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The Influence of Gravity on Single Crystallization in Large Volume Drops 重力对大体积液滴单晶化的影响
Pub Date : 2014-10-06 DOI: 10.4236/JCPT.2014.44025
I. Sandu, I. Iordache, C. Fleaca, F. Dumitrache, A.-M. Niculescu
The chemical, physical, and biological properties of more than two millions of proteins which follow to be synthesized by Pharmaceutical Industry, can be anticipated (by using their XRD diffrac-tograms) if they will be grown from aqueous drops as high quality, large volume single-crystals. This is not a simple task and usually the growing process is seen as art rather than a science. The growing is expensive, time consuming, and finally an amorphous aggregate may result instead one single-crystal. In this article, we show for the first time how one single crystal can be grown in large volume hanging drops through their fast evaporation. The single nucleation is determined by choosing the proper sense of gravitational force relative to the drop triple line contact. In a special configuration, single-crystals of glycine and threonine were rapidly grown.
如果将200多万种蛋白质从液滴中培养成高质量、大体积的单晶,那么它们的化学、物理和生物特性(通过使用它们的XRD衍射图)将被制药工业合成。这不是一项简单的任务,通常生长过程被视为艺术而不是科学。这种生长是昂贵的,耗时的,最后可能是一个无定形的聚集体,而不是一个单晶。在本文中,我们首次展示了单晶如何通过快速蒸发在大体积悬挂液滴中生长。单形核是通过选择相对于滴三线接触的适当的重力感来确定的。在一种特殊的结构中,甘氨酸和苏氨酸的单晶迅速生长。
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引用次数: 1
Synthesis and Characterization of Struvite-k Crystals by Agar Gel 鸟粪石-k晶体的琼脂凝胶合成与表征
Pub Date : 2014-10-06 DOI: 10.4236/JCPT.2014.44026
V. B. Suryawanshi, R. T. Chaudhari
The phosphate mineral struvite is basically formed in urinary tracks and kidney. One of the analogous compounds of struvite is potassium magnesium phosphate hexahydrate (KMgPO4·6H2O), known as struvite-k crystal and found in animal urinary calculi. In the present investigation, struvite-k crystals were grown by single diffusion and double diffusion techniques in agar gelmedium. The grown crystals were analyzed by optical microscopy, scanning electron microscopy (SEM), fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDXA) and thermogravimetric analysis (TGA). Optical microscopy and SEM exhibited the different morphologies. The FTIR spectra revealed the presence of water molecules, stretching and bending vibrations of phosphate (PO4) ions. However the powder XRD results from the crystalline nature. Elemental composition in the crystal was obtained by EDXA, while 36.89% weight loss of water molecules is observed in TGA study.
磷酸盐矿物鸟粪石主要在尿道和肾脏中形成。鸟粪石的一种类似化合物是六水磷酸钾镁(KMgPO4·6H2O),称为鸟粪石-k晶体,存在于动物尿路结石中。在本研究中,鸟粪石-k晶体采用单扩散和双扩散技术在琼脂凝胶培养基中生长。采用光学显微镜、扫描电镜(SEM)、傅里叶变换红外(FTIR)光谱、x射线衍射(XRD)、能量色散x射线分析(EDXA)和热重分析(TGA)对生长的晶体进行了分析。光学显微镜和扫描电镜显示出不同的形态。FTIR光谱显示了水分子的存在,以及磷酸(PO4)离子的拉伸和弯曲振动。粉末的XRD结果是结晶性的。EDXA法测定了晶体的元素组成,TGA法测定了水分子失重36.89%。
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引用次数: 17
Ceramic Nanocrystalline Superconductor Gadolinium Barium Copper Oxide (GdBaCuO) at Different Treating Temperatures 不同处理温度下陶瓷纳米晶超导体钆钡铜氧化物(GdBaCuO)
Pub Date : 2014-06-23 DOI: 10.4236/JCPT.2014.43021
V. Vinila, R. Jacob, Anusha Mony, H. Nair, Sheelakumari Issac, Sam Rajan, A. S. Nair, D. Satheesh, Jayakumari Isac
With the discovery of high-TC superconducting materials like Yttrium Barium Cupric Oxide, Bismuth Strontium Calcium Copper Oxide and Thallium Calcium Barium Copper Oxide, tremendous interest has developed over the past two years in understanding these materials as well as utilizing them in a variety of applications. The thin films of these materials are expected to play an important role in the area of microelectronics, especially for interconnects in integrated circuits, Josephson junctions, magnetic field sensors and optical detectors. Here, the authors designed a new nanocrystalline ceramic type II high-TC superconductor, Gadolinium Barium Copper Oxide (GdBaCuO/GBCO). The GBCO perovskite phase structure was prepared by the conventional solid state thermochemical reaction technique involving mixing, milling, calcination and sintering. In GBCO system, the method for controlling microstructure and superconducting state is related to oxygen content consideration because small changes in oxygen concentration can often lead to huge change in Tc. In order to show the viability of the proposed method, super-conducting powder was prepared in special furnace. The sample was analyzed by X-Ray Diffraction (XRD), an indispensible non-destructive tool for structural materials characterization and quality control which makes use of the Debye-Scherrer method. The comparison of XRD results with JCPDS files confirmed the orthorhombic structure of the sample. Micro-structural features are studied using Scanning Electron Microscopy (SEM) which revealed that its particle size is in the nanometer range. It also confirmed the calculated value of particle size from Debye Scherrer’s formula. EDX plot shows the presence of all the constituents. X-ray instrumental peak broadening analysis was used to evaluate the size and lattice strain by the Williamson-Hall Plot method.
随着高tc超导材料如钇钡铜氧化物、铋锶钙铜氧化物和铊钙钡铜氧化物的发现,在过去的两年里,人们对这些材料的理解以及在各种应用中利用它们产生了巨大的兴趣。这些材料的薄膜有望在微电子领域发挥重要作用,特别是在集成电路互连、约瑟夫森结、磁场传感器和光学探测器方面。在这里,作者设计了一种新的纳米晶陶瓷II型高tc超导体钆钡铜氧化物(GdBaCuO/GBCO)。采用混合、磨矿、煅烧、烧结等常规固相热化学反应技术制备了GBCO钙钛矿相结构。在GBCO体系中,控制微观结构和超导态的方法与氧含量有关,因为氧浓度的微小变化往往会导致Tc的巨大变化。为了证明该方法的可行性,在专用炉中制备了超导粉末。x射线衍射(XRD)是结构材料表征和质量控制不可缺少的非破坏性工具,利用Debye-Scherrer法对样品进行分析。XRD结果与JCPDS文件的比较证实了样品的正交结构。利用扫描电子显微镜(SEM)对其微观结构特征进行了研究,结果表明其粒径在纳米级范围内。同时也证实了Debye Scherrer公式计算出的粒径值。EDX图显示了所有成分的存在。采用Williamson-Hall图法,用x射线仪器峰展宽分析评价了材料的尺寸和晶格应变。
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引用次数: 10
Synthesis and X-Ray Structure of Important Anticancer Nucleosides Intermediate (2R,3S,4S,5R)-2-(acetoxymethyl)-5- (3-bromo-5-(methoxycarbonyl)- 1H-1,2,4-triazol-1-yl)tetrahydrofuran- 3,4-diyl Diacetate 重要抗癌核苷中间体(2R,3S,4S,5R)-2-(乙酰氧基甲基)-5-(3-溴-5-(甲氧基羰基)- 1h -1,2,4-三唑-1-基)四氢呋喃- 3,4-二乙酸二酯的合成和x射线结构
Pub Date : 2014-06-23 DOI: 10.4236/JCPT.2014.43018
Yang Liu, Guanghui Tian, Hongguang Ge, Xiaoyan Cao, Daihua Hu, Dehua Zhang
An important anticancer nucleosides intermediate (2R,3S,4S,5R)-2-(acetoxymethyl)-5-(3-bromo-5-(methoxycar-bonyl)-1H-1,2,4-triazol-1-yl)tetrahydrofuran-3,4-diyl diacetate was synthesized by directly coupling the bromotriazole with the protected ribose sugar, and have given the corresponding product in moderate yield. Its structure and conformation were confirmed by single crystal X-ray diffraction.
将溴三唑与受保护的核糖直接偶联,合成了重要的抗癌核苷中间体(2R,3S,4S,5R)-2-(乙酰氧基甲基)-5-(3-溴-5-(甲氧基羰基)- 1h -1,2,4-三唑-1-基)四氢呋喃-3,4-二乙酸二酯,并以中等产率得到了相应的产物。单晶x射线衍射证实了其结构和构象。
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引用次数: 2
Fluorite Phase Transformations under Vacuum 真空条件下萤石相变研究
Pub Date : 2014-06-23 DOI: 10.4236/JCPT.2014.43020
J. Mouhovski, O. Vitov, V. Dimov, B. Kostova, S. Gechev
Complex crystal aggregates from fluorspar vapor phase were grown at specific low-pressure/high-temperature conditions. The quasi-equilibrium of initiated crystal-chemical reactions at the proceeding vapour-crystal phase transformation was strongly dependent on the mass-transport inside an originally designed multicameral crucible, loaded by several portions of natural fluorite. By changing the temperature pressure over the already molten fluorspar portions as well as the gas-permeability of the channels connecting different sections in crucible interior to vacuum ambient, one may control the rate of gaseous-vapour diffusion and the degree of supper-saturation inside the peripheral crucible compartment wherein nucleation and crystal growing occurred. In this way, grown aggregates revealed a complicated habit formed during three-stage growing process provided by relevant thermodynamic and phase. Residual stresses were not observed in the aggregates whereas those in simultaneously grown boules from the non-vaporized melts in crucible cameras were clearly distinguished. The optical transmittance spectra of the boules were obtained considerably better, especially in the UV, comparing to those for crystal aggregates, both showing several peaks of specific light-absorption due to enhanced presence of rare-earth (RE) impurities. The aggregates manifest nearly full reflectivity from Vis to near IR region. The vapor phase growth mechanisms, when natural fluorite with some RE contents has been used, were explained on thermodynamic grounds that shown the manner of reliable control on the phenomenon. The results were anticipated to help for developing new perspective techniques for growth from vapor of several fluoride compounds with complex structure and composition and wide application. It was speculated that similar growth mechanisms of CaF2 crystals were possible on the moon in its very early period of formation.
在特定的低压/高温条件下,从萤石气相中生长出复杂的晶体聚集体。在气晶相变过程中引发的晶体化学反应的准平衡强烈依赖于原始设计的多组分坩埚内的质量输运,该坩埚由几部分天然萤石加载。通过改变已经熔化的萤石部分的温度压力,以及坩埚内部连接不同部分与真空环境的通道的透气性,可以控制气体-蒸气扩散的速度和坩埚外围室内发生成核和晶体生长的过饱和程度。由此可见,生长的骨料在发育过程中呈现出一种复杂的生长习性。在聚合体中没有观察到残余应力,而在坩埚摄像机中,从非汽化熔体中同时生长的气泡中可以清楚地分辨出残余应力。与晶体聚集体的透射光谱相比,获得了明显更好的光学透射光谱,特别是在紫外线下,由于稀土(RE)杂质的存在增强,两者都显示出几个特定光吸收峰。从可见光区到近红外区,聚集体表现出几乎完全的反射率。从热力学角度解释了含稀土的天然萤石的气相生长机理,指出了控制该现象的可靠方法。研究结果有望为开发结构组成复杂、应用广泛的氟化物气相生长新技术提供参考。据推测,在月球形成的早期,CaF2晶体的类似生长机制是可能的。
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引用次数: 0
Theoretical Model of Diffraction Line Profiles as Combinations of Gaussian and Cauchy Distributions 结合高斯分布和柯西分布的衍射线轮廓理论模型
Pub Date : 2014-06-23 DOI: 10.4236/JCPT.2014.43019
G. B. Mitra
Previously we derived equations determining line broadening in ax-ray diffraction profile due to stacking faults. Here, we will consider line broadening due to particle size and strain which are the other factors affecting line broadening in a diffraction profile. When line broadening in a diffraction profile is due to particle size and strain, the theoretical model of the sample under study is either a Gaussian or a Cauchy function or a combination of these functions, e.g. Voigt and Pseudovoigt functions. Although the overall nature of these functions can be determined by Mitra’s R(x) test and the Pearson and Hartley x test, details of a predicted model will be lacking. Development of a mathematical model to predict various parameters before embarking upon the actual experiment would enable correction of significant sources of error prior to calculations. Therefore, in this study, predictors of integral width, Fourier Transform, Second and Fourth Moment and Fourth Cumulant of samples represented by Gauss, Cauchy, Voigt and Pseudovoigt functions have been worked out. An additional parameter, the coefficient of excess, which is the ratio of the Fourth Moment to three times the square of the Second Moment, has been proposed. For a Gaussian profile the coefficient of excess is one, whereas for Cauchy distributions, it is a function of the lattice variable. This parameter can also be used for determining the type of distribution present in aggregates of distorted crystallites. Programs used to define the crystal structure of materials need to take this parameter into consideration.
先前我们推导了由于层错导致的x射线衍射剖面线展宽的方程。在这里,我们将考虑由于粒度和应变引起的线展宽,这是影响衍射剖面中线展宽的其他因素。当衍射剖面中的线增宽是由于粒度和应变引起的,所研究样品的理论模型是高斯函数或柯西函数或这些函数的组合,例如Voigt函数和Pseudovoigt函数。虽然这些函数的总体性质可以通过Mitra的R(x)检验和Pearson和Hartley x检验来确定,但预测模型的细节将缺乏。在进行实际实验之前,建立一个数学模型来预测各种参数,这将能够在计算之前纠正重要的误差来源。因此,在本研究中,研究了以高斯、柯西、Voigt和Pseudovoigt函数表示的样本的积分宽度、傅里叶变换、第二和第四矩和第四累积量的预测因子。提出了一个附加参数,超额系数,即第四矩与第二矩的平方的三倍之比。对于高斯分布,过剩系数为1,而对于柯西分布,过剩系数是晶格变量的函数。该参数也可用于确定畸变晶体聚集体中存在的分布类型。用于定义材料晶体结构的程序需要考虑这个参数。
{"title":"Theoretical Model of Diffraction Line Profiles as Combinations of Gaussian and Cauchy Distributions","authors":"G. B. Mitra","doi":"10.4236/JCPT.2014.43019","DOIUrl":"https://doi.org/10.4236/JCPT.2014.43019","url":null,"abstract":"Previously \u0000we derived equations determining line broadening in ax-ray diffraction profile \u0000due to stacking faults. Here, we will consider line broadening due to particle \u0000size and strain which are the other factors affecting line broadening in a \u0000diffraction profile. When line broadening in a diffraction profile is due to \u0000particle size and strain, the theoretical model of the sample under study is \u0000either a Gaussian or a Cauchy function or a combination of these functions, \u0000e.g. Voigt and Pseudovoigt functions. \u0000Although the overall nature of these functions can be determined by Mitra’s R(x) test and the Pearson and Hartley x test, details of a predicted model will be lacking. Development of a \u0000mathematical model to predict various parameters before embarking upon the \u0000actual experiment would enable correction of significant sources of error prior \u0000to calculations. Therefore, in this study, predictors of integral width, Fourier \u0000Transform, Second and Fourth Moment and Fourth Cumulant of samples represented \u0000by Gauss, Cauchy, Voigt and Pseudovoigt functions have been worked out. An \u0000additional parameter, the coefficient of excess, which is the ratio of the \u0000Fourth Moment to three times the square of the Second Moment, has been \u0000proposed. For a Gaussian profile the coefficient of excess is one, whereas for \u0000Cauchy distributions, it is a function of the lattice variable. This parameter \u0000can also be used for determining the type of distribution present in aggregates \u0000of distorted crystallites. Programs used to define the crystal structure of \u0000materials need to take this parameter into consideration.","PeriodicalId":64440,"journal":{"name":"结晶过程及技术期刊(英文)","volume":"4 1","pages":"145-155"},"PeriodicalIF":0.0,"publicationDate":"2014-06-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"70943277","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 3
Synthesis and X-Ray Structure of New Anticancer Nucleosides Based on 1-((2-Hydroxyethoxy)methyl)-5-(phenylthio)-1H-1,2,4-triazole-3-carboxamide 基于1-((2-羟基乙氧基)甲基)-5-(苯基硫)- 1h -1,2,4-三唑-3-羧酰胺抗癌核苷的合成及x射线结构
Pub Date : 2014-06-23 DOI: 10.4236/JCPT.2014.43017
Yu Lei, Dehua Zhang, Yang Liu, Guanghui Tian, Hongguang Ge
A pair of new anticancer nucleosides based on 1,2,4-triazole nucleosides and 1-((2-hydroxyethoxy) methyl)-5-(phenylthio)-1H-1,2,4-triazole-3-carboxamide have been synthesized, and have given the corresponding products in excellent yields. Its structures and conformations were confirmed by single crystal X-ray diffraction.
以1,2,4-三唑核苷和1-(2-羟基乙氧基)甲基)-5-(苯基硫代)- 1h -1,2,4-三唑-3-羧基酰胺为基础合成了一对新的抗癌核苷,并以优异的产率得到了相应的产物。单晶x射线衍射证实了其结构和构象。
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引用次数: 2
Reinvestigation of the Crystal Growth of “L-Proline Succinate” and “L-Threonine Zinc Acetate” Showing Use of Infrared Spectra for Product Identification “l -琥珀酸脯氨酸”和“l -苏氨酸醋酸锌”晶体生长的红外光谱再研究
Pub Date : 2014-04-03 DOI: 10.4236/JCPT.2014.42015
S. Natarajan, B. R. Srinivasan, K. Moovendaran
Reinvestigation of the growth of L-proline succinate (1) (Paramasivam and Ramachandra Raja, Journal of Crystallization Process and Technology, 2 (2012) 21 - 24; Balamurugaraj et al., Journal of Material Physics and Chemistry 1 (2013) 4 - 8) and L-threonine zinc acetate (2) (Puhal Raj and Ramachandra Raja, Photonics and Optoelectronics, 2 (2013) 56 - 64) is reported. Slow evaporation of an aqueous solution containing equimolar quantities of L-proline and succinic acid (for 1) and L-threonine and zinc acetate (for 2) results in the fractional crystallization of succinic acid (in the first case) and L-threonine (in the second case) and not any novel organic non-linear optical (NLO) crystals. In this paper, the usefulness of infrared spectra for correct product characterization is demonstrated.
l -琥珀酸脯氨酸生长的再研究(1)(Paramasivam and Ramachandra Raja, Journal of Crystallization Process and Technology, 2 (2012) 21 - 24;Balamurugaraj等人,材料物理与化学杂志1(2013)4 - 8)和l -苏氨酸醋酸锌(2)(Puhal Raj和Ramachandra Raja, Photonics and Optoelectronics, 2(2013) 56 - 64)的报道。缓慢蒸发含有等摩尔量的l -脯氨酸和琥珀酸(1)以及l -苏氨酸和醋酸锌(2)的水溶液会导致琥珀酸(第一种情况)和l -苏氨酸(第二种情况)的分式结晶,而不是任何新的有机非线性光学(NLO)晶体。本文证明了红外光谱对正确表征产品的有用性。
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引用次数: 4
Studies on Optical, Mechanical and Electrical Properties of Organic Nonlinear Optical p-Toluidine p-Toluenesulfonate Single Crystal 有机非线性光学对甲苯胺对甲苯磺酸单晶的光学、力学和电学性质研究
Pub Date : 2014-04-03 DOI: 10.4236/JCPT.2014.42013
S. Sagadevan, P. Murugasen
The optically transparent and bulk single crystal of p-Toluidine p-Toluenesulfonate (PTPT) was grown by slow evaporation technique. The lattice parameters and crystallinity of the grown crystal were estimated by single crystal XRD. The optical absorption of the crystal was recorded using the UV-Vis-NIR spectrophotometer. The optical bandgap and optical constants of the material were determined by using absorption spectrum. The refractive index of the grown crystal has been determined using the Brewster angle method. The dielectric constant and dielectric loss were measured as a function of frequency and temperature for the grown crystal. Nonlinear optical properties were performed to confirm the SHG efficiency of the grown crystal. Hence, PTPT is an excellent NLO material with enhanced SHG efficiency required for important applications in the field of optoelectronic and photonics. This material exhibits NLO behaviour remarkably due to its better optical and dielectric properties.
采用慢蒸发法制备了对甲苯胺对甲苯磺酸盐(PTPT)的光学透明块状单晶。利用单晶XRD分析了生长晶体的晶格参数和结晶度。用紫外-可见-近红外分光光度计记录晶体的光吸收。利用吸收光谱法测定了材料的光学带隙和光学常数。用布鲁斯特角法测定了生长晶体的折射率。测量了晶体的介电常数和介电损耗随频率和温度的变化规律。通过非线性光学特性来验证晶体的SHG效率。因此,PTPT是一种优秀的NLO材料,具有更高的SHG效率,在光电和光子学领域具有重要的应用。由于该材料具有较好的光学和介电性能,因此具有显著的NLO性能。
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引用次数: 8
Precipitation Behavior in Liesegang Systems under Microwave Irradiation 微波辐照下lieesegang体系的沉淀行为
Pub Date : 2014-04-03 DOI: 10.4236/JCPT.2014.42009
Y. Kanazawa, Y. Asakuma
We studied precipitation patterns in a Liesegang system under microwave irradiation in order to investigate metal salt diffusion in an electrolyte gel. The salt species and microwave irradiation power were varied. Microwave irradiation induced periodic patterns of precipitation because polar molecules vibrate and rotate in an electromagnetic field. For example, the number of patterns increased with the irradiation power. Accordingly, microwave irradiation nonlinearly accelerated the diffusion of ionic molecules.
为了研究金属盐在电解质凝胶中的扩散,我们研究了微波辐照下lieesegang体系中的沉淀模式。盐的种类和微波辐照功率不同。由于极性分子在电磁场中振动和旋转,微波照射诱导了周期性的降水模式。例如,图案数量随辐照功率的增加而增加。因此,微波辐射非线性地加速了离子分子的扩散。
{"title":"Precipitation Behavior in Liesegang Systems under Microwave Irradiation","authors":"Y. Kanazawa, Y. Asakuma","doi":"10.4236/JCPT.2014.42009","DOIUrl":"https://doi.org/10.4236/JCPT.2014.42009","url":null,"abstract":"We studied precipitation patterns in a Liesegang system under microwave irradiation in order to investigate metal salt diffusion in an electrolyte gel. The salt species and microwave irradiation power were varied. Microwave irradiation induced periodic patterns of precipitation because polar molecules vibrate and rotate in an electromagnetic field. For example, the number of patterns increased with the irradiation power. Accordingly, microwave irradiation nonlinearly accelerated the diffusion of ionic molecules.","PeriodicalId":64440,"journal":{"name":"结晶过程及技术期刊(英文)","volume":"04 1","pages":"65-70"},"PeriodicalIF":0.0,"publicationDate":"2014-04-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"70943073","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 4
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