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Title: New routes to inorganic nanostructure materials
Author: Al-Shakban, Mundher
ISNI:       0000 0005 0289 8632
Awarding Body: University of Manchester
Current Institution: University of Manchester
Date of Award: 2018
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Metal sulfide thin films and nanoparticles are important in photovoltaic applications owing to their exciting properties. Xanthate complexes are well known for the deposition of metals sulfide films and nanoparticles. This produces suitable physical and chemical properties to deposit films with a very low level or no contamination at low temperature. The work shows the synthesis of a series of metal (Cu, Sn, Zn and In) complexes of xanthate ligands, their spectroscopic characterization, crystal structures and thermal decomposition have been studied. Xanthate complexes of calcium and barium have been also synthesised. The complexes were used as single source precursors for the deposition of SnS, CaS, BaS, CaCu2S2, β-BaCu2S2, β-BaCu4S3 and Cu2ZnSnS4 thin films by spin coating. In addition, Cu(I)-xanthate has been used for the synthesis of highly crystalline copper sulfide nanoparticles. In(III)-xanthate in conjunction with a Cu(I)-xanthate have been used as a single source precursors to the formation of CuInS2 nanoparticles, both CuxS and CuInS2 nanoparticles have been synthesised by hot injection method at 260 oC. The films and nanoparticles were characterised by powder X-ray diffraction, Raman spectra, scanning electron microscopy and energy dispersive X-ray spectroscopy, transmission electron microscopy and selected area electron diffraction. Triphenylphosphine copper(I) xanthate complexes [isobutylxanthate, 2-methoxyethylxanthate, 2-ethoxyethylxanthate, 1- methoxy-2-propylxanthate, 3-methoxy-1-butylxanthate, and 3-methoxy-3-methyl-1-butylxanthate] in addition to the ethyl and n-butyl have been used for the formation of copper sulfide nanorods. At 1 h reaction times chalcocite Cu2S is formed, while at 5 sec result in roxbyite Cu1.74S nanorods. The longer chain xanthates lead to the formation of rods of decreased width. These complexes as well as indium complexes have an ability to control the CuInS2 phase through choice of solvent. A melt reaction of calcium isopropylxanthate and the novel compounds barium isopropylxanthate and bis(triphenylphosphine)copper 2-methoxyethylxanthate at low temperature, atmospheric pressure and short decomposition time leads to a formation of CaCu2S2, β - BaCu2S2 and β - BaCu4S3 19 thin films which have previously been produced from a high temperature, high pressure reaction system. Cu2ZnSnS4 (CZTS) thin films were obtained from melt reaction after heating the [(Ph3P)2CuS2COEt], [Zn(S2COnBu)2] and [Sn(S2COEt)2] at temperatures between 200 and 475 °C. Higher temperatures give the normal tetragonal phase CZTS, while low temperatures are mixed hexagonal and cubic phases.
Supervisor: Lewis, David Sponsor: Not available
Qualification Name: Thesis (Ph.D.) Qualification Level: Doctoral
EThOS ID:  DOI: Not available
Keywords: Metal sulfide nanoparticles ; Metal sulfide thin films ; Xanthate complexes ; single source precursors