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Title: Soft x-ray spectroscopy of high pressure liquid

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:
Grant/Contract Number:
AC02-05CH11231; U1432249
Type:
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)
Research Org:
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Advanced Light Source (ALS)
Sponsoring Org:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22); National Natural Science Foundation of China (NNSFC)
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
OSTI Identifier:
1436167
Alternate Identifier(s):
OSTI ID: 1418709

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., 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. 2018. "Soft x-ray spectroscopy of high pressure liquid". United States. doi:10.1063/1.5008444.
@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},
number = 1,
volume = 89,
place = {United States},
year = {2018},
month = {1}
}

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Polymers with Tailored Electronic Structure for High Capacity Lithium Battery Electrodes
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  • Liu, Gao; Xun, Shidi; Vukmirovic, Nenad
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