skip to main content
OSTI.GOV title logo U.S. Department of Energy
Office of Scientific and Technical Information

Title: Soft x-ray spectroscopy of high pressure liquid

Abstract

Here, we describe a new experimental technique that allows for soft x-ray spectroscopy studies (~100-1000 eV) of high pressure liquid (~100 bars). We achieve this through a liquid cell with a 100 nm-thick Si 3N 4 membrane window, which is sandwiched by two identical O-rings for vacuum sealing. The thin Si 3N 4 membrane allows soft x-rays to penetrate, while separating the high-pressure liquid under investigation from the vacuum required for soft x-ray transmission and detection. The burst pressure of the Si 3N 4 membrane increases with decreasing size and more specifically is inversely proportional to the side length of the square window. It also increases proportionally with the membrane thickness. Pressures > 60 bars could be achieved for 100 nm-thick square Si 3N 4 windows that are smaller than 65 μm. However, above a certain pressure, the failure of the Si wafer becomes the limiting factor. The failure pressure of the Si wafer is sensitive to the wafer thickness. Moreover, the deformation of the Si 3N 4 membrane is quantified using vertical scanning interferometry. As an example of the performance of the high-pressure liquid cell optimized for total-fluorescence detected soft x-ray absorption spectroscopy (sXAS), the sXAS spectra at themore » Ca L edge (~350 eV) of a CaCl 2 aqueous solution are collected under different pressures up to 41 bars.« less

Authors:
 [1];  [2];  [1];  [3];  [1];  [1];  [1]; ORCiD logo [4];  [4];  [5];  [4];  [1]; ORCiD logo [1];  [1];  [6];  [3]; ORCiD logo [1]
  1. Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States). Advanced Light Source (ALS)
  2. Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States). Advanced Light Source (ALS); Soochow Univ., Jiangsu (China). Jiangsu Key Lab. for Carbon-Based Functional Materials and Devices, Inst. of Functional Nano and Soft Materials (FUNSOM) and Joint International Research Lab. of Carbon-Based Functional Materials and Devices
  3. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Center for X-Ray Optic
  4. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Energy Geoscience Division
  5. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Engineering Division
  6. Jiangsu Key Laboratory for Carbon-Based Functional Materials &, Devices, Institute of Functional Nano &, Soft Materials (FUNSOM), Joint International Research Laboratory of Carbon-Based Functional Materials and Devices, Soochow University, Suzhou 215123, Jiangsu, China
Publication Date:
Research Org.:
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22); National Natural Science Foundation of China (NNSFC)
OSTI Identifier:
1436167
Alternate Identifier(s):
OSTI ID: 1418709
Grant/Contract Number:  
AC02-05CH11231; U1432249
Resource Type:
Journal Article: Accepted Manuscript
Journal Name:
Review of Scientific Instruments
Additional Journal Information:
Journal Volume: 89; Journal Issue: 1; Journal ID: ISSN 0034-6748
Publisher:
American Institute of Physics (AIP)
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; 46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND TECHNOLOGY; materials properties; x-ray spectroscopy; semiconductors; etching; interferometry; light sensitive materials; chemical compounds; absorption spectra

Citation Formats

Qiao, Ruimin, Xia, Yujian, Feng, Xuefei, Macdougall, James, Pepper, John, Armitage, Kevin, Borsos, Jason, Knauss, Kevin G., Lee, Namhey, Allezy, Arnaud, Gilbert, Benjamin, MacDowell, Alastair A., Liu, Yi-Sheng, Glans, Per-Anders, Sun, Xuhui, Chao, Weilun, and Guo, Jinghua. Soft x-ray spectroscopy of high pressure liquid. United States: N. p., 2018. Web. doi:10.1063/1.5008444.
Qiao, Ruimin, Xia, Yujian, Feng, Xuefei, Macdougall, James, Pepper, John, Armitage, Kevin, Borsos, Jason, Knauss, Kevin G., Lee, Namhey, Allezy, Arnaud, Gilbert, Benjamin, MacDowell, Alastair A., Liu, Yi-Sheng, Glans, Per-Anders, Sun, Xuhui, Chao, Weilun, & Guo, Jinghua. Soft x-ray spectroscopy of high pressure liquid. United States. doi:10.1063/1.5008444.
Qiao, Ruimin, Xia, Yujian, Feng, Xuefei, Macdougall, James, Pepper, John, Armitage, Kevin, Borsos, Jason, Knauss, Kevin G., Lee, Namhey, Allezy, Arnaud, Gilbert, Benjamin, MacDowell, Alastair A., Liu, Yi-Sheng, Glans, Per-Anders, Sun, Xuhui, Chao, Weilun, and Guo, Jinghua. Mon . "Soft x-ray spectroscopy of high pressure liquid". United States. doi:10.1063/1.5008444. https://www.osti.gov/servlets/purl/1436167.
@article{osti_1436167,
title = {Soft x-ray spectroscopy of high pressure liquid},
author = {Qiao, Ruimin and Xia, Yujian and Feng, Xuefei and Macdougall, James and Pepper, John and Armitage, Kevin and Borsos, Jason and Knauss, Kevin G. and Lee, Namhey and Allezy, Arnaud and Gilbert, Benjamin and MacDowell, Alastair A. and Liu, Yi-Sheng and Glans, Per-Anders and Sun, Xuhui and Chao, Weilun and Guo, Jinghua},
abstractNote = {Here, we describe a new experimental technique that allows for soft x-ray spectroscopy studies (~100-1000 eV) of high pressure liquid (~100 bars). We achieve this through a liquid cell with a 100 nm-thick Si3N4 membrane window, which is sandwiched by two identical O-rings for vacuum sealing. The thin Si3N4 membrane allows soft x-rays to penetrate, while separating the high-pressure liquid under investigation from the vacuum required for soft x-ray transmission and detection. The burst pressure of the Si3N4 membrane increases with decreasing size and more specifically is inversely proportional to the side length of the square window. It also increases proportionally with the membrane thickness. Pressures > 60 bars could be achieved for 100 nm-thick square Si3N4 windows that are smaller than 65 μm. However, above a certain pressure, the failure of the Si wafer becomes the limiting factor. The failure pressure of the Si wafer is sensitive to the wafer thickness. Moreover, the deformation of the Si3N4 membrane is quantified using vertical scanning interferometry. As an example of the performance of the high-pressure liquid cell optimized for total-fluorescence detected soft x-ray absorption spectroscopy (sXAS), the sXAS spectra at the Ca L edge (~350 eV) of a CaCl2 aqueous solution are collected under different pressures up to 41 bars.},
doi = {10.1063/1.5008444},
journal = {Review of Scientific Instruments},
issn = {0034-6748},
number = 1,
volume = 89,
place = {United States},
year = {2018},
month = {1}
}

Journal Article:
Free Publicly Available Full Text
Publisher's Version of Record

Citation Metrics:
Cited by: 1 work
Citation information provided by
Web of Science

Figures / Tables:

FIG. 1. FIG. 1.: Si3N4 membrane window and the high-pressure soft x-ray cell. (a) Front view of the Si3N4 window. (b) A diagram showing the principle of the high-pressure cell. (c) The assembly drawing of the high-pressure soft x-ray cell.

Save / Share:

Works referenced in this record:

A liquid flow cell to study the electronic structure of liquids with soft X-rays
journal, February 2008

  • Fuchs, Oliver; Maier, Florian; Weinhardt, Lothar
  • Nuclear Instruments and Methods in Physics Research Section A: Accelerators, Spectrometers, Detectors and Associated Equipment, Vol. 585, Issue 3
  • DOI: 10.1016/j.nima.2007.10.029

Setup for in situ investigation of gases and gas/solid interfaces by soft x-ray emission and absorption spectroscopy
journal, January 2014

  • Benkert, A.; Blum, M.; Meyer, F.
  • Review of Scientific Instruments, Vol. 85, Issue 1
  • DOI: 10.1063/1.4862059

Development of a liquid flow cell to measure soft X-ray absorption in transmission mode: A test for liquid water
journal, March 2010

  • Nagasaka, Masanari; Hatsui, Takaki; Horigome, Toshio
  • Journal of Electron Spectroscopy and Related Phenomena, Vol. 177, Issue 2-3
  • DOI: 10.1016/j.elspec.2009.11.001

Supercritical and near-critical CO2 in green chemical synthesis and processing
journal, March 2004


Anisotropic Etching of Silicon
journal, October 1969


Electrochemical flowcell for in-situ investigations by soft x-ray absorption and emission spectroscopy
journal, October 2014

  • Schwanke, C.; Golnak, R.; Xiao, J.
  • Review of Scientific Instruments, Vol. 85, Issue 10
  • DOI: 10.1063/1.4899063

Polymers with Tailored Electronic Structure for High Capacity Lithium Battery Electrodes
journal, September 2011

  • Liu, Gao; Xun, Shidi; Vukmirovic, Nenad
  • Advanced Materials, Vol. 23, Issue 40, p. 4679-4683
  • DOI: 10.1002/adma.201102421

Development and application of in situ/operando soft X-ray transmission cells to aqueous solutions and catalytic and electrochemical reactions
journal, April 2015

  • Nagasaka, Masanari; Yuzawa, Hayato; Kosugi, Nobuhiro
  • Journal of Electron Spectroscopy and Related Phenomena, Vol. 200
  • DOI: 10.1016/j.elspec.2015.05.012

The Nanoscale Basis of CO 2 Trapping for Geologic Storage
journal, August 2015

  • Bourg, Ian C.; Beckingham, Lauren E.; DePaolo, Donald J.
  • Environmental Science & Technology, Vol. 49, Issue 17
  • DOI: 10.1021/acs.est.5b03003

In operando observation system for electrochemical reaction by soft X-ray absorption spectroscopy with potential modulation method
journal, October 2014

  • Nagasaka, Masanari; Yuzawa, Hayato; Horigome, Toshio
  • Review of Scientific Instruments, Vol. 85, Issue 10
  • DOI: 10.1063/1.4898054

A reaction cell with sample laser heating for in situ soft X-ray absorption spectroscopy studies under environmental conditions
journal, March 2013

  • Escudero, Carlos; Jiang, Peng; Pach, Elzbieta
  • Journal of Synchrotron Radiation, Vol. 20, Issue 3
  • DOI: 10.1107/s0909049513002434

Direct evidence of gradient Mn(II) evolution at charged states in LiNi0.5Mn1.5O4 electrodes with capacity fading
journal, January 2015


Direct probe of Mott-Hubbard to charge-transfer insulator transition and electronic structure evolution in transition-metal systems
journal, June 2011


An ultra-high vacuum electrochemical flow cell for in situ / operando soft X-ray spectroscopy study
journal, April 2014

  • Bora, Debajeet K.; Glans, Per-Anders; Pepper, John
  • Review of Scientific Instruments, Vol. 85, Issue 4
  • DOI: 10.1063/1.4870795

Geochemical evolution of organic-rich shales with increasing maturity: A STXM and TEM study of the Posidonia Shale (Lower Toarcian, northern Germany)
journal, March 2012


Covalency in oxidized uranium
journal, July 2015


Revealing and suppressing surface Mn(II) formation of Na0.44MnO2 electrodes for Na-ion batteries
journal, September 2015


Nanoscale chemical imaging of a working catalyst by scanning transmission X-ray microscopy
journal, November 2008

  • de Smit, Emiel; Swart, Ingmar; Creemer, J. Fredrik
  • Nature, Vol. 456, Issue 7219
  • DOI: 10.1038/nature07516

A sample holder for soft x-ray absorption spectroscopy of liquids in transmission mode
journal, October 2011

  • Schreck, Simon; Gavrila, Gianina; Weniger, Christian
  • Review of Scientific Instruments, Vol. 82, Issue 10
  • DOI: 10.1063/1.3644192

Characterization of the Acetonitrile Aqueous Solution/Vapor Interface by Liquid-Jet X-ray Photoelectron Spectroscopy
journal, September 2014

  • Perrine, Kathryn A.; Van Spyk, Marijke H. C.; Margarella, Alexandria M.
  • The Journal of Physical Chemistry C, Vol. 118, Issue 50
  • DOI: 10.1021/jp505947h

First experimental results from IBM/TENN/TULANE/LLNL/LBL undulator beamline at the advanced light source
journal, February 1995

  • Jia, J. J.; Callcott, T. A.; Yurkas, J.
  • Review of Scientific Instruments, Vol. 66, Issue 2
  • DOI: 10.1063/1.1145985

Probing ore deposits formation: New insights and challenges from synchrotron and neutron studies
journal, February 2010


Photochemical and Photoelectrochemical Reduction of CO 2
journal, May 2012


Liquid microjet for photoelectron spectroscopy
journal, March 2009

  • Winter, Bernd
  • Nuclear Instruments and Methods in Physics Research Section A: Accelerators, Spectrometers, Detectors and Associated Equipment, Vol. 601, Issue 1-2
  • DOI: 10.1016/j.nima.2008.12.108

Direct Experimental Probe of the Ni(II)/Ni(III)/Ni(IV) Redox Evolution in LiNi 0.5 Mn 1.5 O 4 Electrodes
journal, November 2015

  • Qiao, Ruimin; Wray, L. Andrew; Kim, Jung-Hyun
  • The Journal of Physical Chemistry C, Vol. 119, Issue 49
  • DOI: 10.1021/acs.jpcc.5b07479

Bivalence Mn5O8 with hydroxylated interphase for high-voltage aqueous sodium-ion storage
journal, November 2016

  • Shan, Xiaoqiang; Charles, Daniel S.; Lei, Yinkai
  • Nature Communications, Vol. 7, Issue 1
  • DOI: 10.1038/ncomms13370

Geochemistry of geothermal fluids and well scales, and potential for mineral recovery
journal, June 1998


High-efficiency in situ resonant inelastic x-ray scattering (iRIXS) endstation at the Advanced Light Source
journal, March 2017

  • Qiao, Ruimin; Li, Qinghao; Zhuo, Zengqing
  • Review of Scientific Instruments, Vol. 88, Issue 3
  • DOI: 10.1063/1.4977592

In-situ X-ray absorption study of Iron(II) speciation in brines up to supercritical conditions
journal, June 2009


Phase Transformation and Lithiation Effect on Electronic Structure of Li x FePO 4 : An In-Depth Study by Soft X-ray and Simulations
journal, August 2012

  • Liu, Xiaosong; Liu, Jun; Qiao, Ruimin
  • Journal of the American Chemical Society, Vol. 134, Issue 33
  • DOI: 10.1021/ja303225e

A soft XAS transmission cell for operando studies
journal, October 2016

  • Schwanke, Christoph; Xi, Lifei; Lange, Kathrin Maria
  • Journal of Synchrotron Radiation, Vol. 23, Issue 6
  • DOI: 10.1107/s1600577516014697

Phase transitions in biogenic amorphous calcium carbonate
journal, April 2012

  • Gong, Y. U. T.; Killian, C. E.; Olson, I. C.
  • Proceedings of the National Academy of Sciences, Vol. 109, Issue 16
  • DOI: 10.1073/pnas.1118085109

The development of in situ photon-in/photon-out soft X-ray spectroscopy on beamline 7.0.1 at the ALS
journal, June 2013


Fine structure of the Ca 2 p x-ray-absorption edge for bulk compounds, surfaces, and interfaces
journal, March 1991


Aqueous Solutions of Calcium Ions:  Hydration Numbers and the Effect of Temperature
journal, November 2005

  • Zavitsas, Andreas A.
  • The Journal of Physical Chemistry B, Vol. 109, Issue 43
  • DOI: 10.1021/jp053909i

    Figures/Tables have been extracted from DOE-funded journal article accepted manuscripts.