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Synthesis And Characterization Of Novel Copper(Ⅰ)Complexes As Precursors For Metal-Organic Chemical Vapor Deposition

Posted on:2006-05-05Degree:MasterType:Thesis
Country:ChinaCandidate:Y P ShenFull Text:PDF
GTID:2121360155470276Subject:Physical chemistry
Abstract/Summary:PDF Full Text Request
Chemical Vapor Deposition (CVD) of conformal copper thin films is required for the metallization of multilayered integrated circuits (ULSI). The ability to fill high-aspect ratio holes requires a technique such as Metal-Organic Chemical Vapor Deposition (MOCVD). Specifically, research geared toward the synthesis and identification of the volatile metal copper (I) precursors.A standard Schlenk line has been designed and constructed, and the MOCVD precursors (hfac)Cu(I)(alkene), where hfac = hexafluoroacetylacetone, alkene = COD (1,5-cyclooctadiene), CPE(cyclopentene), CPD(cycIopentadiene), have been prepared in one step, and further characterized by ~1H-NMR, FTIR, DSC-TGA.(hfac)Cu(I)(COD) is a bright yellow crystalline powder synthesized at room temperature and sublimed at 60℃ and at sub-atmospheric pressure. It is pure shown by the spectroscopy ~1H-NMR and FTIR. The thermal stability characterized by DSC-TGA reveals the compound is a good precursor for Cu MOCVD.(hfac)Cu(I)(CPE) is a light yellow crystalline powder synthesized at 10℃ and sublimed at 25℃ and at 40 kPa. It is also pure shown by the spectroscopy ~1H-NMR and FTIR. The thermal analysis data characterized by DSC-TGA show thermal stability of this compound is not very well and the bond breaking temperature for Cu-CPE is approximately 60.7℃.(hfac)Cu(I)(CPD) is a green yellow slimy solid synthesized at room temperature and sublimed at 55℃ and at sub-atmospheric pressure. Characterized by the spectroscopy ~1H-NMR and FTIR shows that the compound is a mixture probably including cyclopentadiene dimmer. The thermal analysis data characterized by DSC-TGA shows thermal stability of the compound is good and the bond breaking temperature for Cu-CPD is approximately 146.5℃. The guess that the productcontains cyclopentadiene dimmer is also proved by the endothermic peak at 166.8℃.At the same time ,the binary azeotropic data of 2-methoxypropene (1) + methanol (2), and + acetone (3) systems were determined at subatmospheric, normal, and elevated pressures by a stainless steel azeotrope apparatus based on rectification principle, and the experimental data were well correlated by a set of empirical equations. The results of correlation show that both the azeotropic composition versusthe azeotropic temperature, and the logarithm of total pressure versus the reciprocal of azeotropic temperature are well linear, and the calculated values are in good agreement with the experimental ones. As the total pressures is decreased, the content of 2-methoxypropene (MPP) in these two systems all increases, which suggests that it might be easier to make the mixtures separation at subatmospheric pressures, especially at 49.7 kPa for MPP-acetone mixtures, the MPP content is approaching 99.7 %. The azeotropic data and its correlations proposed in this work are of great importance in the process design for separation and purification of azeotropic mixtures, azeotropic rectification, and reactive rectification in MPP production.
Keywords/Search Tags:Copper (Ⅰ) Precursors, Synthesis and Characterization, 1,5-Cyclooctadiene, Cyclopentene, Cyclopentadiene, azeotrope, 2-methoxypropene
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