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Research on growth mechanism of magnesium hydroxide crystal thin films based on hydrothermal system 基于水热体系的氢氧化镁晶体薄膜生长机理研究
IF 1.7 4区 材料科学 Q3 CRYSTALLOGRAPHY Pub Date : 2024-06-29 DOI: 10.1016/j.jcrysgro.2024.127810
Limei Bai , Meijia Wang , Xiaozheng Liang , Wenqing Zhao , Shujuan Dai

Thin film crystal materials have excellent properties such as a fine-scale structure, high strain strength, and flame retardancy. In this work, the preparation of magnesium hydroxide thin films was achieved by analyzing the main exposed groups on the surface of magnesium hydroxide and utilizing self-assembly film technology in a hydrothermal system with triethanolamine as a crystal additive. By combining experimental and simulation calculations, the study explored the alterations in morphology and growth mode of magnesium hydroxide thin films, the adsorption of triethanolamine on different crystal surfaces of magnesium hydroxide, and the control of magnesium hydroxide crystal growth by dynamically adjusting growth unit diffusion in the system under the influence of triethanolamine concentration. The results showed that the addition of triethanolamine increased the concentration of OH ions in the solution, facilitating the adsorption of Mg(OH)64− growth units on the (1 0 1) surface with more Mg-O bonds. This allows the magnesium hydroxide (1 0 1) crystal surface to serve as tangential growth drivers for the system, the normal growth of the crystal surface transitions to tangential extension, promoting the gradual expansion of the hexagonal wafer into crystal films. The regrowth mechanism of magnesium hydroxide thin films promotes the regrowth of crystals under hydrothermal conditions, and realizes the high value-added utilization of magnesite resources.

薄膜晶体材料具有结构细腻、应变强度高、阻燃等优良特性。本研究通过分析氢氧化镁表面的主要暴露基团,在水热体系中利用自组装成膜技术,以三乙醇胺为晶体添加剂,实现了氢氧化镁薄膜的制备。研究结合实验和模拟计算,探讨了氢氧化镁薄膜形貌和生长方式的改变、三乙醇胺在氢氧化镁不同晶面上的吸附情况,以及在三乙醇胺浓度影响下,通过动态调节生长单元在体系中的扩散来控制氢氧化镁晶体的生长。结果表明,三乙醇胺的加入增加了溶液中 OH- 离子的浓度,有利于 Mg(OH)64- 生长单元吸附在具有更多 Mg-O 键的(1 0 1)表面上。这使得氢氧化镁(1 0 1)晶体表面成为体系的切向生长驱动力,晶体表面的正常生长过渡到切向延伸,促进六边形晶片逐渐扩展成晶体薄膜。氢氧化镁薄膜的再生长机制促进了水热条件下晶体的再生长,实现了菱镁矿资源的高附加值利用。
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引用次数: 0
Effects of coil frequency on the carbon transport in the top-seeded solution growth of SiC single crystal 线圈频率对碳化硅单晶顶籽溶液生长过程中碳迁移的影响
IF 1.7 4区 材料科学 Q3 CRYSTALLOGRAPHY Pub Date : 2024-06-22 DOI: 10.1016/j.jcrysgro.2024.127801
Yuhui Liu, Mengyu Li, Zhaoyang Yan, Xiaofang Qi, Wencheng Ma, Jianli Chen, Yongkuan Xu, Zhanggui Hu

The flow pattern and carbon transport in the solution for the solution growth of silicon carbide (SiC) in an induction-heating system can be effectively controlled by adjusting the coil frequency to obtain a relatively uniform distribution of growth rate. In this paper, a global heat and mass transfer model was first verified by the SiC crystal growth experiment results at the coil frequency of 8 kHz. Then, the influence of coil frequency on the fluid flow, carbon concentration, and growth rate for the growth of SiC crystals was numerically investigated. The results indicated that electromagnetic convection (at low frequencies) greatly enhances the upward convection beneath the crystal and weakens the adverse effects of Marangoni convection, resulting in a uniform distribution of radial temperature along the growth interface. Consequently, the carbon transport from the crucible wall to the crystal center is strengthened, leading to a uniform region of high carbon supersaturation with a lower coil frequency. The optimal radial uniformity of the growth rate along the growth interface is achieved at the coil frequency of 3 kHz.

在感应加热系统中进行碳化硅(SiC)溶液生长时,溶液中的流动模式和碳传输可通过调节线圈频率得到有效控制,从而获得相对均匀的生长率分布。本文首先通过 8 kHz 线圈频率下 SiC 晶体生长实验结果验证了全局传热和传质模型。然后,对 SiC 晶体生长过程中线圈频率对流体流动、碳浓度和生长率的影响进行了数值研究。结果表明,电磁对流(低频)大大增强了晶体下方的向上对流,减弱了马兰戈尼对流的不利影响,从而导致沿生长界面的径向温度分布均匀。因此,从坩埚壁到晶体中心的碳传输得到加强,从而以较低的线圈频率形成均匀的高碳过饱和区域。当线圈频率为 3 kHz 时,沿生长界面的生长率达到最佳径向均匀性。
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引用次数: 0
The effects of processing technique on formation temperature of calcium aluminate magnesium (CaO.2MgO.8Al2O3) 加工技术对铝酸钙镁(CaO.2MgO.8Al2O3)形成温度的影响
IF 1.7 4区 材料科学 Q3 CRYSTALLOGRAPHY Pub Date : 2024-06-20 DOI: 10.1016/j.jcrysgro.2024.127797
Sahar Sajjadi Milani, Mahdi Ghassemi Kakroudi, Mohammad Rezvani

This study aims at the synthesis of a ternary phase crystal CaO.2MgO.8Al2O3 (CM2A8) in the Al-rich part of the ternary system CaO-Al2O3-MgO through two techniques: (1) sol–gel citrate and (2) solid-state reaction. Based on the measurement of particle size, density, phase analysis, nature of bounds, and microscopic observation, the effect of the processing technique on the crystal purity, crystallite size, and synthesis temperature of the as-prepared CM2A8 powder was investigated. Phases analysis (XRD patterns) showed in the sol–gel citrate combustion method almost a single-phase material (calcium aluminate magnesium phases) at relatively lower temperatures while in the solid-state method as-prepared CM2A8 powder with a small amount of spinel (MgAl2O4 = MA) and calcium hexaaluminate (CaAl12O19 = CA6) secondary phases. The generated heat through the combustion of the reaction of ammonium nitrate and citrate-based complexes decreases the synthesis temperature of nanocrystalline CM2A8, and the CM2A8 phase is formed at a temperature of 1400 °C. While growth mechanism in the solid-state reaction method adheres to the two-dimensional nucleation theory and a thick hexagonal flake known as CM2A8 is produced at a temperature of 1700 °C. In comparison with the crystals synthesized by the solid-state reaction method, the powder density of the nanocrystals synthesized by a sol–gel combustion method exhibits higher values (3.54 g.cm−3 and 3.65 g.cm−3, respectively). Peak intensities in the 400–1000 cm−1 range, according to FTIR measurements, correspond to metal–oxygen–metal (M–O–M) bonds (vibrations of Al–O stretching in Mg–O–Al and Ca–O–Al), and they grow as the temperature rises from 200 °C to 1400 °C, indicating that CM2A8 was the crystal that was formed. The morphological analysis (FESEM) revealed that most of the agglomerate particles synthesized by the sol–gel citrate combustion remained within the range of 50–83 nm, while the particles synthesized by the had particles as 1 μm. The specific surface area synthesized CM2A8 via the sol–gel method is in the range of 10–24 m2/g. The main advantages of the sol–gel citrate process are the high purity of the product, the narrow particle size distribution, and the achievement of uniform nanostructure at low temperatures.

本研究旨在通过(1)溶胶-凝胶柠檬酸盐和(2)固态反应两种技术合成 CaO-Al2O3-MgO 三元体系富铝部分的三元相晶体 CaO.2MgO.8Al2O3(CM2A8)。在测量粒度、密度、相分析、边界性质和显微观察的基础上,研究了加工技术对制备的 CM2A8 粉末的晶体纯度、晶粒尺寸和合成温度的影响。相分析(XRD 图谱)显示,在溶胶-凝胶柠檬酸盐燃烧法中,在相对较低的温度下几乎是单相材料(钙铝酸盐镁相),而在固态法中,制备的 CM2A8 粉末含有少量尖晶石(MgAl2O4 = MA)和六铝酸钙(CaAl12O19 = CA6)次生相。硝酸铵和柠檬酸基络合物反应燃烧产生的热量降低了纳米晶 CM2A8 的合成温度,CM2A8 相在 1400 ℃ 的温度下形成。固态反应法的生长机理遵循二维成核理论,在 1700 ℃ 的温度下生成了被称为 CM2A8 的厚六边形薄片。与固态反应法合成的晶体相比,溶胶-凝胶燃烧法合成的纳米晶体的粉末密度值更高(分别为 3.54 g.cm-3 和 3.65 g.cm-3)。根据傅立叶变换红外光谱测量,400-1000 cm-1 范围内的峰强度对应于金属-氧-金属(M-O-M)键(Mg-O-Al 和 Ca-O-Al 中 Al-O 的伸展振动),它们随着温度从 200 °C 升至 1400 °C 而增长,表明形成的晶体是 CM2A8。形态分析(FESEM)显示,溶胶-凝胶柠檬酸盐燃烧法合成的团聚颗粒大部分保持在 50-83 nm 的范围内,而合成法合成的颗粒为 1 μm。通过溶胶-凝胶法合成的 CM2A8 的比表面积在 10-24 m2/g 之间。溶胶-凝胶柠檬酸盐工艺的主要优点是产品纯度高、粒度分布窄、可在低温下获得均匀的纳米结构。
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引用次数: 0
Piezoelectric temperature acoustic sensor of LiNbO3 crystal fibers operating at radio frequencies 在无线电频率下工作的铌酸锂晶体纤维压电温度声学传感器
IF 1.7 4区 材料科学 Q2 Physics and Astronomy Pub Date : 2024-06-19 DOI: 10.1016/j.jcrysgro.2024.127799
Francisco Enilton Alves Nogueira , Raphael Victor Barros Campos , João Paulo Costa do Nascimento , Felipe Felix do Carmo , Marcelo Antonio Santos da Silva , Sergio Paulo Marcondes , Antonio Carlos Hernandes , Antonio Sergio Bezerra Sombra

This study focuses on the growth and characterization of crystalline LiNbO3 (LN) piezoelectric fibers pulled by the Laser Heated Pedestal Growth (LHPG) technique. The electrical properties of the fibers were investigated using an impedance analyzer, which yielded values for resonance frequency, anti-resonance frequency, and phase angle. Subsequently, elastic constants and coupling factor were determined through calculations based on thickness resonance modes. The accuracy of the resonance method was validated through numerical simulations utilizing COMSOL software, demonstrating a close agreement between experimental and simulated results. Additionally, a temperature sensing was conducted, subjecting the fibers to a wide temperature range from 30 °C to 236 °C to assess their sensitivity to temperature variations. The coupling factors of K = 0.37 for LN-1 and K = 0.35 for LN-2 demonstrated efficient performance of the crystalline fibers. Furthermore, the numerical simulations exhibited strong correlation between simulated and experimental data. The sensitivity analysis revealed the potential of LN fibers for temperature sensor applications, exhibiting a sensitivity of −87 Hz.°C−1. These findings underscore the promise of LN piezoelectric fibers in advanced sensing technologies.

本研究的重点是通过激光加热台架生长(LHPG)技术拉制晶体铌酸锂(LN)压电纤维的生长和表征。使用阻抗分析仪研究了纤维的电气特性,得出了共振频率、反共振频率和相位角的值。随后,通过基于厚度共振模式的计算确定了弹性常数和耦合因子。利用 COMSOL 软件进行的数值模拟验证了共振方法的准确性,表明实验结果与模拟结果非常接近。此外,还进行了温度传感,将纤维置于 30 °C 至 236 °C 的宽温度范围内,以评估其对温度变化的敏感性。LN-1 和 LN-2 的耦合系数分别为 K = 0.37 和 K = 0.35,这表明结晶光纤具有高效的性能。此外,数值模拟显示模拟数据与实验数据之间具有很强的相关性。灵敏度分析显示了 LN 纤维在温度传感器应用方面的潜力,其灵敏度为 -87 Hz.°C-1。这些发现强调了 LN 压电纤维在先进传感技术中的应用前景。
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引用次数: 0
“Efficacy of datura metel leaf extract on MnSrO2 NPs synthesized using a green method in terms of pollutant reduction and antimicrobial activity.” "用绿色方法合成的 MnSrO2 NPs 在减少污染物和抗菌活性方面的功效"。
IF 1.8 4区 材料科学 Q2 Physics and Astronomy Pub Date : 2024-06-17 DOI: 10.1016/j.jcrysgro.2024.127796
Prathap A. , H.S. Bhojya Naik , R. Viswanath , Maruthi Nayaka T.H. , Kotresh K.R.

In this work, we prepared both chemical and biogenic synthesis of MnSrO2 (0, 5, 20 ml DLE) nanoparticles using datura metel leaf extraction by co-precipitation method and also prepared Sulfadiazine dye for catalytic activity. The applications and properties of green MnSrO2 nanoparticles have compared and they were characterized via XRD, SEM, FT-IR, EDX, UV–visible, and PL techniques. These nanoparticles showed an 18–8 nm diameter range, which was arranged in a spherical form combined randomly. The evidence from FTIR spectra showed peaks around 492, 487, 483, 655, 606, and 603 cm−1 for the creation of SrMnO2 NPs. Antibacterial activity of MnSrO2 (0, 5, 20 ml DLE) was measured by the well-diffusion method against pathogens, Staphylococcus aureus and Klebsiella pneumonia. The photocatalytic activity of the synthesized metal oxide nanoparticles was investigated by UV–visible spectroscopy for Sulfadiazine dye degradation with bare MnSrO2 NPs, g-MnSrO2 NPs [5 ml DLE], and g-MnSrO2 NPs [20 ml DLE] in presence of visible light irradiation.

在这项工作中,我们采用共沉淀法,利用达图拉叶提取物制备了化学和生物合成的 MnSrO2 纳米粒子(0、5、20 ml DLE),并制备了磺胺嘧啶染料用于催化活性。通过 XRD、SEM、FT-IR、EDX、UV-visible 和 PL 技术对绿色 MnSrO2 纳米粒子的应用和特性进行了比较和表征。这些纳米粒子的直径范围为 18-8 纳米,呈球形随机组合排列。傅立叶变换红外光谱显示,SrMnO2 NPs 在 492、487、483、655、606 和 603 cm-1 附近出现峰值。采用井扩散法测定了 MnSrO2(0、5、20 ml DLE)对病原体金黄色葡萄球菌和肺炎克雷伯菌的抗菌活性。在可见光照射下,用紫外可见光谱研究了裸 MnSrO2 NPs、g-MnSrO2 NPs [5 ml DLE] 和 g-MnSrO2 NPs [20 ml DLE] 降解磺胺嘧啶染料的光催化活性。
{"title":"“Efficacy of datura metel leaf extract on MnSrO2 NPs synthesized using a green method in terms of pollutant reduction and antimicrobial activity.”","authors":"Prathap A. ,&nbsp;H.S. Bhojya Naik ,&nbsp;R. Viswanath ,&nbsp;Maruthi Nayaka T.H. ,&nbsp;Kotresh K.R.","doi":"10.1016/j.jcrysgro.2024.127796","DOIUrl":"https://doi.org/10.1016/j.jcrysgro.2024.127796","url":null,"abstract":"<div><p>In this work, we prepared both chemical and biogenic synthesis of MnSrO<sub>2</sub> (0, 5, 20 ml DLE) nanoparticles using <em>datura metel</em> leaf extraction by co-precipitation method and also prepared Sulfadiazine dye for catalytic activity. The applications and properties of green MnSrO<sub>2</sub> nanoparticles have compared and they were characterized via XRD, SEM, FT-IR, EDX, UV–visible, and PL techniques. These nanoparticles showed an 18–8 nm diameter range, which was arranged in a spherical form combined randomly. The evidence from FTIR spectra showed peaks around 492, 487, 483, 655, 606, and 603 cm<sup>−1</sup> for the creation of SrMnO<sub>2</sub> NPs. Antibacterial activity of MnSrO<sub>2</sub> (0, 5, 20 ml DLE) was measured by the well-diffusion method against pathogens, <em>Staphylococcus aureus</em> and <em>Klebsiella pneumonia</em>. The photocatalytic activity of the synthesized metal oxide nanoparticles was investigated by UV–visible spectroscopy for Sulfadiazine dye degradation with bare MnSrO<sub>2</sub> NPs, g-MnSrO<sub>2</sub> NPs [5 ml DLE], and g-MnSrO<sub>2</sub> NPs [20 ml DLE] in presence of visible light irradiation.</p></div>","PeriodicalId":353,"journal":{"name":"Journal of Crystal Growth","volume":null,"pages":null},"PeriodicalIF":1.8,"publicationDate":"2024-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141428724","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Numerical study on gas reaction path of InN-MOVPE with three typical reactors 使用三种典型反应器对 InN-MOVPE 的气体反应路径进行数值研究
IF 1.7 4区 材料科学 Q2 Physics and Astronomy Pub Date : 2024-06-17 DOI: 10.1016/j.jcrysgro.2024.127798
Guangyu Zheng , Yukang Sun , Hong Zhang , Peng Su , Ran Zuo , Lijun Liu

This study investigates the controversies about the gas-phase reaction path in the InN MOVPE process. Numerical modeling of the reaction-transport processes in three typical reactors was conducted for main reaction paths. By comparisons of the molar concentrations of the major In-containing species, it was determined that the different approaches of the gas mixing and heating led to three distinct reaction paths. When the non-premixed gas precursors are heated very fast upon entering the reactor, the adduct/amide formation path predominates and the pyrolysis path is negligible (Path 1). When the precursors are mixed at room temperature and heated gradually, the adduct TMIn:NH3 dissociates back into TMIn, with the pyrolysis path dominating. However, the formation of amides DMInNH2 intensifies the generation of nanoparticles (Path 2). When mixing occurs at warm temperature and heated fast, both the pyrolysis and adduct paths co-exist, but their effects are different (path 3). In the CCS reactor the dominant reaction path will be Path 1, while in the vertical reactor with a greater height, Path 2 is predominant. In the pre-mixed horizontal reactor, Path 3 is dominant, the pyrolysis path forms a competition with the adduct path near the substrate, and the adduct path dominating at the top of the reactor.

本研究调查了有关 InN MOVPE 工艺中气相反应路径的争议。针对主要反应路径,对三个典型反应器中的反应-传输过程进行了数值建模。通过比较主要含 In 物种的摩尔浓度,确定了不同的气体混合和加热方法会导致三种不同的反应路径。当未预混合的气体前驱体进入反应器后被快速加热时,加成物/酰胺的形成路径占主导地位,而热解路径可以忽略不计(路径 1)。当前驱体在室温下混合并逐渐加热时,加合物 TMIn:NH3 会解离回 TMIn,热解路径占主导地位。然而,酰胺 DMInNH2 的形成会加剧纳米粒子的生成(路径 2)。当在高温和快速加热条件下进行混合时,热解和加成途径同时存在,但它们的效果不同(途径 3)。在 CCS 反应器中,主要的反应路径是路径 1,而在高度较大的垂直反应器中,路径 2 是主要的。在预混合水平反应器中,路径 3 占主导地位,热解路径与基质附近的加成路径形成竞争,加成路径在反应器顶部占主导地位。
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引用次数: 0
Holmium-doped TbVO4 as a highly potential magneto-optical crystal for Faraday isolator 掺钬 TbVO4 作为一种极具潜力的磁光晶体用于法拉第隔离器
IF 1.8 4区 材料科学 Q2 Physics and Astronomy Pub Date : 2024-06-15 DOI: 10.1016/j.jcrysgro.2024.127795
Wenyu He, Hu Liu, Ziqi Guo, Xianchao Zhu

Tb1-xHoxVO4 (THV) magneto-optical crystal with diameter of 27 mm and length of 40 mm was grown by the Czochralski (Cz) technique for the first time. The structural perfection of THV crystal was studied by the high-resolution X-ray diffraction rocking curve measurement, proving the high crystallinity quality of THV. THV shows high transmittance of greater than 75 % within the wavelength range of 665–1600 nm. The Verdet constants of THV at 532, 633 and 1064 nm are 370, 226 and 56 rad·m−1T−1, 40 %–95 % higher than these of commercial TGG crystal. Additionally, THV exhibits lower absorption coefficient (0.05 cm−1), higher magneto-optical figure of merit (175 deg/dB) and extinction ratio (43 dB) at 1064 nm compared with TGG. Evaluation of thermal performance and laser-induced damage threshold of THV were also made to promote the potential application in high-power optical isolators.

首次采用 Czochralski(Cz)技术生长出直径为 27 毫米、长度为 40 毫米的 Tb1-xHoxVO4 (THV)磁光学晶体。通过高分辨率 X 射线衍射摇摆曲线测量研究了 THV 晶体的完美结构,证明了 THV 晶体的高结晶性。在 665-1600 纳米波长范围内,THV 的透射率大于 75%。THV 在 532、633 和 1064 纳米波长的维尔德常数分别为 370、226 和 56 rad-m-1T-1,比商用 TGG 晶体的维尔德常数高 40%-95%。此外,与 TGG 相比,THV 在 1064 纳米波长处的吸收系数(0.05 cm-1)更低、磁光系数(175 deg/dB)和消光比(43 dB)更高。此外,还对 THV 的热性能和激光诱导损伤阈值进行了评估,以促进其在大功率光隔离器中的潜在应用。
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引用次数: 0
Ce3+ ion-induced distortion in a perovskite-structured KMgF3 single crystal 包晶结构 KMgF3 单晶中由 Ce3+ 离子诱发的畸变
IF 1.7 4区 材料科学 Q3 CRYSTALLOGRAPHY Pub Date : 2024-06-13 DOI: 10.1016/j.jcrysgro.2024.127787
Mayrene A. Uy , Angelo P. Rillera , Keito Shinohara , Melvin John F. Empizo , Toshihiko Shimizu , Kohei Yamanoi , Akira Yoshikawa , Nobuhiko Sarukura , Hitoshi Abe

We investigate the local structural distortion induced by

ion in a (cubic) perovskite-structured KMgF3 crystal for potential vacuum ultraviolet (VUV) applications. The crystal with 1.0 mol% nominal doping concentration exhibits five absorption bands centered at 196, 203, 209, 227, and 233 nm and two emission bands centered at 266 and 282 nm. These absorption and emission bands are attributed to the 4f5d transitions of the
ion. Our Ce K- and
-edge XAS analyses confirm the presence of
oxidation state in the KMgF3 crystal. Our analyses reveal a significantly distorted coordination environment which has a coordination number (CN) of 5.03±0.55 and an average Ce–F bond length of 2.44±0.01 Å. Strong mixing of the 4f and 5d states and large ligand-field effects are also implied in the Ce
-edge XANES spectrum, as evidenced by an intense pre-edge peak. Optically, these mixing and ligand field effects conform to the large crystal field splitting of 1.03 eV (8285
). Although this was the case,
-doped KMgF3 remains a candidate VUV optical material due to its small Stokes shift of 0.64eV (5141
).

我们研究了离子在(立方)包晶石结构的 KMgF3 晶体中引起的局部结构畸变,该晶体具有潜在的真空紫外线(VUV)应用前景。标称掺杂浓度为 1.0 摩尔的晶体显示出以 196、203、209、227 和 233 纳米为中心的五个吸收带和以 266 和 282 纳米为中心的两个发射带。这些吸收带和发射带归因于离子的 4f-5d 转变。我们的 Ce K- 和 - 边 XAS 分析证实了 KMgF3 晶体中存在氧化态。我们的分析揭示了一个明显扭曲的配位环境,其配位数(CN)为 5.03±0.55,Ce-F 键的平均长度为 2.44±0.01 Å。4f 和 5d 态的强烈混合和巨大的配体场效应也隐含在 Ce -edge XANES 光谱中,一个强烈的前沿峰就是证明。从光学角度来看,这些混合效应和配体场效应与 1.03 eV 的大晶体场分裂(8285)相一致。尽管如此,掺杂的 KMgF3 仍然是一种候选的紫外光学材料,因为它的斯托克斯位移很小,只有 0.64eV (5141 )。
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引用次数: 0
X-ray computed tomography for 3D crystallization monitoring: A use case with paracetamol 用于三维结晶监测的 X 射线计算机断层扫描:扑热息痛应用案例
IF 1.7 4区 材料科学 Q2 Physics and Astronomy Pub Date : 2024-06-13 DOI: 10.1016/j.jcrysgro.2024.127794
Sébastien Clercq , Jérôme Vicente , Philippe Moulin

This work highlights the capabilities and limits of X-ray computed tomography in crystallization monitoring through a use case involving paracetamol as the solute, recrystallized from ethanol, methanol, or a mixture of both. The cooling crystallization operation was set up in two different containers, prepared with cotton yarns stretched vertically, acting as linear nucleation sites that immobilize the grown crystals in the recording area. The largest container (10 mL test tubes) allowed the acquisition of a larger number of crystals (up to 300 particles) for a more appropriate bulk analysis. The smallest container (5 mL pipette tips) allowed for a finer resolution of the recorded solid phase at the expense of a reduced recording volume. Crystallization was monitored in terms of the number of individual crystals, their size, and the overall volume, thus leading to the nucleation and growth rates, and solid-phase production rate. The main benefit of X-ray computed tomography is in the 3D analysis of the reconstructed solid phase. The crystal habit of paracetamol form I was predicted using force-field modeling. The predicted habit was in great accordance with the reconstructed solids, confirming the polymorphic form. Furthermore, face-specific growth rates of reconstructed crystals were measured, paving the way for a novel approach to the investigation of crystal-solvent interactions.

这项研究通过一个以扑热息痛为溶质,从乙醇、甲醇或两者的混合物中重结晶的应用案例,强调了 X 射线计算机断层扫描技术在结晶监测方面的能力和局限性。冷却结晶操作在两个不同的容器中进行,容器中的棉纱垂直拉伸,作为线性成核点,将生长的晶体固定在记录区域。最大的容器(10 mL 试管)可以采集更多的晶体(多达 300 个颗粒),以便进行更适当的批量分析。使用最小的容器(5 mL 移液器吸头)可获得更精细的固相记录分辨率,但记录体积有所减少。根据单个晶体的数量、大小和总体积监测结晶情况,从而得出成核率、生长率和固相生成率。X 射线计算机断层扫描的主要优势在于对重建的固相进行三维分析。利用力场模型预测了扑热息痛 I 型的晶体习性。预测的习性与重建的固相非常吻合,证实了其多晶形态。此外,还测量了重建晶体的特定面生长率,为研究晶体与溶剂的相互作用铺平了道路。
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引用次数: 0
Growth of AlGaN alloys with ∼ 90 % AlN mole fraction by plasma-assisted molecular beam epitaxy: Indication of phase-segregation effects 通过等离子体辅助分子束外延生长 AlGaN 摩尔分数为 90% 的 AlGaN 合金:相分离效应的迹象
IF 1.8 4区 材料科学 Q2 Physics and Astronomy Pub Date : 2024-06-13 DOI: 10.1016/j.jcrysgro.2024.127792
Pushan Guha Roy , Sayantani Sen , Chirantan Singha , Anirban Bhattacharyya

AlGaN alloys with very high AlN mole fraction (∼90 %) were grown by plasma-assisted molecular beam epitaxy (PA-MBE) and their alloy properties were investigated by high-resolution X-ray diffraction (HR-XRD) measurements. Growth was carried out employing a series of group III/V ratios and for samples grown under a high group-III regime, phase-segregation in the alloy was evident from a characteristic splitting of the AlGaN (0002) peak in the HR-XRD pattern. With decreasing excess group-III conditions the separation of peak positions continuously reduced, till a single peak was observed. However, for samples where such splitting was absent, spontaneous superlattice peaks were seen at lower incident angles of the XRD patterns indicating the presence of long-range atomic ordering (LRAO). Thus, for AlGaN alloys with extremely high Al content, effects of phase-segregation, or of LRAO were observed, depending on the kinetics of growth. These results on phase-segregation effects are expected to promote the development of high-efficiency deep ultraviolet emitters for skin-safe germicidal action by mitigating the detrimental effect of dislocations and related non-radiative recombination centers through carrier localization processes at potential minima.

通过等离子体辅助分子束外延(PA-MBE)生长出了具有极高 AlN 分子分数(∼ 90 %)的 AlGaN 合金,并通过高分辨率 X 射线衍射(HR-XRD)测量研究了其合金特性。生长过程采用了一系列 III/V 族比,对于在高 III 族条件下生长的样品,合金中的相分离从 HR-XRD 图形中 AlGaN (0002) 峰的特征性分裂中显而易见。随着 III 族过量条件的降低,峰位置的分离不断减小,直至观察到单一峰。然而,对于不存在这种分离的样品,在 XRD 图样的较低入射角处可以看到自发的超晶格峰,这表明存在长程原子有序(LRAO)。因此,对于铝含量极高的 AlGaN 合金,根据生长动力学的不同,可以观察到相分离或 LRAO 的影响。这些关于相分离效应的研究结果有望通过载流子在电位极小值处的定位过程,减轻位错和相关非辐射重组中心的有害影响,从而促进高效深紫外发射器的开发,达到皮肤安全杀菌的目的。
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Journal of Crystal Growth
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