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Synthesis of complex fluorides for optical applications.

机译：用于光学应用的复杂氟化物的合成。

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摘要

Large single crystals of alkali metal fluorides are desirable for many reasons. Fluoride laser crystals have a wide transmission range and on account of their low phonon energies, many efficient laser emissions have been obtained from 285 nm to 4.34 microm.1,2 Inorganic fluoride single crystals feature large bandgaps, very wide optical transmittance ranges from vacuum-ultraviolet (VUV) to mid-IR wavelength regions, lower refractive indices than those of oxides, and typically lower phonon energies (which drastically reduce multiphonon relaxation rates of rare earth ions).3;The main goal of this work was to investigate the hydrothermal synthesis of alkali metal fluorides. Melt techniques have been used thoroughly to research a variety of fluoride systems and showed many phases that were inaccessible due to incongruent melting or phase stability. The existence of these phases was shown but never characterized or grown as a crystalline material. Solution growth in supercritical water was an ideal way to attempt the synthesis of novel compounds and phases. New synthetic routes to known phases and compounds also arose as a part of this work.;Optically clear colorless crystals of K2BeF4 were synthesized up to 2 mm in size, and showed no phase transitions up to 1029 K, which suggests paraelectricitys at room temperature, contradicting previous reports.4 Attempts to incorporate a rare earth ion into the fluoroberyllate lattice proved unsuccessful however reactions between beryllium fluoride and lanthanide fluorides could be exploited as a synthetic route to single crystal rare earth fluorides.;Hydrothermal reactions with KF produced crystals of three different phases: hexagonal KY2F7, trigonal KYF4 and orthorhombic K2YF5. All were optically clear, colorless crystals, with the K2YF5 crystals growing the largest. This compound is beneficial due to its application as a radiation dosimeter and laser host. 5,6 Optical quality colorless crystals of RbY2F7 and CsY2F7 up to 4 mm in size were produced, and many spectroscopically active rare earth elements were doped into both hosts. A novel synthetic pathway to the hexagonal beta-RbGd3F 10, was discovered which led to the novel compound, beta-RbHo 3F10. The hydrothermal synthesis of hexafluoroelpasolites and lanthanide sesquioxides is also investigated. The hydrothermal synthesis described in this work has furthered the study of complex fluorides for optical applications. Novel synthetic pathways were discovered to known optical materials. Novel materials were also discovered.;1Takashima, M. In Advanced Inorganic Fluorides: Synthesis, Characterization and Applications, Nakajima, T.; Zemva, B.; Tressaud, A.; Elsevier: Amsterdam, The Netherlands, 2000, 176. 2Fouassier, C. In Advanced Inorganic Fluorides: Synthesis, Characterization and Applications, Nakajima, T.; Zemva, B.; Tressaud, A.; Elsevier: Amsterdam, The Netherlands, 2000, 316. 3Capper, P. In Bulk Crystal Growth of Electronic, Optical and Optoelectronic Materials, John Wiley and Sons: Great Britain, 2005. 4Solans, X.; Gonzalez-Silgo, C.; Calvet, T.; Ruiz-Perez, C.; Martinez-Sarrion, M. L.; Mestres, L. Phys. Rev. B 1998, 57(9), 5122-5125. 5Azorin-Nieto, J.; Khaidukov, N.M.; Sanchez-Rodriguez, A.; Azorin-Vega, J.C. Nuclear Instruments and Methods in Physics Research, 2007, B263, 36-40. 6Wang, D.; Min, Y.; Xia, S.; Makhov, V.N.; Khaidukov, N.M.; J.C. Krupa, J.C. Journal of Alloys and Compounds, 2003, 361, 294-298.
机译：由于许多原因，需要碱金属氟化物的大单晶。氟化物激光晶体具有宽的传输范围，并且由于其低声子能量，在285 nm至4.34微米范围内获得了许多有效的激光发射。1,2无机氟化物单晶具有较大的带隙，非常宽的光学透射率范围从真空到紫外线（VUV）到中红外波长区域，折射率比氧化物低，并且声子能量通常较低（这大大降低了稀土离子的多声子弛豫速率）。3;这项工作的主要目的是研究水热碱金属氟化物的合成。熔融技术已被广泛用于研究各种氟化物系统，并显示出由于熔融或相稳定性不一致而无法进入的许多相。显示了这些相的存在，但从未表征或生长为结晶材料。在超临界水中的溶液生长是尝试合成新化合物和新相的理想方法。这项工作的一部分还出现了向已知相和化合物的新合成路线。合成了光学透明的K2BeF4无色晶体，尺寸最大为2 mm，在1029 K以下没有相变，这表明在室温下为顺电， 4试图将稀土离子掺入氟铍酸酯晶格中的尝试未获成功，但氟化铍和镧系氟化物之间的反应可被用作合成单晶稀土氟化物的途径。；与KF的水热反应产生了三种不同的晶体相：六角形KY2F7，三角形KYF4和正交晶体K2YF5。所有晶体均为光学透明无色晶体，其中K2YF5晶体生长最大。由于其作为辐射剂量计和激光主体的应用，因此该化合物是有益的。 5,6光学尺寸的无色晶体RbY2F7和CsY2F7的尺寸最大为4 mm，许多光谱活性稀土元素都掺入了这两种基质中。发现了通往六边形β-RbGd3F10的新型合成途径，这导致了新型化合物β-RbHo3F10。还研究了六氟锂辉石和镧系倍半氧化物的水热合成。这项工作中描述的水热合成进一步促进了用于光学应用的复杂氟化物的研究。发现了已知光学材料的新型合成途径。还发现了新的材料。1高岛，M。，《高级无机氟化物：合成，表征与应用》，中岛，T .； Zemva，B .； Tressaud，A .； Elsevier：荷兰阿姆斯特丹，2000年，第176页。2 Fouassier，C。《高级无机氟化物：合成，表征和应用》，中岛，T。 Zemva，B .； Tressaud，A .； Elsevier：荷兰阿姆斯特丹，2000年，第316页。3Capper，P。《电子，光学和光电材料的块状晶体生长》，John Wiley and Sons：英国，2005年。4 Solans，X。 Gonzalez-Silgo，C .；卡尔维特（T.） Ruiz-Perez，C .； Martinez-Sarrion，M. L .； Mestres，L.Phys。版本B 1998，57（9），5122-5125。 5 Azorin-Nieto，J .; N.M. Khaidukov；桑切斯-罗德里格斯（A. Azorin-Vega，J.C.核仪器和方法在物理研究中，2007，B263，36-40。 6王D.敏，Y。夏，S.弗吉尼亚州马霍夫; N.M. Khaidukov； J.C. Krupa，J.C。Journal of Alloys and Compounds，2003，361，294-298。

著录项

  • 作者

    Stepleton, Seth Eugene.;

  • 作者单位

    Clemson University.;

  • 授予单位 Clemson University.;
  • 学科 Chemistry Inorganic.;Engineering Materials Science.
  • 学位 Ph.D.
  • 年度 2009
  • 页码 232 p.
  • 总页数 232
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 无机化学;工程材料学;
  • 关键词

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