翻译:化学英语(谢绝机器)
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The temperature can be controlled within variation of ¡2 uC at the set temperature by a thermal sensor in the sealed digestion vessels. The system operates at 2450 MHz frequency, and works at 0–1000 W power. Users can program the reaction temperature and time. The reaction vessel was double walled and consisted
of a Teflon inner liner and cover surrounded by a high strength vessel shell of Ultem polyetherimide. CdTe nanocrystals were prepared using the reaction between Cd2+ and NaHTe solution. Cd precursor solutions were prepared by mixing a solution of CdCl2 andMPA as stabilizer in ultrapure water, and then adjusted to different pH values with 1 M NaOH. The typical molar ratio of Cd : Te :MPA was 2 : 1 : 4.8 in our experiments. The solution was deaerated with N2 bubbling for 30 min. Under vigorous stirring, the oxygen-free NaHTe solution prepared according to the protocol13 was injected; 20 ml mixture solution (CdTe precursors) was transferred into a vessel (total volume 60 ml) and placed into the microwave digestion furnace. Under microwave irradiation (300 W), the reaction system reached certain temperature and pressure (the temperature decides the pressure). Various sizes of CdTe NCs with high QY were prepared by controlling microwave irradiation time and reaction temperature. Because the reaction vessel was closed, high temperature and pressure were produced in this system. Noticeably, when the temperature of the vessel was naturally cooled to lower than 90 uC, we opened the cover of the reaction vessel and took the samples. The asprepared colloid samples were diluted for optical characterizations, and precipitated by 2-propanol8 for the XRD characterization. TEM samples were prepared by dropping the aqueous CdTe solution onto carbon-coated copper grids with the excess solvent evaporated. The QY of CdTe NC was measured according to the method described in the references.Briefly, rhodamine 6G (ethanol as solvent) was chosen as a reference standard (QY 5 95%), the absorbance for the standard and the CdTe colloid samples at the excitation wavelengths and the fluorescence spectra of the same solutions were measured respectively. The integrated fluorescence intensity (that is, the area of the fluorescence spectrum) from the fully corrected fluorescence spectrum was calculated. Six different concentration solutions of rhodamine 6G and CdTe colloid solutions (absorbance at excitation wavelength , 0.1) were used in the measurements. The areas of the integrated fluorescence intensity vs. absorbance were plotted. The plot obtained should be a straight line with a gradient M, which was used to calculate the quantum yield according to the following equation:
参考答案:温度可用置于密封器中的热传感器控制在设定温度上下2℃的误差范围内。该体系在2450 MHz 频率和0-1000 W功率下操作。 用户可对反应温度和时间进行编程。双层反应器由一层特氟隆(聚四氟乙烯)内衬和聚醚酰亚胺高强度外壳组成。碲化镉纳米晶体用镉离子和碲氢化钠液反应制备。镉母液用超纯水中混合二氯化镉液和3-巯基丙酸稳定剂、然后用1 M 氢氧化钠液调节不同pH 值的方法来制备。本实验中镉:碲:3-巯基丙酸典型摩尔比是2 : 1 : 4.8 。该溶液在氮气气泡中脱气30 分钟。强烈搅拌下注入按方案13制备的无氧碲氢化钠液;然后将20 ml碲化镉母液转入60 ml反应器中并置于微波炉内。在300 W微波辐照下,反应体系达到特定温度和压力(温度决定了压力大小)。带有高量子产额的各种大小的碲化镉纳米晶体用控制微波辐照时间和反应温度来制备。因反应器密封,故该体系产生了高温高压。值得注意的是,当反应器温度自然冷却到90 ℃以下,打开反应器盖并采样。所制备的胶体样品稀释后用于光学特性研究,并用2-丙醇8沉淀后用于x射线衍射研究。透射电镜样品用滴加稀碲化镉液到碳涂布的铜网上并挥去过量溶剂的方法制备。碲化镉纳米晶体的量子产额按文献描述的方法测量。简言之, 选用罗丹明6G(玫瑰红6G)的乙醇溶液(量子产额5.95%)作为参照标准,分别测量参照物和处于激发波长的碲化镉胶体样品的吸收值,以及同一溶液的荧光光谱。计算了收集的荧光光谱的光强总积分 (也就是说荧光光谱的面积) 。测量中使用6个不同浓度的罗丹明6G溶液和碲化镉胶体溶液 (在激发波长0.1处吸收) 。以荧光强度积分面积对吸收值进行作图。所得图象应是斜率为M的直线, 按下述方程用该图象计算量子产额: