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

Journal Article · · Review of Scientific Instruments
DOI:https://doi.org/10.1063/1.5008444· OSTI ID:1436167
 [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

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.

Research Organization:
Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES); National Natural Science Foundation of China (NSFC)
Grant/Contract Number:
AC02-05CH11231; U1432249
OSTI ID:
1436167
Alternate ID(s):
OSTI ID: 1418709
Journal Information:
Review of Scientific Instruments, Vol. 89, Issue 1; ISSN 0034-6748
Publisher:
American Institute of Physics (AIP)Copyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 7 works
Citation information provided by
Web of Science

References (35)

A liquid flow cell to study the electronic structure of liquids with soft X-rays
  • 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 https://doi.org/10.1016/j.nima.2007.10.029
journal February 2008
Setup for in situ investigation of gases and gas/solid interfaces by soft x-ray emission and absorption spectroscopy journal January 2014
Development of a liquid flow cell to measure soft X-ray absorption in transmission mode: A test for liquid water journal March 2010
Novel spectro-electrochemical cell for in situ / operando observation of common composite electrode with liquid electrolyte by X-ray absorption spectroscopy in the tender X-ray region journal August 2014
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
Polymers with Tailored Electronic Structure for High Capacity Lithium Battery Electrodes journal September 2011
Development and application of in situ/operando soft X-ray transmission cells to aqueous solutions and catalytic and electrochemical reactions journal April 2015
The Nanoscale Basis of CO 2 Trapping for Geologic Storage journal August 2015
In operando observation system for electrochemical reaction by soft X-ray absorption spectroscopy with potential modulation method journal October 2014
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
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
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
A sample holder for soft x-ray absorption spectroscopy of liquids in transmission mode journal October 2011
Characterization of the Acetonitrile Aqueous Solution/Vapor Interface by Liquid-Jet X-ray Photoelectron Spectroscopy journal September 2014
First experimental results from IBM/TENN/TULANE/LLNL/LBL undulator beamline at the advanced light source journal February 1995
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
Core Level Spectroscopy of Solids book January 2008
Liquid microjet for photoelectron spectroscopy journal March 2009
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
Bivalence Mn5O8 with hydroxylated interphase for high-voltage aqueous sodium-ion storage journal November 2016
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
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
A soft XAS transmission cell for operando studies journal October 2016
Phase transitions in biogenic amorphous calcium carbonate journal April 2012
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

Cited By (4)


Figures / Tables (6)