Synthesis and characterization of zinc bis(O-isopropylxanthate) as a single-source chemical vapor deposition precursor for ZnS

Barreca, Davide; Gasparotto, Alberto; Maragno, Cinzia; Seraglia, Roberta; Tondello, Eugenio; Venzo, Alfonso; Krishnan, Venkata; Bertagnolli, Helmut

doi:10.1002/aoc.948

Cited by 19 publications

(9 citation statements)

References 33 publications

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“…For the nontreated TMSC/CuXa/InXa film, characteristic bands for the xanthates as well as those for the TMSC were detected. The bands at 1081, 1054, and 1016 cm –1 can be assigned to C–S stretching vibrations and those at 1237 and 1212 cm –1 to asymmetric C–O–C stretching vibrations of the metal xanthates. , The bands associated with the TMSC matrix are present at 848 cm –1 , which is characteristic for ν Si–C . After the heat treatment, all bands associated with CuXa and InXa vanished, indicating the decomposition of the xanthates and the formation of CuInS 2 nanoparticles.…”

Section: Resultsmentioning

confidence: 99%

“…Furthermore, it is demonstrated that the heating step led to decomposition of both xanthates while the TMSC remains unaffected.For the nontreated TMSC/CuXa/InXa film, characteristic bands for the xanthates as well as those for the TMSC were detected. The bands at 1081, 1054, and 1016 cm −1 can be assigned to C−S stretching vibrations and those at 1237 and 1212 cm −1 to asymmetric C−O−C stretching vibrations of the metal xanthates 27,28. The bands associated with the TMSC matrix are present at 848 cm −1 , which is characteristic for νSi−C .…”

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confidence: 95%

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Biobased Cellulosic–CuInS₂ Nanocomposites for Optoelectronic Applications

Reishofer

Rath

Ehmann

et al. 2017

ACS Sustainable Chem. Eng.

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A generic approach to design optoelectronic devices using renewable biopolymers is demonstrated. As a proof of principle, a biopolymer/CuInS 2 nanocomponent-based solar cell has been assembled by using a cellulose derivative with a reasonable life cycle performance, namely trimethylsilyl cellulose (TMSC). The solar cells are manufactured using a mixture of copper and indium xanthates as precursors, which decompose and form CIS nanoparticles within the biopolymer matrix during a thermal treatment, which was investigated by in situ combined grazing incidence small and wide angle X-ray scattering experiments. The growth of the nanoparticles is thereby controlled by the TMSC matrix. The nanocrystals exhibit an average diameter of approx. 4 nm. Using this composite, it was possible to fabricate solar cells, generating current in a wide range of the solar spectrum and exhibiting power conversion efficiencies of ca. 1%.

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Section: Resultsmentioning

confidence: 99%

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confidence: 95%

Biobased Cellulosic–CuInS₂ Nanocomposites for Optoelectronic Applications

Reishofer

Rath

Ehmann

et al. 2017

ACS Sustainable Chem. Eng.

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“…To this end, a variety of metalorganic complexes of zinc (including dialkyldithiocarbamates, , alkyl xanthates, thiosemicarbazones, dialkylthiocarbamates and monothiocarboxylates, dithiophosphinate, N -thiophosphorylated-thioureas, and thio- and dithio-biuret) have been designed and developed for application in the chemical vapor deposition (CVD) of ZnS thin films . Reviews by Gleizes and O’Brien , provide detailed accounts of the use of other single source precursors for the deposition of chalcogenide materials by MOCVD.…”

Section: Introductionmentioning

confidence: 99%

Aerosol-Assisted Chemical Vapor Deposition of ZnS from Thioureide Single Source Precursors

et al. 2019

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A family of 12 zinc(II) thoureide complexes, of the general form [{L}ZnMe], [{L}Zn{N(SiMe 3 ) 2 }], and [{L} 2 Zn], have been synthesized by direct reaction of the thiourea pro-ligands i PrN(H)CS(NMe 2 ) H[L 1 ], CyN(H)CS(NMe 2 ) H[L 3 ], t BuN(H)CS(NMe 2 ) H[L 2 ], and MesN(H)CS(NMe 2 ) H[L 4 ] with either ZnMe 2 (1:1) or Zn{N(SiMe 3 ) 2 } 2 (1:1 and 2:1) and characterized by elemental analysis, NMR spectroscopy, and thermogravimetric analysis (TGA). The molecular structures of complexes [{L 1 9), and [{L 4 } 2 Zn] 2 (12) have been unambiguously determined using single crystal X-ray diffraction studies. Thermogravimetric analysis has been used to assess the viability of complexes 1−12 as single source precursors for the formation of ZnS. On the basis of TGA data compound 9 was investigated for its utility as a single source precursor to deposit ZnS films on silica-coated glass and crystalline silicon substrates at 150, 200, 250, and 300 °C using an aerosol assisted chemical vapor deposition (AACVD) method. The resultant films were confirmed to be hexagonal-ZnS by Raman spectroscopy and PXRD, and the surface morphologies were examined by SEM and AFM analysis. Thin films deposited from (9) at 250 and 300 °C were found to be comprised of more densely packed and more highly crystalline ZnS than films deposited at lower temperatures. The electronic properties of the ZnS thin films were deduced by UV−Vis spectroscopy to be very similar and displayed absorption behavior and band gap (E g = 3.711−3.772 eV) values between those expected for bulk cubic-ZnS (E g = 3.54 eV) and hexagonal-ZnS (E g = 3.91 eV).

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“…The most intense Raman bands of 1 are centered at 91, 167, 232, 339, 406, 439, 665, 845, 998, and 1029 cm −1 . Raman band centers of 1, with possible assignments from compounds similar to SbEX [43,48,50], are listed in Table S2. Raman bands attributed to only 1 were found above the limit of detection.…”

Section: Identification Ofmentioning

confidence: 99%

“…Xanthates, e.g., potassium ethyl xanthate (KS 2 COCH 2 CH 3 , KEX) were discovered by W. C. Zeise in 1822 [4]. Since then, xanthates and related organometallic compounds are being used in ore flotation, in organic chemistry, in analytical chemistry, in biochemistry, in coordination chemistry, and in materials science to fabricate metal chalcogenide powders and layers, e.g., ZnS, NiS, Fe 2 S 3 , Cu 2 S, PbS, As 2 S 3 , Sb 2 S 3 , Bi 2 S 3 , and lead-free perovskites [4,32,[34][35][36][37][38][39][40][41][42][43][44]. Antimony ethyl xanthate (SbEX) has risen to prominence in the last decade as a single-source precursor to fabricate Sb 2 S 3 powders for various applications, or to make porous layers for use as the absorber in solar cells by solution-based chemical methods, e.g., solvothermal, or spin-coating coupled with post-deposition annealing at 160-240 °C [33,39,45].…”

Section: Introductionmentioning

confidence: 99%

Thermal decomposition of tris(O-ethyldithiocarbonato)-antimony(III)—a single-source precursor for antimony sulfide thin films

Eensalu

Tõnsuaadu

Adamson

et al. 2021

J Therm Anal Calorim

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Thermal decomposition of tris(O-ethyldithiocarbonato)-antimony(III) (1), a precursor for Sb2S3 thin films synthesized from an acidified aqueous solution of SbCl3 and KS2COCH2CH3, was monitored by simultaneous thermogravimetry, differential thermal analysis and evolved gas analysis via mass spectroscopy (TG/DTA-EGA-MS) measurements in dynamic Ar, and synthetic air atmospheres. 1 was identified by Fourier transform infrared spectroscopy (FTIR) and nuclear magnetic resonance (NMR) measurements, and quantified by NMR and elemental analysis. Solid intermediates and final decomposition products of 1 prepared in both atmospheres were determined by X-ray diffraction (XRD), Raman spectroscopy, and FTIR. 1 is a complex compound, where Sb is coordinated by three ethyldithiocarbonate ligands via the S atoms. The thermal degradation of 1 in Ar consists of three mass loss steps, and four mass loss steps in synthetic air. The total mass losses are 100% at 800 °C in Ar, and 66.8% at 600 °C in synthetic air, where the final product is Sb2O4. 1 melts at 85 °C, and decomposes at 90–170 °C into mainly Sb2S3, as confirmed by Raman, and an impurity phase consisting mostly of CSO 2 2− ligands. The solid-phase mineralizes fully at ≈240 °C, which permits Sb2S3 to crystallize at around 250 °C in both atmospheres. The gaseous species evolved include CS2, C2H5OH, CO, CO2, COS, H2O, SO2, and minor quantities of C2H5SH, (C2H5)2S, (C2H5)2O, and (S2COCH2CH3)2. The thermal decomposition mechanism of 1 is described with chemical reactions based on EGA-MS and solid intermediate decomposition product analysis.

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Synthesis and characterization of zinc bis(O-isopropylxanthate) as a single-source chemical vapor deposition precursor for ZnS

Cited by 19 publications

References 33 publications

Biobased Cellulosic–CuInS₂ Nanocomposites for Optoelectronic Applications

Biobased Cellulosic–CuInS₂ Nanocomposites for Optoelectronic Applications

Aerosol-Assisted Chemical Vapor Deposition of ZnS from Thioureide Single Source Precursors

Thermal decomposition of tris(O-ethyldithiocarbonato)-antimony(III)—a single-source precursor for antimony sulfide thin films

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Synthesis and characterization of zinc bis(O-isopropylxanthate) as a single-source chemical vapor deposition precursor for ZnS

Cited by 19 publications

References 33 publications

Biobased Cellulosic–CuInS2 Nanocomposites for Optoelectronic Applications

Biobased Cellulosic–CuInS2 Nanocomposites for Optoelectronic Applications

Aerosol-Assisted Chemical Vapor Deposition of ZnS from Thioureide Single Source Precursors

Thermal decomposition of tris(O-ethyldithiocarbonato)-antimony(III)—a single-source precursor for antimony sulfide thin films

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Biobased Cellulosic–CuInS₂ Nanocomposites for Optoelectronic Applications

Biobased Cellulosic–CuInS₂ Nanocomposites for Optoelectronic Applications