Mullaugh Katherine M, Luther George W
Department of Chemistry and Biochemistry, University of Delaware, Newark, Delaware 19716, USA.
J Environ Monit. 2010 Apr;12(4):890-7. doi: 10.1039/b919917a. Epub 2010 Jan 22.
A multi-technique approach was adopted using UV/visible spectroscopy, fluorescence spectroscopy, dynamic light scattering (DLS), and transmission electron microscopy (TEM) in the characterization of cadmium sulfide (CdS) nanoparticles. CdS nanoparticle sizes could be determined by the Brus equation, which relates the UV/vis spectroscopic properties of CdS nanoparticles to size based on the quantum confinement effect. The diameters calculated from the wavelength of absorbance in UV/vis spectra were within 10% of the mean nanoparticle diameter measured in TEM. UV/vis spectroscopy provided an aqueous phase measurement of the CdS core size of the nanoparticles (<2 nm to approximately 10 nm diameter) that is based on a physical property rather than light scattering. CdS nanoparticles readily formed upon addition of sulfide to a Cd(ii)-thiolate complex with the thiolate molecules acting as capping agents that passivate the nanoparticle surface, thereby preventing bulk mineral precipitation. Using UV/vis as a method of nanoparticle sizing, we were able to demonstrate how aqueous conditions dictate the resulting nanoparticle size. High pH, capping thiolate concentration and Cd : S ratio all resulted in smaller nanoparticles. Ionic strength did not influence nanoparticle size, but DLS data indicate the formation of aggregates above ionic strengths of 0.1 M.
采用了多种技术方法,利用紫外/可见光谱、荧光光谱、动态光散射(DLS)和透射电子显微镜(TEM)对硫化镉(CdS)纳米颗粒进行表征。CdS纳米颗粒的尺寸可以通过布儒斯方程确定,该方程基于量子限域效应将CdS纳米颗粒的紫外/可见光谱性质与尺寸联系起来。从紫外/可见光谱中吸光度波长计算出的直径与TEM测量的平均纳米颗粒直径相差在10%以内。紫外/可见光谱基于一种物理性质而非光散射提供了纳米颗粒CdS核尺寸的水相测量(直径<2nm至约10nm)。向Cd(ii)-硫醇盐络合物中加入硫化物时,CdS纳米颗粒很容易形成,硫醇盐分子作为封端剂钝化纳米颗粒表面,从而防止大量矿物沉淀。使用紫外/可见光谱作为纳米颗粒尺寸测定的方法,我们能够证明水相条件如何决定所得纳米颗粒的尺寸。高pH值、封端硫醇盐浓度和Cd:S比均导致纳米颗粒尺寸较小。离子强度不影响纳米颗粒尺寸,但DLS数据表明在离子强度高于0.1M时会形成聚集体。