This document discusses the use of synchrotron radiation for in-situ studies of the crystalline structure evolution during deposition of multilayer thin films. An experimental setup was designed with a reactive sputtering magnetron installed in an X-ray diffraction beamline at a synchrotron facility. This allowed for real-time X-ray diffraction patterns during film growth. Two deposition processes led to multilayer films with alternating amorphous and textured layers. Process A resulted in initial (10.0) and (00.2) orientation layers followed by (00.2), amorphous, and ending with (10.0). Process B began with an amorphous layer followed by alternating (00.2) and am

1. XIV Reunión Anual de la AACr Buenos Aires - 2018
THE USE OF SYNCHROTRON IN THE IN-SITU STUDIES OF
CRYSTALLINE STRUCTURES EVOLUTION DURING MULTILAYERED
THIN FILMS DEPOSITION ON SURFACES.
J. Bürghi1
; A. Craievich2
; G. Kellermann3
; J. Molleja4
; E. Bemporad5
and J. Feugeas1*
1
Instituto de Física Rosario, CONICET-UNR, Bv. 27 de Febrero 210bis. 2000 Rosario.
2
Instituto de Física, Universidade de São Paulo, Rua do Matão 1371 CEP 05508-090
São Paulo, Brazil.
3
Departamento de Física, Universidade Federal do Paraná, Caixa Postal 19044,
CEP81531-990 Curitiba, Brazil.
4
Yachay Tech University, School of Physical Sciences and Nanotechnology, 100119-
Urcuquí, Ecuador.
5
Department of Engineering, University of Rome “Roma Tre”, Via della Vasca Navale
79, 00146 Rome, Italy.
*feugeas@ifir-conicet.gov.ar
In this work we present the design, construction and first use of an experimental device
consisting of a specially designed chamber under vacuum equipped with a reactive
sputtering magnetron (RSM) [1] to be used for controlled deposition of thin films on a
flat substrate. The setup was designed to allow for in situ and real-time recordings of
X-ray diffraction patterns during the growth of deposited films and was installed in the
X-ray Diffraction and Spectroscopy beam line emerging from a superconducting
wiggler source at the Brazilian Synchrotron Light Laboratory [2]. The RSM setup was
used for in situ and real time X-ray diffraction studies of the process of growth of
multilayered wurzitic aluminum nitride thin films while the operation parameters of
the reactor were sequentially changed. In te past, in situ and real time studies using
synchrotron radiation were successfully used in kinetic of expanded austenite
development on the surface of austenitic stainless steel using ion nitriding process [3].
In the case of this work, the RSM sequential RSM led to the development of
multilayered films. Alternate variations in chamber pressure and magnetron power
density allowed us to obtain thin films composed of several micrometer thick layers,
with alternate amorphous and (10∙0), (00∙2) or (10∙1) textured polycrystalline
structures.
In particular, we present the results of two different processes (A and B) in which two
different sequences of layers with different textures were developed. In case A, a first
layer (on the substrate surface), a mixture of (10.0) and (00.2) orientation were
obtained, sequentially followed by other with (00.2), amorphous, and ended with one
with (10.0) orientation. The process B instead, develops a sequence with the first one
with amorphous structure, followed by a sequence of layers with (00.2) orientation,
amorphous, (00.2) and amorphous at the end.
The final structure of those multilayer films were ex-situ subsequently studied using
FIB end TEM techniques, showing the successive well differentiated layers but with a
columnar structure common to all of them.
Key words: Multilayer thin films, In-siyu X Ray diffracion, synchrotron, Sputter Magnetron
[1] J. Feugeas et al, Surf. Coat. Technol. 154 (2002) 167-175 ISSN 0257-8972
[2] https://www.lnls.cnpem.br/linhas-de-luz/xds/overview/
[3] G. Kellermann et al. Meth. in Phys. Res. A, 467-468, 1097-1100 (2001) ISSN: 0168-583X.