In-situ studies of the recrystallization process of CuInS2 thin films by energy dispersive X-ray diffraction

AbstractChalcopyrite CuInS2 and the structurally related kesterite Cu2ZnSnS4 are known as photovoltaic absorber materials. In this study different precursor thin films of the quaternary Cu-Zn-Sn-S system (stacking: Mo/CuS/ZnS-SnS) and of the pentenary Cu-In-Zn-Sn-S system (stacking: Mo/CuIn/ZnS-SnS) were annealed in sulfur atmosphere. The predominant crystalline phases were detected by in-situ energy dispersive X-ray diffraction (EDXRD). Additionally the X-ray fluorescence signals of the film components were recorded to detect diffusion effects. For the quaternary system we found ZnS, CuS, Cu2-xS, Sn2S3 and SnS as main binary phases during annealing. The Sn2S3-SnS phase transition had a significant impact on the later formation of ternary/quaternary phases. A high diffusivity of copper can explain the little influence of the precursor stacking on the reaction path and may also be responsible for the poor adhesion of the films. For annealing temperatures above 450°C Cu2ZnSnS4 can be identified clearly by XRD. The incorporation of indium in the system leads to new diffraction peaks which can be explained by the formation of solid solutions in the system CuInS2-Cu2ZnSnS4.

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In-situ Studies of Lithium/Silver Vanadium Phosphorous Oxide Batteries Using Synchrotron based Energy Dispersive X-ray Diffraction

ECS Transactions ◽

10.1149/06609.0247ecst ◽

2015 ◽

Vol 66 (9) ◽

pp. 247-255 ◽

Cited By ~ 1

Author(s):

Y. R. Li ◽

K. C. Kirshenbaum ◽

K. J. Takeuchi ◽

A. C. Marschilok ◽

E. S. Takeuchi

Keyword(s):

Energy Dispersive ◽

X Ray Diffraction ◽

X Ray ◽

In Situ Studies ◽

Silver Vanadium Phosphorous Oxide

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In-situ energy-dispersive X-ray diffraction of metal sulfide assisted crystallization of strongly (001) textured photoactive tungsten disulfide thin films

Thin Solid Films ◽

10.1016/j.tsf.2008.11.118 ◽

2009 ◽

Vol 517 (10) ◽

pp. 3148-3151 ◽

Cited By ~ 12

Author(s):

S. Brunken ◽

R. Mientus ◽

K. Ellmer

Keyword(s):

Thin Films ◽

Metal Sulfide ◽

Tungsten Disulfide ◽

Energy Dispersive ◽

X Ray Diffraction ◽

X Ray

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Pressure Dependent Rapid Thermal Processing of CuInS2 Thin Films Investigated by In-Situ Energy Dispersive X-ray Diffraction

MRS Proceedings ◽

10.1557/proc-1012-y13-09 ◽

2007 ◽

Vol 1012 ◽

Cited By ~ 1

Author(s):

Immo Michael Kötschau ◽

Humberto Rodriguez-Alvarez ◽

Cornelia Streeck ◽

Alfons Weber ◽

Manuela Klaus ◽

...

Keyword(s):

Thin Films ◽

Partial Pressure ◽

Thermal Processing ◽

Reaction Pathway ◽

Rapid Thermal Processing ◽

Energy Dispersive ◽

X Ray Diffraction ◽

Crystalline Phases ◽

X Ray

AbstractThe rapid thermal processing (RTP) of Cu-rich Cu/In precursors for the synthesis of CuInS2 thin films is possible within a broad processing window regarding leading parameters like top temperature, heating rate, and Cu excess. The key reaction pathway for the CuInS2 phase formation has already been investigated by in-situ energy dispersive X-ray diffraction (EDXRD) for various precursor stoichiometries, heating rates and top temperatures at sulphur partial pressure conditions which are typical for physical vapour deposition processes. According to the phase diagrams of the binary sulphide phases, the sulfur partial pressure strongly determines the occuring crystalline phases. However, a controlled variation of the maximum sulphur partial in a typical RTP experiment has not been carried out yet. In order to study the influence of this parameter a special RTP reaction chamber was designed suitable for in-situ EDXRD experiments at the EDDI beamline at BESSY, Berlin. In a typical in-situ RTP/EDXRD experiment sulphur and a Cu/In/Mo/glass precursor are placed in an evacuated graphite reactor. The amount of sulphur determines the maximum pressure available at the top temperature of the experiment. As the RTP process proceeds a complete EDXRD spectrum is acquired every 10 seconds and thus the various stages of the reaction path and the crystalline phases can be monitored. The first experiments show already a significant change in the reaction pathway and the secondary Cu-S phases which segregate on top of the CuInS2 thin film during the reaction.

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In-situ studies of the hydrothermal synthesis of zeolites using synchrotron energy-dispersive X-ray diffraction

Phase Transitions ◽

10.1080/01411599208203476 ◽

1992 ◽

Vol 39 (1-4) ◽

pp. 129-134 ◽

Cited By ~ 40

Author(s):

J. Munn ◽

P. Barnes ◽

D. Häusermann ◽

S. A. Axon ◽

J. Klinowski

Keyword(s):

Hydrothermal Synthesis ◽

Energy Dispersive ◽

X Ray Diffraction ◽

X Ray ◽

In Situ Studies

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In Situ Recrystallization of Co-Evaporated Cu(In,Ga)Se2 Thin Films by Copper Chloride Vapor Treatment towards Solar Cell Applications

Energies ◽

10.3390/en14133938 ◽

2021 ◽

Vol 14 (13) ◽

pp. 3938

Author(s):

Deewakar Poudel ◽

Benjamin Belfore ◽

Tasnuva Ashrafee ◽

Elizabeth Palmiotti ◽

Shankar Karki ◽

...

Keyword(s):

Thin Films ◽

Secondary Ion Mass Spectrometry ◽

Copper Chloride ◽

Recrystallization Process ◽

X Ray Diffraction ◽

X Ray ◽

Stage Process ◽

Secondary Ion ◽

Vapor Treatment

Cu(In,Ga)Se2 (or CIGS) thin films and devices were fabricated using a modified three-stage process. Using high deposition rates and a low temperature during the process, a copper chloride vapor treatment was introduced in between the second and third stages to enhance the films properties. X-ray diffraction and scanning electron microscopy demonstrate that drastic changes occur after this recrystallization process, yielding films with much larger grains. Secondary ion mass spectrometry shows that the depth profile of many elements is not modified (such as Cu, In and Se) while others change dramatically (such as Ga and Na). Because of the competing effects of these changes, not all parameters of the solar cells are enhanced, yielding an increase of 15% in the device efficiency at the most.

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In situ Characterization of Functional Organic Thin Films by Energy Dispersive Grazing Incidence X-ray Diffraction

MRS Proceedings ◽

10.1557/proc-502-151 ◽

1997 ◽

Vol 502 ◽

Author(s):

Yuji Yoshida ◽

Hiroshi Takiguchi ◽

Nobutaka Tanigaki ◽

Kiyoshi Yase

Keyword(s):

Thin Films ◽

Growth Process ◽

Organic Thin Films ◽

Grazing Incidence ◽

Energy Dispersive ◽

Vacuum System ◽

Initial Growth ◽

X Ray Diffraction ◽

X Ray

ABSTRACTWe are investigating well-ordered highly crystalline thin films made using organic molecular beam deposition (OMBD) since it is important to control the formation mechanism at the initial growth process. Then, we developed a new in situ technique of energy dispersive grazing incidence X-ray diffraction utilized within an ultrahigh vacuum system. This technique (in situ ED-GID) makes it possible to examine the crystal structure, orientation and morphology of organic thin films during deposition without any damage to the film. In the present review, we examined the growth process of thin films of functional organic dyes, fullerene (C60) and p-sexiphenyl (6P) by using this in situ ED-GID. The crystal strucutre and molecular orientation in epitaxially-grown thin films were confirmed during the initial stages of growth. Also, the morphology of C60 thin films was examined during the deposition. As a result, it was confirmed that the decay curves of X-ray fluorescence indicate different island growth in C60 thin films.

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In Situ Synchrotron X-Ray Diffraction Study of a Deformed Cu-Fe-P Alloy during Heating

Materials Science Forum ◽

10.4028/www.scientific.net/msf.850.191 ◽

2016 ◽

Vol 850 ◽

pp. 191-196 ◽

Cited By ~ 1

Author(s):

Wei Wang ◽

Cun Lei Zou ◽

Ren Geng Li ◽

Wen Wen ◽

Hui Jun Kang ◽

...

Keyword(s):

Room Temperature ◽

Lattice Distortion ◽

Copper Matrix ◽

Heating Process ◽

Recrystallization Process ◽

Full Width ◽

X Ray Diffraction ◽

Dramatic Decrease ◽

X Ray

In situ synchrotron X-ray diffraction was used to study a deformed Cu-0.88 Fe-0.24 P alloy during heating process. The measurements were performed at room temperature and also at high temperatures up to 893 K in order to determine the recovery, ageing and recrystallization process. With the increase of temperature, the angles of copper matrix peaks moved left and the FWHM (full width at half maximum) decreased slightly. Fe3P precipitates were first detected at 533 K, reached the maximum at 673 K, and re-dissolved into matrix at 853 K. A dramatic decrease in FWHM was observed accompanied by the precipitation of Fe3P phases, indicating the reduction of lattice distortion of copper matrix.

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