In Situ X-Ray Study During Thermal Cycle Treatment Combined with Complementary Ex Situ Investigation of InGaN Quantum Wells

In situ X-ray reciprocal space mapping was performed during the interval heating and cooling of InGaN/GaN quantum wells (QWs) grown via metal–organic vapor phase epitaxy (MOVPE). Our detailed in situ X-ray analysis enabled us to track changes in the peak intensities and radial and angular broadening...

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Main Authors: Ewa Grzanka, Sondes Bauer, Artur Lachowski, Szymon Grzanka, Robert Czernecki, Byeongchan So, Tilo Baumbach, Mike Leszczyński
Format: Article
Language:English
Published: MDPI AG 2025-01-01
Series:Nanomaterials
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Online Access:https://www.mdpi.com/2079-4991/15/2/140
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author Ewa Grzanka
Sondes Bauer
Artur Lachowski
Szymon Grzanka
Robert Czernecki
Byeongchan So
Tilo Baumbach
Mike Leszczyński
author_facet Ewa Grzanka
Sondes Bauer
Artur Lachowski
Szymon Grzanka
Robert Czernecki
Byeongchan So
Tilo Baumbach
Mike Leszczyński
author_sort Ewa Grzanka
collection DOAJ
description In situ X-ray reciprocal space mapping was performed during the interval heating and cooling of InGaN/GaN quantum wells (QWs) grown via metal–organic vapor phase epitaxy (MOVPE). Our detailed in situ X-ray analysis enabled us to track changes in the peak intensities and radial and angular broadenings of the reflection. By simulating the radial diffraction profiles recorded during the thermal cycle treatment, we demonstrate the presence of indium concentration distributions (ICDs) in the different QWs of the heterostructure (1. QW, bottom, 2. QW, middle, and 3. QW, upper). During the heating process, we found that the homogenization of the QWs occurred in the temperature range of 850 °C to 920 °C, manifesting in a reduction in ICDs in the QWs. Furthermore, there is a critical temperature (<i>T</i> = 940 °C) at which the mean value of the indium concentration starts to decrease below 15% in 1. QW, indicating the initiation of decomposition in 1. QW. Moreover, further heating up to 1000 °C results in extended diffuse scattering along the angular direction of the diffraction spot, confirming the propagation of the decomposition and the formation of trapezoidal objects, which contain voids and amorphous materials (In-Ga). Heating InGaN QWs up to <i>T</i> = 1000 °C led to a simultaneous decrease in the indium content and ICDs. During the cooling phase, there was no significant variation in the indium concentrations in the different QWs but rather an increase in the defect area, which contributes to the amplification of diffuse scattering. A comparison of ex situ complementary high-resolution transmission microscopy (Ex-HRTEM) measurements performed at room temperature before and after the thermal cycle treatment provides proof of the formation of four different types of defects in the QWs, which result from the decomposition of 1. QW during the heating phase. This, in turn, has strongly influenced the intensity of the photoluminescence emission spectra without any detectable shift in the emission wavelength λ<sub>MQWs</sub>.
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series Nanomaterials
spelling doaj-art-09f7e99405ec48cd909df21d4f3500d62025-01-24T13:44:17ZengMDPI AGNanomaterials2079-49912025-01-0115214010.3390/nano15020140In Situ X-Ray Study During Thermal Cycle Treatment Combined with Complementary Ex Situ Investigation of InGaN Quantum WellsEwa Grzanka0Sondes Bauer1Artur Lachowski2Szymon Grzanka3Robert Czernecki4Byeongchan So5Tilo Baumbach6Mike Leszczyński7Institute of High Pressure Physics, Polish Academy of Sciences, Sokolowska 29/37, 01-142 Warsaw, PolandInstitute for Photon Science and Synchrotron Radiation, Karlsruhe Institute of Technology, Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, GermanyInstitute of High Pressure Physics, Polish Academy of Sciences, Sokolowska 29/37, 01-142 Warsaw, PolandInstitute of High Pressure Physics, Polish Academy of Sciences, Sokolowska 29/37, 01-142 Warsaw, PolandInstitute of High Pressure Physics, Polish Academy of Sciences, Sokolowska 29/37, 01-142 Warsaw, PolandCompetence Center for III-Nitride Technology, C3NiT-Janzén, Solid State Physics and NanoLund, Lund University, P.O. Box 118, 22100 Lund, SwedenInstitute for Photon Science and Synchrotron Radiation, Karlsruhe Institute of Technology, Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, GermanyInstitute of High Pressure Physics, Polish Academy of Sciences, Sokolowska 29/37, 01-142 Warsaw, PolandIn situ X-ray reciprocal space mapping was performed during the interval heating and cooling of InGaN/GaN quantum wells (QWs) grown via metal–organic vapor phase epitaxy (MOVPE). Our detailed in situ X-ray analysis enabled us to track changes in the peak intensities and radial and angular broadenings of the reflection. By simulating the radial diffraction profiles recorded during the thermal cycle treatment, we demonstrate the presence of indium concentration distributions (ICDs) in the different QWs of the heterostructure (1. QW, bottom, 2. QW, middle, and 3. QW, upper). During the heating process, we found that the homogenization of the QWs occurred in the temperature range of 850 °C to 920 °C, manifesting in a reduction in ICDs in the QWs. Furthermore, there is a critical temperature (<i>T</i> = 940 °C) at which the mean value of the indium concentration starts to decrease below 15% in 1. QW, indicating the initiation of decomposition in 1. QW. Moreover, further heating up to 1000 °C results in extended diffuse scattering along the angular direction of the diffraction spot, confirming the propagation of the decomposition and the formation of trapezoidal objects, which contain voids and amorphous materials (In-Ga). Heating InGaN QWs up to <i>T</i> = 1000 °C led to a simultaneous decrease in the indium content and ICDs. During the cooling phase, there was no significant variation in the indium concentrations in the different QWs but rather an increase in the defect area, which contributes to the amplification of diffuse scattering. A comparison of ex situ complementary high-resolution transmission microscopy (Ex-HRTEM) measurements performed at room temperature before and after the thermal cycle treatment provides proof of the formation of four different types of defects in the QWs, which result from the decomposition of 1. QW during the heating phase. This, in turn, has strongly influenced the intensity of the photoluminescence emission spectra without any detectable shift in the emission wavelength λ<sub>MQWs</sub>.https://www.mdpi.com/2079-4991/15/2/140MOVPEInGaN QWsin situ X-ray diffractionannealingindium homogenizationthermal treatment
spellingShingle Ewa Grzanka
Sondes Bauer
Artur Lachowski
Szymon Grzanka
Robert Czernecki
Byeongchan So
Tilo Baumbach
Mike Leszczyński
In Situ X-Ray Study During Thermal Cycle Treatment Combined with Complementary Ex Situ Investigation of InGaN Quantum Wells
Nanomaterials
MOVPE
InGaN QWs
in situ X-ray diffraction
annealing
indium homogenization
thermal treatment
title In Situ X-Ray Study During Thermal Cycle Treatment Combined with Complementary Ex Situ Investigation of InGaN Quantum Wells
title_full In Situ X-Ray Study During Thermal Cycle Treatment Combined with Complementary Ex Situ Investigation of InGaN Quantum Wells
title_fullStr In Situ X-Ray Study During Thermal Cycle Treatment Combined with Complementary Ex Situ Investigation of InGaN Quantum Wells
title_full_unstemmed In Situ X-Ray Study During Thermal Cycle Treatment Combined with Complementary Ex Situ Investigation of InGaN Quantum Wells
title_short In Situ X-Ray Study During Thermal Cycle Treatment Combined with Complementary Ex Situ Investigation of InGaN Quantum Wells
title_sort in situ x ray study during thermal cycle treatment combined with complementary ex situ investigation of ingan quantum wells
topic MOVPE
InGaN QWs
in situ X-ray diffraction
annealing
indium homogenization
thermal treatment
url https://www.mdpi.com/2079-4991/15/2/140
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