Min Won Ja, Jung Sunghan, Lim Sung Jun, Kim Yongwook, Shin Seung Koo
Bio-Nanotechnology Center, Department of Chemistry, Pohang University of Science and Technology, San 31 Hyoja-dong Namgu, Pohang, Kyungbuk 790-784, Korea.
J Phys Chem A. 2009 Sep 3;113(35):9588-94. doi: 10.1021/jp905153v.
The metal (M = Cd2+ and Zn2+) complexes with trioctylphosphine chalcogenide (TOPE, E = O, S, and Se) are prepared by electrospray ionization, and their relative stabilities and intramolecular reactions are studied by collision-induced dissociation (CID) with Xe under single collision conditions. These metal-TOPE complexes are considered as molecular precursors for the colloidal synthesis of II-VI compound semiconductor nanocrystals employing TOPO as a metal-coordinating solvent and TOPS or TOPSe as a chalcogen precursor. Of the various [M + nTOPE]2+ (n = 2-7) ions generated by ESI, the n = 2-4 complexes are characterized by CID as a function of collision energy. The collision energy at 50% dissociation (E50%) is determined from the cracking curve and the relative stabilities of the complexes are established. Between the two metal ions, the zinc-TOPE complexes are more stable than the cadmium-TOPE complexes when n = 2-3, whereas their stabilities are reversed when n = 4. Of the TOPE, TOPO binds most strongly to the metal ion, while TOPSe does most weakly. Upon CID, loss of TOPE occurs exclusively from the tetra-TOPE complexes, while extensive fragmentation of TOPE takes place from the di-TOPE complexes, showing the signature of the metal chacogenide formation. The nucleation of nanocrystals appears to begin with cracking of [M + 2TOPE]2+ (E = S and Se).
通过电喷雾电离制备了金属(M = Cd2+ 和 Zn2+)与三辛基膦硫属化物(TOPE,E = O、S 和 Se)的配合物,并在单碰撞条件下通过与 Xe 的碰撞诱导解离(CID)研究了它们的相对稳定性和分子内反应。这些金属 - TOPE 配合物被视为使用 TOPO 作为金属配位溶剂以及 TOPS 或 TOPSe 作为硫属前驱体进行 II - VI 族化合物半导体纳米晶体胶体合成的分子前驱体。在通过电喷雾电离产生的各种 [M + nTOPE]2+(n = 2 - 7)离子中,通过 CID 表征了 n = 2 - 4 的配合物作为碰撞能量的函数。由裂解曲线确定 50% 解离时的碰撞能量(E50%),并确定配合物的相对稳定性。在两种金属离子之间,当 n = 2 - 3 时,锌 - TOPE 配合物比镉 - TOPE 配合物更稳定,而当 n = 4 时它们的稳定性相反。在 TOPE 中,TOPO 与金属离子结合最强,而 TOPSe 最弱。在 CID 过程中,TOPE 的损失仅发生在四 - TOPE 配合物中,而 TOPE 的广泛碎片化发生在二 - TOPE 配合物中,显示出金属硫属化物形成的特征。纳米晶体的成核似乎始于 [M + 2TOPE]2+(E = S 和 Se)的裂解。