Every material experiences atomic and molecular motions that are generally termed vibrations in gases and liquids or phonons in solid state materials. Optical spectroscopy techniques, such as Raman, infrared absorption spectroscopy, or inelastic neutron scattering (INS), can be used to measure the vibrational/phonon spectrum of ground state materials properties. A variety of optical pump probe spectroscopies enable the measurement of excited states or elucidate photochemical reaction pathways and kinetics. So far, it has not been possible to study photoactive materials or processes in situ using INS due to the mismatch between neutron and photon penetration depths, differences between the flux density of photons and neutrons, cryogenic temperatures for INS measurements, vacuum conditions, and a lack of optical access to the sample space. These experimental hurdles have resulted in very limited photochemistry studies using INS. Here we report on the design of two different photochemistry sample sticks that overcome these experimental hurdles to enable in situ photochemical studies using INS, specifically at the VISION instrument at Oak Ridge National Laboratory. We demonstrate the use of these new measurement capabilities through (1) the in situ photodimerization of anthracene and (2) the in situ photopolymerization of a 405 nm photoresin using 405 nm excitation as simple test cases. These new measurement apparatus broaden the science enabled by INS to include photoactive materials, optically excited states, and photoinitiated reactions.
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August 2023
Research Article|
August 04 2023
Photochemistry sample sticks for inelastic neutron scattering
Daniel Vong
;
Daniel Vong
(Conceptualization, Data curation, Formal analysis, Investigation, Methodology, Writing – original draft, Writing – review & editing)
1
Department of Materials Science and Engineering, University of California Davis
, 1 Shields Ave., Davis, California 95616, USA
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Eric C. Novak
;
Eric C. Novak
(Conceptualization, Data curation, Investigation, Resources, Supervision, Writing – review & editing)
2
Neutron Scattering Division, Oak Ridge National Laboratory
, Oak Ridge, Tennessee 37830, USA
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Adam J. Moulé
;
Adam J. Moulé
(Conceptualization, Funding acquisition, Supervision, Writing – review & editing)
3
Department of Chemical Engineering, University of California Davis
, 1 Shields Ave., Davis, California 95616, USA
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Luke L. Daemen
Luke L. Daemen
a)
(Conceptualization, Data curation, Funding acquisition, Investigation, Resources, Supervision, Writing – review & editing)
2
Neutron Scattering Division, Oak Ridge National Laboratory
, Oak Ridge, Tennessee 37830, USA
a)Author to whom correspondence should be addressed: [email protected]
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a)Author to whom correspondence should be addressed: [email protected]
Rev. Sci. Instrum. 94, 085102 (2023)
Article history
Received:
April 14 2023
Accepted:
July 18 2023
Citation
Daniel Vong, Eric C. Novak, Adam J. Moulé, Luke L. Daemen; Photochemistry sample sticks for inelastic neutron scattering. Rev. Sci. Instrum. 1 August 2023; 94 (8): 085102. https://doi.org/10.1063/5.0154605
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