物>乙腈溶剂化物。用单晶X射线衍射分析了晶体结构,并用Hirshfeld表面分析法分析了晶体中的分子间相互作用。结果表明,五种溶剂化物的稳定性与分子在晶体中的排列方式有关。结果表明,不稳定溶剂中溶质分子和溶剂分子呈层间模式排列,而稳定溶剂中溶质分子和溶剂分子呈交错模式排列。
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引用次数: 1
Amylopectin Regulated Mineralization of Calcium Carbonate and Its Application in Removing of Pb(II) 支链淀粉调控碳酸钙矿化及其在Pb(II)脱除中的应用
IF 1.5 4区 材料科学 Pub Date : 2021-06-15 DOI: 10.1002/crat.202100012
Qinjiang Zhao, Lihong Zhou, Jie Du, Guanghui Wang, X. Pei
As an ecological and environment‐friendly building material, sticky rice mortar has attracted the attention of many researchers. Amylopectin is the most important organic matter of it, which can improve the mechanical properties and durability of sticky rice mortar by inducing mineralization of calcium carbonate (CaCO3). However, amylopectin induced formation of CaCO3 has not been reported. In this paper, mineralization of CaCO3 induced by gelatinized amylopectin is investigated. For comparison, the different morphologies of CaCO3 are studied in the presence of Mg2+, Fe3+. Moreover, these CaCO3 products with different morphologies are used to clean the waste water. The results indicate that gelatinized amylopectin is conducive to formation of pumpkin‐like vaterite. It forms uniform rod and dumbbell‐shaped calcite in the presence of Mg2+, form calcite with stepped depressions in the presence of Fe3+. The adsorption of Pb(II) can reach extremely high level (1445.86 mg g−1) with the rod‐like calcite.
糯米砂浆作为一种生态环保的建筑材料,受到了众多研究者的关注。支链淀粉是糯米砂浆中最重要的有机物,支链淀粉通过诱导碳酸钙矿化来改善糯米砂浆的力学性能和耐久性。然而,支链淀粉诱导CaCO3的形成尚未见报道。本文研究了糊化支链淀粉对CaCO3矿化的影响。为了比较,研究了Mg2+、Fe3+存在下CaCO3的不同形貌。此外,这些不同形态的碳酸钙产品被用来净化废水。结果表明,糊化支链淀粉有利于南瓜样淀粉体的形成。在Mg2+存在下形成均匀的棒状和哑铃状方解石,在Fe3+存在下形成阶梯式凹陷方解石。棒状方解石对Pb(II)的吸附达到极高水平(1445.86 mg g−1)。
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引用次数: 6
Dislocation Etching Morphology on the A Plane of Sapphire Crystal 蓝宝石晶体A面位错蚀刻形貌研究
IF 1.5 4区 材料科学 Pub Date : 2021-06-12 DOI: 10.1002/crat.202100022
F. Cao, Fei Li, Zhiyong Yuan, Lunyong Zhang, Sida Jiang, Hongxian Shen, Z. Ning, Yongjiang Huang, D. Xing, H. Zuo, Jiecai Han, Jianfei Sun
In this work, the dislocation etching pit morphology and etching kinetics on the A‐{11 2¯ 0} plane of sapphire crystal (α‐Al2O3) are studied experimentally. The results show that the etch pit exhibits a subrhombic 3D morphology, which is consistent with the atom arrangement symmetry of the A plane. Further analysis shows that the two adjacent sides of the rhombic etch pits correspond to the directions [3 3¯ 0 1¯ ] and [3 3¯ 02], respectively; both of them are in the atomic close‐packing direction of A plane. The etch pits are controlled by a chemical reaction between Al2O3 and potassium hydroxide (KOH) with the reaction activation energy of 51.7 kJ mol−1, which is developed in a manner of kinematic wave by the step moving with a constant speed.
本文研究了蓝宝石晶体(α‐Al2O3)在A‐{11.2¯0}平面上的位错蚀刻坑形态和蚀刻动力学。结果表明,蚀坑呈现出亚菱形的三维形貌,符合a面原子排列的对称性。进一步分析表明,菱形蚀刻坑的两个相邻边分别对应于[3 3¯0 ~ 1¯]和[3 3¯02]方向;它们都在A平面的原子密排方向。蚀坑是由Al2O3与氢氧化钾(KOH)的化学反应控制的,反应活化能为51.7 kJ mol−1,反应活化能以等速阶跃运动的运动波形式发展。
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引用次数: 2
Synthesis and Characterization of TiC Nanofibers Obtained via a Modified Carbothermal Process 改性碳热法制备TiC纳米纤维的合成与表征
IF 1.5 4区 材料科学 Pub Date : 2021-06-07 DOI: 10.1002/crat.202000231
Chung‐Ying Tsai, K. Mondal
A simple method for synthesis of titanium carbide (TiC) nanofibers by a modified carbothermal reduction of electrospun titanium‐based fibers is reported. The effect of synthesis steps on the final product is discussed. Continuous TiC fibers synthesized have a smooth surface morphology, with average diameter of 148 nm and length in the centimeter range. X‐ray diffraction and high‐resolution transmission electron microscopy analysis results indicate that the fibers consist of TiC of high purity. Impact of heat treatment on the morphology and chemical and crystalline composition of the product is also investigated. Based on the experimental evidence, it is hypothesized that the carbothermal reduction of calcined electrospun fibers with precoated carbon proceeds through diffusion‐limited shrinking core pathway while that of the as‐spun fibers follows the reaction‐limited solution precipitation mechanism. The TiC nanofibers also show superior sintering properties by increasing theoretical density of hot pressed TiB2 from 94.5% of theoretical density to 97.9% of theoretical density. When sintered with ceria, it improves the conductivity of the ceria by 18.29 times as compared to 2.94 times by TiC nanoparticles at 800 °C. The TiC nanofibers show metallic behavior as well as potential for application as electrochemical double layer capacitor supercapacitors.
报道了一种以电纺钛基纤维为原料,经碳热还原改性合成碳化钛纳米纤维的简单方法。讨论了合成步骤对最终产物的影响。合成的连续TiC纤维表面形貌光滑,平均直径为148 nm,长度在厘米范围内。X射线衍射和高分辨率透射电镜分析结果表明,纤维中含有高纯度的TiC。研究了热处理对产品形貌、化学成分和结晶组成的影响。基于实验证据,假设预包覆碳电纺纤维的碳热还原是通过扩散-限制缩芯途径进行的,而预包覆碳电纺纤维的碳热还原是通过反应-限制溶液沉淀机制进行的。热压TiB2的理论密度从理论密度的94.5%提高到理论密度的97.9%,TiC纳米纤维表现出优异的烧结性能。在800℃烧结时,与TiC纳米颗粒相比,其电导率提高了2.94倍,而与二氧化铈烧结时,其电导率提高了18.29倍。TiC纳米纤维具有良好的金属性能,具有作为电化学双层电容超级电容器的应用潜力。
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引用次数: 0
Facile Synthesis, Crystal Structure, Spectral Characterization, Quantum Chemical Calculations, and Hirshfeld Surface Analysis of 5‐Chloro‐3‐Methoxy‐4‐Hydroxybenzaldehyde 5‐氯‐3‐甲氧基‐4‐羟基苯甲醛的易合成、晶体结构、光谱表征、量子化学计算和Hirshfeld表面分析
IF 1.5 4区 材料科学 Pub Date : 2021-06-04 DOI: 10.1002/crat.202100017
P. Nagapandiselvi
This article deals with synthesis, growth, structure, and characterization of 5‐chloro‐3‐methoxy‐4‐hydroxybenzaldehyde (5CMHBA or 5‐chlorovanillin) single crystals. A facile one‐pot method is employed for the chlorination of vanillin using N‐chlorosuccinimide. After chlorination, the single crystals of 5CMHBA are grown by slow evaporation solution growth technique. Grown crystals are subjected to single crystal X‐ray diffraction (SXRD), Fourier Transform Infrared (FTIR), and Thermogravimetric‐Differential Thermal Analysis (TG‐DTA). 5CMHBA crystallizes in the tetragonal crystal system with the space group P42/n. Vibrational characteristics are studied using FTIR. Further, thermal studies of the crystal are carried out using simultaneous TG‐DTA thermal analyzer. The molecular structure and its intermolecular interactions are studied by applying time–dependent density functional theory (TD‐DFT) using Gaussian 09 program and Hirshfeld surface analysis. A lesser energy gap of the 5CMHBA compared to that of vanillin shows the high reactivity of the molecule. Dipole moment, polarizability, and hyper‐polarizability are calculated in the molecular level and found to have greater polarizability than vanillin and also higher in order than that of standard urea molecule. This reveals the suitability of the molecule for nonlinear optical applications. The intermolecular interactions and porosity are analyzed and compared with vanillin and its polymorphs by Hirshfeld surface analysis.
本文研究了5‐氯‐3‐甲氧基‐4‐羟基苯甲醛(5CMHBA或5‐氯香草醛)单晶的合成、生长、结构和表征。用N -氯丁二酰亚胺进行香兰素的一锅氯化反应。氯化后,采用慢蒸发溶液生长技术生长出5CMHBA单晶。生长的晶体进行了单晶X射线衍射(SXRD),傅里叶变换红外(FTIR)和热重-差热分析(TG - DTA)。5CMHBA在空间群P42/n的四方晶系中结晶。用FTIR研究了其振动特性。此外,使用TG - DTA热分析仪对晶体进行了热研究。利用高斯09程序和Hirshfeld表面分析,应用时变密度泛函理论(TD‐DFT)研究了分子结构及其分子间相互作用。与香兰素相比,5CMHBA的能隙较小,表明该分子具有较高的反应活性。偶极矩、极化率和超极化率在分子水平上进行了计算,发现其极化率高于香兰素,也高于标准尿素分子。这揭示了该分子在非线性光学应用中的适用性。利用Hirshfeld表面分析法对其分子间相互作用和孔隙度进行了分析,并与香兰素及其多晶体进行了比较。
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引用次数: 0
Optimization of Substrate Temperature for Uniform Graphene Synthesis by Numerical Simulation and Machine Learning 基于数值模拟和机器学习的均匀石墨烯合成衬底温度优化
IF 1.5 4区 材料科学 Pub Date : 2021-06-04 DOI: 10.1002/crat.202100006
W. Deng, Yaosong Huang
High uniformity graphene has extensive application prospect in many important fields due to its excellent features. During large‐area graphene synthesis by chemical vapor deposition, the optimization of the substrate temperature can improve the uniformity of graphene. Here, machine learning is used to design and optimize the substrate surface temperature for uniform graphene deposition. The computational fluid dynamics simulations based on a developed computational model are first performed to obtain the training data for machine learning, such as the gas temperature, velocity, concentrations, etc. Then, the neural network model is used to optimize the substrate temperature using the simulated data. It is found that the high accuracy is achieved through the validation of testing set. The optimal substrate temperature distribution is finally obtained, in which the carbon deposition rate and its uniformity are optimized to the specified values.
高均匀性石墨烯以其优异的特性在许多重要领域具有广泛的应用前景。在化学气相沉积法大面积合成石墨烯过程中,优化衬底温度可以提高石墨烯的均匀性。在这里,机器学习被用于设计和优化衬底表面温度,以实现均匀的石墨烯沉积。首先基于建立的计算模型进行计算流体动力学模拟,获得气体温度、速度、浓度等机器学习训练数据。然后,利用仿真数据,利用神经网络模型对衬底温度进行优化。通过对测试集的验证,发现该方法具有较高的准确率。最终得到最优的衬底温度分布,其中积碳速率和均匀性优化到规定值。
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引用次数: 1
Masthead: Crystal Research and Technology 6'2021 报头:晶体研究与技术6'2021
IF 1.5 4区 材料科学 Pub Date : 2021-06-01 DOI: 10.1002/crat.202170021
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引用次数: 0
Highly Accurate Thickness Determination of 2D Materials (Crystal Research and Technology 6/2021) 高精度二维材料厚度测定(晶体研究与技术6/2021)
IF 1.5 4区 材料科学 Pub Date : 2021-06-01 DOI: 10.1002/crat.202170020
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引用次数: 1
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Crystal Research and Technology
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