Department of Chemistry, Kansas State University, Manhattan, Kansas 66506, USA.
Langmuir. 2012 Feb 21;28(7):3569-75. doi: 10.1021/la203624p. Epub 2012 Feb 9.
We report the transformation of polydispersed dodecanethiol stabilized indium nanoparticles, obtained from bulk indium shot by evaporation/condensation solvated metal atom dispersion (SMAD) technique, into highly monodispersed partially alkyl thiolate-capped β-indiumsulfide (In(2)S(3)) by a postpreparative digestive ripening in high boiling point t-butyltoluene (190 °C) solvent. Upon digestive ripening, the as-prepared polydispersed black indium nanoparticles showed a characteristic color transition from black to cream, pale yellow, yellow, and finally to brown, indicating the transformation of the indium metal nanoparticles into intermediates composed of indium thiolates, sulfides, and polysulfides, and finally into the product In(2)S(3) nanoparticles whose surfaces are partially capped with thiolates. The transformed product (In(2)S(3)) was characterized with UV-vis, XRD, EDX, SEM, XPS, and TEM. From XRD and TEM measurements, the average size of the transformed In(2)S(3) nanoparticles is 5 nm. The optical absorbance of the as-prepared sample showed absorption peaks around 538 and 613 nm; upon digestive ripening these two peaks disappeared and stabilized at 375 nm, providing evidence of strong quantum confinement of excitons. The visible light-induced photocatalytic activity test with the In(2)S(3) nanoparticles showed that 95% of Rhodamine B (RhB) dye degraded after 100 min of irradiation with visible light.
我们报告了多分散的十二硫醇稳定的铟纳米粒子的转化,这些纳米粒子是通过蒸发/冷凝溶剂化金属原子分散(SMAD)技术从大块铟射流中获得的,通过在高沸点叔丁基甲苯(190°C)溶剂中进行预制备的消化陈化,转化为高度单分散的部分烷基硫醇封端的β-硫化铟(In(2)S(3))。在消化陈化过程中,制备的多分散黑色铟纳米粒子表现出从黑色到奶油色、淡黄色、黄色,最终到棕色的特征颜色转变,表明铟金属纳米粒子转化为由硫醇盐、硫化物和多硫化物组成的中间体,最终转化为表面部分被硫醇盐封端的产物 In(2)S(3)纳米粒子。转化产物(In(2)S(3))用 UV-vis、XRD、EDX、SEM、XPS 和 TEM 进行了表征。从 XRD 和 TEM 测量结果来看,转化后的 In(2)S(3)纳米粒子的平均尺寸为 5nm。所制备样品的光吸收显示在 538 和 613nm 左右有吸收峰;在消化陈化过程中,这两个峰消失并稳定在 375nm,这提供了激子强量子限制的证据。用 In(2)S(3)纳米粒子进行的可见光诱导光催化活性测试表明,在可见光照射 100 分钟后,95%的罗丹明 B(RhB)染料被降解。