Real-time studies of phase transformations in Cu–In–Se–S thin films 2. Sulfurization of Cu–In precursors

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

doi:10.1016/j.jcrysgro.2005.10.106

Cited by 42 publications

(30 citation statements)

References 23 publications

(44 reference statements)

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“…We exploit the fact that in energydispersive x-ray diffraction (EDXRD), diffraction signals and fluorescence signals, are measured simultaneously. 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.…”

Section: Introductionmentioning

confidence: 99%

“…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%

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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%

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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“…2 Theta (degree) phase typically begins to occur during sulfurization at a temperature between 250 and 320°C as mentioned above [9,10,12,19]. Concurrently Cu 16 In 9 appears as it is thermodynamically stable between 310 and 389°C [20].…”

Section: Resultsmentioning

confidence: 99%

“…198CuInS 2 + 154CuS. The use of elemental sulfur during sulfurization was also studied using in situ XRD analysis [12]. The following reaction was proposed: 4Cu 11 In 9 + 9S 8 ?…”

Section: Introductionmentioning

confidence: 99%

Ex situ structural characterization during the formation of CuInS2 thin films

2011

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“…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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Real-time studies of phase transformations in Cu–In–Se–S thin films 2. Sulfurization of Cu–In precursors

Cited by 42 publications

References 23 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

Ex situ structural characterization during the formation of CuInS2 thin films

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

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