Synthesis and crystal structures of novel glycoluril carboxylic acids conglomerates

The two novel conglomerates were obtained by crystallization of racemic (2'S,3aS,6aR)/(2'R,3aR,6aS) (glycoluril-1-yl)-3-methylbutanoic acid and (2'R,3aR,6aR)/(2'S,3aS,6aS) (4,6-dimethylglycoluril-1-yl)pentanoic acid synthesized by highly diastereoselective condensation of 4,5-dihydroxy- imidazolidin-2-ones with racemic ureido acids. The differences in the molecular geometry of synthesized racemates were studied by X-ray diffraction that showed them to crystallize as conglomerates in non-centrosymmetric space groups Pna2₁ and P2₁2₁2₁, respectively     

气相输运沉积制备c轴择优取向的碘化铋薄膜

铋基卤化物材料因其无毒和优良的光电性能而显示出巨大的应用潜力。BiI₃作为一种层状重金属半导体,已被用于X射线检测、γ射线检测和压力传感器等领域,最近其作为一种薄膜太阳能电池吸收材料备受关注。本文采用简单的气相输运沉积(VTD)法,以BiI₃晶体粉末作为蒸发源,在玻璃基底上得到高质量c轴择优取向的BiI₃薄膜。并通过研究蒸发源温度和沉积距离对薄膜物相和形貌的影响,分析了BiI₃薄膜择优生长的机理。结果表明VTD法制备的BiI₃薄膜属于三斜晶系,其光学带隙为~1.8 eV。沉积温度对薄膜的择优取向有较大影响,在沉积温度低于270 ℃时,沉积的薄膜具有沿c轴择优取向生长的特点,超过此温度,c轴择优取向生长消失。在衬底温度为250 ℃、沉积距离为15 cm时制备的薄膜结晶性能最好,晶体形貌为片状八面体。     

Synthesis of 29H,31H-phthalocyanine and chloro (29H,31H-phthalocyaninato) aluminum derivatives showed anti-cancer and anti-bacterial actions

Continuous administration of most chemotherapeutic drugs can induce different types of side effects. There has been growing interest in exploring an alternative approach to synthesizing compounds that are most effective and have fewer side effects. We synthesized 29H,31H-Phthalocyanine, and Chloro (29H,31H- phthalocyaninato) aluminum at low temperatures using lithium in the present study with diisopropylamide as the nucleophile. The physical characteristics of 29H,31H-Phthalocyanine, and Chloro (29H,31H- phthalocyaninato) aluminum were confirmed by FT-IR method, XRD, SEM, and the impact of these compounds on human colorectal carcinoma (HCT-116) and human cervical cells (HeLa) was examined. Treatment with 29H,31H-Phthalocyanine significantly decreased cancer cell growth and proliferation, as determined by MTT and DAPI staining analysis. In contrast, Chloro (29H,31H- phthalocyaninato) aluminum treatment did not show any inhibitory action on colon or cervical cancer cells. We also calculated the inhibitory concentration (IC50) of 29H,31H-Phthalocyanine, which was 30 µg/ml (HCT-116) and 33 µg/ml (HeLa cells). The antibacterial effectiveness of 29H,31H-Phthalocyanine, and chloro (29H,31H- phthalocyaninato) aluminum was studied using Enterococcus faecalis (E. faecalis). The CFU (colony frequency unit) assay confirmed significant activity against the test bacterium after treatment with 29H,31H-Phthalocyanine. However, no activity was seen upon treatment with chloro (29H,31H- phthalocyaninato) aluminum against E. faecalis.     

A novel UPLC–MS/MS method for simultaneous quantification of trigonelline, 4-hydroxyisoleucine,and diosgenin from Trigonella foenum-graecum extract: Application to pharmacokinetic study in healthy and type 2 diabetic rats

Trigonelline (TR), 4-hydroxyisoleucine (4-HI), and diosgenin (DG) are the main bioactives of the purified standardized extract of the popular plant Trigonella foenum-graecum L. (TFG), and it has been proven effective for the treatment of various diseases. However, to the best of our knowledge, no study has investigated the pharmacokinetic parameters of purified standardized T. foenum-graecum extract in normal and diabetic Wistar rats. The present study has developed and validated a rapid, reliable, and sensitive simultaneous ultra-performance liquid chromatography MS method to estimate these bioactives. The chromatographic separation was achieved using methanol, acetonitrile, and 0.1% formic acid with the ideal gradient flow system on a BEH Shield RP 18 column. A positive electrospray ionization mode was selected to estimate m/z values of TR (138.14 > 94.63), 4-HI (148.19 > 74.08), and DG (415.54 > 271.33). The method was robust and reproducible over the linearity range of 60–5000, 6–5000, and 15–5000 ng/mL for TR, 4-HI, and DG, respectively. Using this novel validated method, we investigated the pharmacokinetic parameters of bioactives using Phoenix WinNonlin version 8.0 (Certera) in normal and diabetic rats. The assay was successfully applied for the estimation of pharmacokinetic parameters using noncompartmental analysis. This investigation shows that the absorption rate increased, whereas distribution and elimination processes slowed down in diabetic rats compared with normal rats.     

Y掺杂WS2二维材料的第一性原理研究

WS₂由于其优异的物理和光电性质引起了广泛关注。本研究基于第一性原理计算方法,探索了本征单层WS₂及不同浓度W原子替位钇(Y)掺杂WS₂的电子结构和光学特性。结果表明本征单层WS₂为带隙1.814 eV的直接带隙半导体。进行4%浓度(原子数分数)的Y原子掺杂后,带隙减小为1.508 eV,依旧保持着直接带隙的特性,随着Y掺杂浓度的不断增大,掺杂WS₂带隙进一步减小,当浓度达到25%时,能带结构转变为0.658 eV的间接带隙,WS₂表现出磁性。适量浓度的掺杂可以提高材料的导电性能,且掺杂浓度增大时,体系依旧保持着透明性并且在红外光和可见光区对光子的吸收能力、材料的介电性能都有着显著提高。本文为WS₂二维材料相关光电器件的研究提供了理论依据。     

基于视觉辐条图案识别方法的蓝宝石引晶机制研究

工业生产蓝宝石晶体过程中,引晶步骤有着至关重要的地位。引晶必须在温度梯度较小,温度分布趋于稳定的条件下进行。目前,工业生产蓝宝石主要依靠人工经验操控籽晶杆实现引晶操作,但是人工引晶操作的准确性不高会导致成品品质不佳、资源浪费。为此,本文提出一种基于蓝宝石视觉辐条图案识别方法来检测蓝宝石熔体状态自由液面状态,从而实现一种高效率引晶的机制。此方法利用经典骨架化算法细化辐条图案,Harris算子实现特征信息的提取,提取的特征信息放入运动轨迹模型中判断熔体稳定性,分析液面温度分布稳定性从而实现引晶。结果表明,此算法具有有效性,蓝宝石晶体引晶效率大大提高,生产出的成品良率也有提升,可有效指导蓝宝石的工业生产。     

基于2,5-二溴对苯二甲酸配体的锌/钴配合物合成、晶体结构及性质

将有机物2,5-二溴对苯二甲酸(H₂L₁)和2,2′-联吡啶(L₂)作为双配体,使用溶剂热法和七水合硫酸锌(ZnSO₄·7H₂O)、六水合硝酸钴(Co(NO₃)₂·6H₂O)分别反应,得到配合物[Zn(L₁)(L₂)(H₂O)]_n(1)和配合物[Co(L₁)(L₂)(H₂O)]_n(2)。采用单晶X射线衍射、元素分析、红外光谱、紫外光谱、荧光光谱、热重分析等测试方法对这两种物质进行分析研究。单晶测试结果表明配合物1是单斜晶系,以Zn²⁺配位连接L^2-₁与L₂形成一维链状结构,各条链在分子间氢键和π…π共轭作用下有规律地堆叠形成三维网络结构。配合物2是三斜晶系,Co1离子和Co1ⁱ离子由H₂L₁上的羧酸氧原子O4和O4ⁱ连接,形成双齿螯合的配位结构单元,以Co²⁺配位连接 L^2-₁和L₂形成二维网格结构,各层在O—H…O分子间氢键和范德瓦耳斯力作用下有规律的堆叠形成三维网络结构。配合物1和2均含有芳香杂环、羧基杂环和氮杂环,具有良好的荧光性质和热稳定性,最大发射波长分别为345 nm和333 nm。     

Bicomponent Cocatalyst Decoration on Flux-assisted CaTaO2N Single Crystals for Photocatalytic CO2 Reduction under Visible Light

Cubic-like CaTaO₂N photocatalysts with high crystallinity and uniform particle size were successfully prepared by the flux-assisted nitridation method. The growth of CaTaO₂N single crystals under different synthesis conditions was systematically investigated to understand the effects of the crystallinity and optical property on photocatalytic performance of CO₂ reduction. Moreover, the modification of CaTaO₂N single crystals with core-shell Ni−Ag bicomponent cocatalyst by two-step decoration process gave a 2.4 times higher amount of CO evolution than the deposition of sole Ag cocatalyst, because of the synergistic effects of bicomponent cocatalyst on the interfacial electron transfer and surface catalytic process. This study provides a valuable way to construct high-crystalline photocatalysts with effective bicomponent cocatalyst for visible-light-driven CO₂ reduction with H₂O.     

The covalent functionalization of few-layered MoTe2 thin films with iodonium salts

Covalent functionalization of 2D materials provides a tailored approach towards tuning of their chemical, optical, and electronic properties making the search for new ways to graft small molecules important. Herein, the reaction with (3,5-bis(trifluoromethyl)phenyl)iodonium salt is revealed as an effective strategy for functionalization of MoTe₂ thin films. Upon decomposition of the salt, the generated radicals graft covalently as aryl-(CF₃)₂ groups at the surface of both metallic (1T’) and semiconducting (2H) polymorphs of MoTe₂. Remarkably, the reactivity of the salt is governed by the electronic structure of the given polymorph. While the functionalization of the metallic MoTe₂ occurs spontaneously, the semiconducting MoTe₂ requires activation by light. The reaction proceeds with the elimination of oxide from the original films yielding the functionalized products that remain protected in ambient conditions, presenting a viable solution to the ageing of MoTe₂ in air.     

一种通过梯形PPMgLN波导倍频实现带宽可调谐光源的理论研究

本文设计了一种梯形的周期极化掺镁铌酸锂(PPMgLN)波导,并通过在传播方向上引入温度梯度来拓宽其倍频(SHG)过程的泵浦光源可接收带宽。通过有限差分的光束传输法,计算波导的有效折射率,并进行波导尺寸的设计。结果表明,通过改变梯形波导不同位置的温度,使其形成一个温度梯度,可拓宽泵浦光源的波长可接收带宽。本文所设计的PPMgLN波导最大泵浦光源可接收带宽为C波段,即1 530~1 565 nm,该波导可倍频C波段,得到输出波段带宽为765~782.5 nm,温度调谐范围为30~150 ℃。