Coating processes – Coating by vapor – gas – or smoke
Patent
1996-08-02
1998-11-17
Lusignan, Michael
Coating processes
Coating by vapor, gas, or smoke
4272553, 427226, C23C 1618
Patent
active
058373217
DESCRIPTION:
BRIEF SUMMARY
The present invention relates to volatile organic lanthanide compounds (adduct complexes) and methods for the preparation of lanthanide-containing layered materials from those compounds.
In particular, the present invention relates to volatile organic yttrium compounds. In this specification, the term lanthanide includes yttrium as well as all the elements (metals) with atomic numbers 57-71. Lanthanide elements 57-71 in particular are used in opto-electronic materials.
BACKGROUND OF THE INVENTION
Lanthanide compounds, especially lanthanide beta-diketonate complexes are of particular interest as starting materials (precursors) for so-called metal-organic chemical vapour deposition (MOCVD) of lanthanide (e.g. yttrium)-containing materials. Important examples are the deposition of mixed metal oxides which are superconducting at relatively high temperatures, of buffer layers, of anode- and electrolyte materials for fuel cells and of magnetic oxides.
Under some circumstances deposition of pure metal may he possible and the term metal-containing materials as used herein is to be interpreted accordingly. More than one metal may be present in the metal-containing material (normally metal oxide).
P. Lu, J. Zhao, C. S. Chern, Y. Q. Li, G. A. Kulesha, B. Gallois, P. Norris, B. Kear and F. Cosandey for instance, in J. Mater. Res., 7 (1992) 1993, describe the use of the 2,2,6,6-tetramethyl-3,5-heptanedione (TMHD) complex of Y, that is Y(TMHD).sub.3, as a precursor for yttrium during MOCVD of 90.degree. K. superconducting YBa.sub.2 Cu.sub.3 O.sub.7-x. However, in J. Phys., 50:C5 (1989) 981 (L. G. Hubert-Pfalzgraf, M. C. Massiani, R. Papiernik and O. Poncelet) and in Appl. Organomet. Chem., 6 (1992) 627 (L. G. Hubert-Pfalzgraf) there is described how water, always present in precursors, and also in this (commercially available) compound, can lead to hydrolysis during evaporation in a MOCVD process, with the consequence that the mass transport is not constant during the whole process. In addition, Y(TMHD).sub.3 has a rather high melting point (170.degree. C.), which means that it is evaporated from the solid phase. Due to the appearance of differences in crystal shape and crystal size, varying evaporation rates can occur.
Also other volatile, though fluorine-containing, yttrium-.beta.-diketonates are used, such as yttrium-6,6,7,7,8,8,8-heptafluoro-2,2-dimethyl-3.5-octanedionate monohydrate--Y(FOD).sub.3.H.sub.2 O--, for example in J. Mater. Res., 5 (1990) 2706 (D. J. Larkin, L. V. Interrante and A. Bose). This compound also contains water and, moreover, gives problems in the deposition of layers and their properties due to the presence of fluorine.
In J. Phys., 50:C5 (1989) 981 (L. G. Hubert-Pfalzgraf, M. C. Massiani, R. Papiernik and O. Poncelet), the easy formation of a coordination complex between an Y(.beta.-diketonate).sub.3 and for instance dimethylformamide, pyridine or dimethylsulphoxide, is suggested, but no actual examples with Y(TMHD).sub.3 are given. The existence of a number of Ln(TMHD).sub.3.DMF (Ln is a lanthanide metal) adducts is reported in Inorg. Synth., 11 (1968) 94 (K. J. Eisentraut and R. E. Sievers) and in Inorg. Chem., 6 (1967) 1933 (J. E. Schwarberg, D. R. Gere, R. E. Sievers and K. J. Eisentraut), but the compound Y(TMHD).sub.3.DMF is not described.
WO 89/07666 (T. J. Marks and K. H. Dahmen) describes three Y precursors. The first is Y(TMHD).sub.3 but this is non ideal as it has a high melting point (175.degree.-6.degree. C.) and is mildly moisture sensitive. The second is Y(FOD).sub.3 (FOD=C.sub.3 F.sub.7 COCHCOC(CH.sub.3).sub.3) but this has a high melting point and also contains fluorine. The third is Y(ACAC).sub.3 (ACAC=H.sub.3 CCOCHCOCH.sub.3) and this has insufficient thermal stability to be an acceptable precursor; it is also high melting (138.degree.-140.degree. C.).
CA 99: 30325w describes adduct complexes ML.sub.3 Q (where Q=o-phenanthroline, bipyridyl and Ph.sub.3 P=O) but these are so labile that they fully disintegrate in the process of mass spectra acquisition. These complexes ar
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Cook Stephen L.
Spee Carolus
Timmer Klaas
Lusignan Michael
Meeks Timothy
The Associated Octel Company Limited
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