4,4＇-二氯甲基联苯自聚合树脂合成条件优化及表征

通过正交实验对4,4＇-二氯甲基联苯（BCMBP）自聚合反应的工艺条件进行优化,对4种影响因素进行考察,得到影响产品比表面积大小因素的顺序为：预聚合时间、预聚合温度、单体浓度和催化剂用量.在优化条件下所得树脂的比表面积为1 512.66 m^2/g,树脂具有丰富的微孔和较高的聚合度.通过氮气吸附-脱附、SEM和热失重实验对树脂的孔径分布、微观形貌和热稳定性进行了研究.     

山西忻州麻地沟煤业有限公司可采煤层的煤类探讨

通过对麻地沟矿可采煤层的煤类探讨,得出结论:该矿可采煤层是13号煤层,其浮煤干燥无灰基挥发分(Vdaf)38.15%~43.02%,平均为39.73%;黏结指数(GR·1)6.87~27.65,平均为14.67;胶质层厚度(Y值)0~8.08 mm,平均为4.13 mm。由上述各煤层分类的各项指标,确定该井田13号煤为长焰煤(CY42)。     

单双层石墨烯的制备及电导特性调控

石墨烯二维材料有着优异的物理、化学特性,在多个科学领域展现出广阔的应用前景.采用化学气相沉积方法在Cu-Ni合金表面制备了二维石墨烯薄膜并揭示其生长机制;研究生长时间、温度等对石墨烯覆盖度和晶格质量的影响.通过优化生长条件,成功制备了大面积单层及具有强烈层间耦合作用的AB堆叠双层石墨烯薄膜.进一步运用表面沉积技术在单层石墨烯上构建零维Au团簇和二维Au薄膜,研究其对石墨烯电导特性的影响;并结合第一性原理计算,揭示Au的形态及覆盖度影响石墨烯电导特性的规律.据此制作了石墨烯场效应晶体管器件,通过精确控制Au的覆盖度,实现石墨烯电导类型和载流子浓度的有效调控,拓展了其在微电子领域的应用.     

北祁连石灰沟奥陶纪玄武岩流体组成及其地质意义

北祁连石灰沟地区中奥陶世发育了一套海相细碧岩--碱性火山岩组合,为岛弧火山作用产物.应用分步加热法测试了该区碱性玄武岩中橄榄石斑晶和基质的流体组成.玄武岩橄榄石斑晶和基质中流体组份都具有分阶段释放的特征,可分为低温(200～400?C)、中温(400～900?C)和高温(900～1 200?C)3个温度段,流体化学组成以H2O,CO2,CO+N2为主,次要组份是H2,SO2,CH4,O2,H2S等.石灰沟碱性玄武岩发育于相对氧化的流体环境,揭示其源区具有高的氧逸度,代表古岛弧形成的流体环境.     

Bi_(1.6)La_(0.4)Ti_2O_7薄膜的制备及性能研究

采用化学溶液沉积法在ITO基片上制备不同退火温度的掺镧钛酸铋Bi1.6La0.4Ti2O7(BLT)薄膜。研究了其结构、介电性能、漏电流密度与外加电压I-V关系曲线和光学带隙。XRD射线衍射测试结果表明,经500、550、600℃1 h退火后的薄膜的主晶相为烧绿石结构,无杂相生成,600℃时BLT薄膜衍射峰比其他两种温度的强。在1 kHz频率下测得的介电常数、损耗因子分别为114,3%;129,3%;194,6%。BLT薄膜的漏电流密度与外加电压关系曲线表明,BLT薄膜600℃的漏电流比550和500℃稍微减小。通过透射谱分析得到BLT薄膜的光学带隙几乎不受温度影响,均为3.7 eV。这些结果表明制备BLT固溶体薄膜较佳为退火温度600℃,具有较好的性能,在光电器件有良好的应用前景。     

原创中药红珠胶囊基于RRLC-ESI-MS/MS技术的化学成分分析

采用快速液相-三重串联四极杆质谱(RRLC-ESI-MS/MS)技术,在电喷雾质谱正模式和负模式下,对红珠胶囊内容物进行分析鉴定。通过质谱中分子离子峰和碎片离子峰的精确相对分子质量匹配,保留时间,紫外光谱对比,与对照品比对并结合参考文献鉴定,确证和指认了红珠胶囊中的新北美圣草苷、樱桃苷、柚皮苷、忍冬苷、野漆树苷、橙皮内酯水合物、7-(2″-α-鼠李糖基-6″-(3″″-羟基-3″″-甲基戊二酰)-β-D-葡萄糖基)柚皮素、异橙皮内酯、柚皮素9个化学成分。研究揭示了红珠胶囊的化学物质基础,为控制该药质量提供了依据。     

Microstructure and oxidation resistance of SiC–MoSi2 multi-phase coating for SiC coated C/C composites

In order to improve the anti-oxidation of C/C composites, a SiC–MoSi2multi-phase coating for SiC coated carbon/carbon composites(C/C)was prepared by low pressure chemical vapor deposition(LPCVD) using methyltrichlorosilane(MTS) as precursor, combined with slurry painting from MoSi2 powder. The phase composition and morphology were analyzed by scanning electron microscope(SEM) and X-ray diffraction(XRD) methods, and the deposition mechanism was discussed. The isothermal oxidation and thermal shock resistance were investigated in a furnace containing air environment at 1500 1C. The results show that the as-prepared SiC–MoSi2coating consists of MoSi2 particles as a dispersing phase and CVD–SiC as a continuous phase. The weight loss of the coated samples is 1.51% after oxidation at 1500 1C for 90 h, and 4.79% after 30 thermal cycles between 1500 1C and room temperature. The penetrable cracks and cavities in the coating served as the diffusion channel of oxygen, resulted in the oxidation of C/C composites, and led to the weight loss in oxidation.     

Cu衬底上ZnO纳米结构及其光催化性能分析

采用两步电化学沉积法在Cu衬底上沉积得到ZnO纳米结构薄膜。用X-射线衍射（XRD）和扫描电子显微镜（SEM）对其结构及形貌进行表征,发现先在Cu衬底上沉积一层Zn致密膜,更有利于在其表面上得到附着力强、形貌较好的ZnO纳米结构膜。系统考察了沉积温度和沉积时间等工艺参数对ZnO纳米结构的影响。结果表明,沉积温度和沉积时间对晶体结构和形貌有显著影响,通过对工艺进行适宜控制可以得到结晶性良好的六方纤锌矿型ZnO纳米结构膜。以罗丹明B为目标有机污染物,分析了ZnO膜的光催化性能,表明所制备的ZnO膜可以作为光催化剂,其光催化效率可达到72.4%。     

Al-Salen配合物催化聚己内酯与聚乙二醇共聚物合成与性能分析

以聚乙二醇为引发剂,以Al-Salen为催化剂,催化己内酯的开环聚合,研究了时间、温度及单体与引发剂的比例对产率和分子量的影响。采用红外、GPC和DSC等手段对聚合物结构和热性能进行分析。实验结果表明：要得到分子量较高的三嵌段共聚物,最佳聚合条件为：聚合时间17h,聚合温度180℃,单体与引发剂的质量比为20：1;要得到较高产率的三嵌段聚合物,最佳聚合条件为：聚合时间14h,聚合温度140℃,单体与引发剂的质量比为24：1。     

Properties and Morphology of TiN Films Deposited by Atomic Layer Deposition

In this study,TiN films were deposited on SiO2 substrates by Atomic Layer Deposition(ALD) using TiCl4and NH3 as precursors. Properties and morphology of the TiN films were characterized by different methods.Using Grazing Incidence X-Ray Diffraction(GIXRD),TiN films demonstrated polycrystalline structure with(111)preferred orientation. Film thickness was measured by Spectroscopic Ellipsometry(SE) and a stable growth rate of 0.0178 nm/cycle was reached after 500 deposition cycles,which was consistent with the essence of ALD as a surface-saturated self-limiting reaction. Film resistivity measured by a four-point probe continuously decreased with increasing deposition cycles until it reached the minimum value of 300μΩ cm at 5000 deposition cycles with a thickness of 87.04 nm. The surface roughness and morphology of the TiN films at different deposition cycles ranging from 50 to 400 were analyzed by Atomic Force Microscopy(AFM). The AFM results indicated that the initial film growth follows the Stranski-Krastanov mode.