In situ investigation of decomposing ammonia and ammonobasic solutions under supercritical conditions via UV/vis and Raman Spectroscopy
[Display omitted] •Visualization of temperature dependence of NH3 decomposing to N2 and H2.•Maximum temperature in the autoclave = 563 °C, at heating temperature = 617 °C.•Maximum pressure = 254 MPa.•In situ Raman spectra in the range of 200–4500 cm−1. An optical cell was used in this work, which al...
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| Published in: | The Journal of supercritical fluids Vol. 134; pp. 96 - 105 |
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01-04-2018
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| Abstract | [Display omitted]
•Visualization of temperature dependence of NH3 decomposing to N2 and H2.•Maximum temperature in the autoclave = 563 °C, at heating temperature = 617 °C.•Maximum pressure = 254 MPa.•In situ Raman spectra in the range of 200–4500 cm−1.
An optical cell was used in this work, which allows spectroscopic measurements of fluids up to 600 °C and 300 MPa. The maximum pressure reached in this work was 254 MPa and the internal cell temperature was a maximum of 563 °C at a heating temperature of 617 °C. In the following, a combination of Raman and UV/vis spectroscopy was used for in situ investigation of the breakdown of sodium azide above 300 °C combined with the formation of sodium amide. It was verified that the breakdown of NaN3 occurs before the formation of NaNH2 starts.
In a second step the decomposition of supercritical ammonia under ammonothermal conditions was investigated solely via Raman spectroscopy. The study comprises four different fluid compositions: pure ammonia, ammonia with a ruthenium catalyst, ammonia and mineralizer (sodium azide) and last ammonia, mineralizer and gallium nitride (GaN). By this, it was possible to proof that with pure ammonia and without a proper catalyst the decomposition of ammonia stops quite far before chemical equilibrium is reached. |
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| AbstractList | [Display omitted]
•Visualization of temperature dependence of NH3 decomposing to N2 and H2.•Maximum temperature in the autoclave = 563 °C, at heating temperature = 617 °C.•Maximum pressure = 254 MPa.•In situ Raman spectra in the range of 200–4500 cm−1.
An optical cell was used in this work, which allows spectroscopic measurements of fluids up to 600 °C and 300 MPa. The maximum pressure reached in this work was 254 MPa and the internal cell temperature was a maximum of 563 °C at a heating temperature of 617 °C. In the following, a combination of Raman and UV/vis spectroscopy was used for in situ investigation of the breakdown of sodium azide above 300 °C combined with the formation of sodium amide. It was verified that the breakdown of NaN3 occurs before the formation of NaNH2 starts.
In a second step the decomposition of supercritical ammonia under ammonothermal conditions was investigated solely via Raman spectroscopy. The study comprises four different fluid compositions: pure ammonia, ammonia with a ruthenium catalyst, ammonia and mineralizer (sodium azide) and last ammonia, mineralizer and gallium nitride (GaN). By this, it was possible to proof that with pure ammonia and without a proper catalyst the decomposition of ammonia stops quite far before chemical equilibrium is reached. |
| Author | Hertweck, Benjamin Balouschek, Johannes Steigerwald, Thomas G. Kimmel, Anna-Carina L. Alt, Nicolas S.A. Schluecker, Eberhard |
| Author_xml | – sequence: 1 givenname: Thomas G. surname: Steigerwald fullname: Steigerwald, Thomas G. email: sd@ipat.fau.de organization: Institute of Process Machinery and Systems Engineering, Friedrich-Alexander-Universitaet Erlangen-Nuernberg, Germany – sequence: 2 givenname: Johannes surname: Balouschek fullname: Balouschek, Johannes organization: Institute of Process Machinery and Systems Engineering, Friedrich-Alexander-Universitaet Erlangen-Nuernberg, Germany – sequence: 3 givenname: Benjamin surname: Hertweck fullname: Hertweck, Benjamin organization: Institute of Process Machinery and Systems Engineering, Friedrich-Alexander-Universitaet Erlangen-Nuernberg, Germany – sequence: 4 givenname: Anna-Carina L. surname: Kimmel fullname: Kimmel, Anna-Carina L. organization: Institute of Process Machinery and Systems Engineering, Friedrich-Alexander-Universitaet Erlangen-Nuernberg, Germany – sequence: 5 givenname: Nicolas S.A. surname: Alt fullname: Alt, Nicolas S.A. organization: Institute of Process Machinery and Systems Engineering, Friedrich-Alexander-Universitaet Erlangen-Nuernberg, Germany – sequence: 6 givenname: Eberhard surname: Schluecker fullname: Schluecker, Eberhard organization: Institute of Process Machinery and Systems Engineering, Friedrich-Alexander-Universitaet Erlangen-Nuernberg, Germany |
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| Cites_doi | 10.1016/j.supflu.2015.07.032 10.1016/j.jcat.2004.12.013 10.3390/inorganics2010029 10.1021/j100563a010 10.1039/C2EE02865D 10.1016/S1464-2859(13)70332-8 10.1016/j.jcrysgro.2014.06.013 10.1021/cg050271r 10.1021/ja01667a011 10.1016/j.apcata.2015.11.024 10.1006/jcat.1997.1877 10.1063/1.1563591 10.1002/pssc.201100361 10.1016/j.jcrysgro.2014.06.015 10.1039/b922045c 10.1021/ic50051a001 10.1016/j.ijhydene.2013.09.054 10.1002/ceat.201300719 10.1016/j.apcata.2007.01.029 10.1016/j.supflu.2014.08.006 |
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| Keywords | UV/vis spectroscopy Supercritical ammonia Raman spectroscopy Ammonia decomposition Ammonothermal crystal growth |
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Chem. doi: 10.1021/ic50051a001 contributor: fullname: Kirschke – volume: 38 year: 2013 ident: 10.1016/j.supflu.2017.12.028_bib0010 article-title: Review of electrochemical ammonia production technologies and materials publication-title: Int. J. Hydrogen Energy doi: 10.1016/j.ijhydene.2013.09.054 contributor: fullname: Giddey – volume: 37 start-page: 1903 year: 2014 ident: 10.1016/j.supflu.2017.12.028_bib0055 article-title: Corrosive degeneration of autoclaves for the ammonothermal synthesis: experimental approach and first results publication-title: Chem. Eng. {&} Technol. doi: 10.1002/ceat.201300719 contributor: fullname: Hertweck – year: 2015 ident: 10.1016/j.supflu.2017.12.028_bib0075 contributor: fullname: Braeuer – volume: 320 year: 2007 ident: 10.1016/j.supflu.2017.12.028_bib0025 article-title: Catalytic ammonia decomposition over Ru/carbon catalysts: the importance of the structure of carbon support publication-title: Appl. Catal. A Gen. doi: 10.1016/j.apcata.2007.01.029 contributor: fullname: Li – volume: 95 start-page: 158 year: 2014 ident: 10.1016/j.supflu.2017.12.028_bib0130 article-title: Different corrosion behaviour of autoclaves made of nickel base alloy 718 in ammonobasic and ammonoacidic environments publication-title: J. Supercrit. Fluids doi: 10.1016/j.supflu.2014.08.006 contributor: fullname: Hertweck |
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| Title | In situ investigation of decomposing ammonia and ammonobasic solutions under supercritical conditions via UV/vis and Raman Spectroscopy |
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