Real-time studies of phase transformations in Cu–In–Se–S thin films

Klopmann, C. von; Djordjevic, J.; Scheer, Roland

doi:10.1016/j.jcrysgro.2005.10.105

Cited by 32 publications

(16 citation statements)

References 19 publications

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“…10 EDXRD has been used for several years and is well established for analyzing phase formations during reactive film growth processes. [10][11][12][13][14][15] In situ fluorescence signals recorded during EDXRD measurements have been discussed as indications for changes of depth distributions. 10,16 Also, a) Author to whom correspondence should be addressed.…”

Section: Introductionmentioning

confidence: 99%

In situ analysis of elemental depth distributions in thin films by combined evaluation of synchrotron x-ray fluorescence and diffraction

Mainz

2011

Journal of Applied Physics

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In this work we present a method for the in situ analysis of elemental depth distributions in thin films using a combined evaluation of synchrotron x-ray fluorescence and energy-dispersive x-ray diffraction signals. We recorded diffraction and fluorescence signals simultaneously during the reactive annealing of thin films. By means of the observed diffraction signals, the time evolution of phases in the thin films during the annealing processes can be determined. We utilized this phase information to parameterize the depth distributions of the elements in the films. The timedependent fluorescence signals were then taken to determine the parameters representing the parameterized depth distributions. For this latter step, we numerically calculated the fluorescence intensities for a given set of depth distributions. These calculations handle polychromatic excitation and arbitrary functions of depth distributions and take into account primary and secondary fluorescence. Influences of lateral non-uniformities of the films, as well as the accuracy limits of the method, are investigated. We apply the introduced method to analyze the evolution of elemental depth distributions and to quantify the kinetic parameters during a synthesis process of CuInS 2 thin films via the reactive annealing of Cu-In precursors in a sulfur atmosphere.

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Section: Introductionmentioning

confidence: 99%

In situ analysis of elemental depth distributions in thin films by combined evaluation of synchrotron x-ray fluorescence and diffraction

Mainz

2011

Journal of Applied Physics

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“…Indium released in this transformation moves towards the bottom of the layer. The release of In has been found in Part 1 of this series [9]. The row of intermetallic transformations continues at around 320 1C (mark b in Fig.…”

Section: Cu X In Selenization With X41mentioning

confidence: 70%

“…While in the first [9] and second paper [10] we have analyzed the annealing of Cu-In precursor films and their reaction with elemental sulfur vapor, respectively, the third paper concentrates on selenization of Cu, In, Cu x In, and Cu 16 In 9 precursor films. Thereby particular focus is on the process dynamics and the kinetic limitations of the selenization.…”

Section: Introductionmentioning

confidence: 99%

Real-time studies of phase transformations in Cu–In–Se–S thin films—3: Selenization of Cu–In precursors

Djordjevic¹,

Rudigier²,

Scheer³

2006

Journal of Crystal Growth

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Phase transformations during selenization of thin films of elemental Cu, elemental In, and intermetallic Cu x In with x ¼ (1.8, 1.0, 0.8) are investigated using real-time energy dispersive X-ray diffraction. From the temporal development of the X-ray peak intensities, phase predominance sequence diagrams are constructed including the intensity ratio of the CuK a /InK a fluorescence lines. It was found that vapor selenization of Cu layers results in the formation of Cu 2Àx Se. At elevated temperature, linear growth of Cu 2Àx Se is observed which is interpreted as a surface controlled reaction mechanism. Indium selenization proceeds via the phase sequence In 4 Se 3 -InSe-In 2 Se 3 . During Cu x In selenization, the transformation sequence towards more Cu-rich intermetallic phases CuIn 2 -Cu 11 In 9 and Cu 11 In 9 -Cu 16 In 9 precedes the selenization process. During selenization of precursors with x41.4, this sequence continues bringing up the intermetallic phases Cu 7 In 3 and a-CuIn. The latter are formed at the bottom of the films. Thus, the bottom of the film becomes depleted from Indium by In diffusion. In general, the selenization process is slower than the sulfurization processes investigated in Part 2 of this study. A model is proposed which includes Cu 2Àx Se as a preliminary precursor for CuInSe 2 growth. This Cu 2Àx Se formation at the surface of the films is proposed to be surface reaction limited and is proposed to be the limiting step for the CuInSe 2 formation. Precursors with xp1 transform into CuInSe 2 with the participation of In-Se phases. r

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“…This study of the simultaneous sulfo-selenisation of metal precursors is intended to compare the formation reactions in a binary chalcogen atmosphere with the pure selenisation or sulfurisation of precursors. The selenisation and sulfurisation of Cu-In was studied by energy-dispersive X-ray diffraction (EDXRD) [11][12][13]. The selenisation and sulfurisation of Cu-In was studied by energy-dispersive X-ray diffraction (EDXRD) [11][12][13].…”

Section: Introductionmentioning

confidence: 99%

“…The reactions of pure copper or indium thin films with the chalcogen mixture S 0.5 Se 0.5 were investigated [10] to clarify the affinities of the metals to sulfur and selenium and to investigate the possible crystallisation of mixed metal sulfoselenides. The formation of the chalcopyrites CuInS 2 and CuInSe 2 reported in [11][12][13] proceeds differently and may be connected to a varied precursor assembly and the offer of sulfur by gas phase during the annealing. The formation of the chalcopyrites CuInS 2 and CuInSe 2 reported in [11][12][13] proceeds differently and may be connected to a varied precursor assembly and the offer of sulfur by gas phase during the annealing.…”

Section: Introductionmentioning

confidence: 99%

Real-time Investigations on the Formation of CuIn(S,Se)₂ while annealing precursors with varying sulfur content

Hölzing

Schurr

Jost³

et al. 2009

MRS Proc.

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CIS based chalcopyrite absorber materials are usually substituted in the cation and anion lattice to yield mixed pentanary crystals with the general composition Cu(In,Ga)(Se,S) 2 to achieve an optimised adaptation of the semiconductor bandgap to the terrestrial solar spectrum. Real-time investigations during the annealing of stacked elemental layers (SEL) of sputtered metals Cu and In and evaporated chalcogens S and Se with varying ratios were performed by angle-dispersive time-resolved XRD (X-ray diffraction) measurements. After qualitative phase analysis the measured powder diagrams were quantitatively analysed by the Rietveld method, the phases formed determined and their reaction kinetics obtained. Ternary indium and copper sulfoselenides form by the sulfoselenisation of the intermetallic alloy yielding different educts for the chalcopyrite formation with varying sulfur content. For S/(S+Se) ≥ 0.5 the formation of the chalcopyrite CuIn(S,Se) 2 is similar to the crystallisation path of CuInS 2 . With increasing amount of selenium (S/(S+Se) = 0.25) different ternary sulfoselenides contribute to the semiconductor formation. For small amounts of sulfur, i.e. S/(S+Se) ≤ 0.1, the chalcopyrite crystallisation proceeds comparable to the one observed for sulfur-free Cu-In-Se precursors. The formation of CuIn(S,Se) 2 is accelerated and proceeds mainly after the peritectic decomposition of Cu(S,Se) to Cu 2 (S,Se). The sulfur content determines the crystallisation temperature of the semiconductor because Cu(S,Se) decomposes at higher temperatures with increasing sulfur. Upon heating S ↔ Se exchange reactions take place in the Cu-S-Se and Cu-In-S-Se system.

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Real-time studies of phase transformations in Cu–In–Se–S thin films

Cited by 32 publications

References 19 publications

In situ analysis of elemental depth distributions in thin films by combined evaluation of synchrotron x-ray fluorescence and diffraction

In situ analysis of elemental depth distributions in thin films by combined evaluation of synchrotron x-ray fluorescence and diffraction

Real-time studies of phase transformations in Cu–In–Se–S thin films—3: Selenization of Cu–In precursors

Real-time Investigations on the Formation of CuIn(S,Se)₂ while annealing precursors with varying sulfur content

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Real-time studies of phase transformations in Cu–In–Se–S thin films

Cited by 32 publications

References 19 publications

In situ analysis of elemental depth distributions in thin films by combined evaluation of synchrotron x-ray fluorescence and diffraction

In situ analysis of elemental depth distributions in thin films by combined evaluation of synchrotron x-ray fluorescence and diffraction

Real-time studies of phase transformations in Cu–In–Se–S thin films—3: Selenization of Cu–In precursors

Real-time Investigations on the Formation of CuIn(S,Se)2 while annealing precursors with varying sulfur content

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Real-time Investigations on the Formation of CuIn(S,Se)₂ while annealing precursors with varying sulfur content