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Synthesis, characterization, and thermal decomposition of single source precursors to nanocrystalline binary and ternary 13-15 materials.

机译：单源前体的合成，表征和热分解为纳米晶二元和三元13-15材料。

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摘要

The growing application of semiconductor materials continually invigorates research into their preparation. The use of single source precursors for the formation of 13–15 materials is advantageous in that it reduces or eliminates many of the safety concerns that plague the conventional industrial methods of 13–15 materials preparation, namely OMCVD and MBE. Additionally, the temperatures required for the conversion of a 13–15 single source precursor to its corresponding material are significantly reduced relative to conventional methods. Finally, single source precursors, upon thermolysis, have a propensity to form materials on the nanoscale size regime—an important feature as the drive toward smaller and smaller devices continues.; The research presented herein is focused on two aspects: (1) the preparation and characterization of novel organometallic single source precursor compounds and (2) the thermal decomposition of the precursors to form nanocrystalline binary and ternary 13–15 materials.; The utilization of a new class of compounds, the lithium pnictidometallates, as reagent materials for the preparation of precursors to ternary 13–15 materials was investigated with interesting results. Novel ligand replacement and molecular rearrangement accompanied the expected lithium halide coupling reactions as evinced by the isolation of the mixed group 13 compound (Me 3Si)2P(Cl)Ga[μ–P(SiMe3)2] 2B(H)Me) (4).; Dehalosilylation methodology was also applied for the formation single source precursors to nanocrystalline binary and ternary 13–15 materials. Reactions involving diethyl gallium chloride and diethyl indium chloride with tris(trimethylsilyl)phosphine, arsine, and stibine resulted both in oligomeric 13–15 compounds such as the dimeric [Et2InP(SiMe3) 2]2 (8) as well as mixed pnicogen compounds such as (Me3Si)2P[μ–GaEt2] 2Sb(SiMe3)2 (12). These compounds were subsequently pyrolyzed using bulk thermolysis techniques.; Powder X-ray diffraction and elemental analysis of the powders by obtained from the bulk thermolyses experiments showed not only that the precursors decompose to form their respective binary and ternary 13–15 materials, but also that the materials formed are in the nanocrystalline size regime.; Finally, the thermal decomposition of precursors to binary 13–15 materials was investigated using the combined technique of thermogravirnmetric analysis - mass spectrometry. This technique allowed for the mass analysis of the volatile elimination products produced during the thermolyses of the series of precursors, [Et2ME(SiMe3)2]n (M = Ga; E = P, As, Sb; M = In; E = P, As; n = 2; M = In; E = Sb; n = 3). Based on this analysis, the assignment of the primary mode of decomposition of these precursors as that of group 13–C and pnicogen–Si bond homolysis was made.
机译：半导体材料的日益增长的应用不断激发着对其制备的研究。使用单一来源的前体来形成13-15材料的优势在于，它减少或消除了困扰13-15材料制备的常规工业方法（即OMCVD和MBE）的许多安全隐患。此外，与传统方法相比，将13-15单源前体转化为其相应材料所需的温度大大降低。最终，单源前驱物在热解后倾向于形成纳米级尺寸的材料，这是随着越来越多的器件不断发展的重要特征。本文介绍的研究集中在两个方面：（1）新型有机金属单源前体化合物的制备和表征，以及（2）前体的热分解以形成纳米晶二元和三元13-15材料。研究了一种新型化合物，金属硫氰酸锂，作为制备13-15三元材料前体的试剂材料，得到了有趣的结果。新的配体置换和分子重排伴随着预期的卤化锂偶联反应，如分离出混合的13族化合物（Me 3 Si） 2 P（Cl）Ga [ μ–P（SiMe 3 ） 2 ] 2 B（H）Me）（ 4 ）。脱卤硅烷化方法也适用于形成纳米晶二元和三元13-15材料的单源前体。涉及二乙基氯化镓和二乙基氯化铟与三（三甲基甲硅烷基）膦，砷化氢和替比滨的反应均导致低聚13–15化合物，例如二聚体[Et 2 InP（SiMe 3 < / sub>） 2 ] 2 （ 8 ）以及混合的致癌物质化合物，例如（Me 3 Si ） 2 P [μ–GaEt 2 ] 2 Sb（SiMe 3 ） 2 （ 12 ）。随后使用本体热解技术将这些化合物热解。从本体热解实验获得的粉末的X射线粉末衍射和元素分析结果表明，不仅前体分解形成各自的13-15三元和二元材料，而且所形成的材料均处于纳米晶尺寸范围内。 ;最后，使用热重分析-质谱的组合技术研究了前体到13-15二元材料的热分解。该技术可对一系列前体[Et 2 ME（SiMe 3 ）2] n热解过程中产生的挥发消除产物进行质量分析。 （M = Ga； E = P，As，Sb； M = In； E = P，As； n = 2； M = In； E = Sb； n = 3）。基于此分析，确定了这些前体的主要分解模式，即13-C组和pnicogen-Si键均质分解。

著录项

  • 作者

    Jouet, Richard Jason.;

  • 作者单位

    Duke University.;

  • 授予单位 Duke University.;
  • 学科 Chemistry Inorganic.
  • 学位 Ph.D.
  • 年度 2000
  • 页码 189 p.
  • 总页数 189
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 无机化学;
  • 关键词

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