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

This content will become publicly available on February 20, 2020

Title: Hybrid X-ray Spectroscopy-Based Approach To Acquire Chemical and Structural Information of Single-Walled Carbon Nanotubes with Superior Sensitivity

Abstract

High-resolution nondestructive chemical analysis of both bulk and surface of application-ready carbon nanomaterials is needed to connect the material properties to the observed performance. This is needed to enable application-specific tailoring of carbon nanomaterials. However, detailed studies of effects of oxidizing treatments on the chemical composition and structural integrity of carbon and on the metal seed materials are rare. Here we show a hybrid X-ray-based study retrieving this hard-to-access chemical and structural information of application-ready ferrocene-grown single-walled carbon nanotubes and their nitric acid- and oxygen plasma-treated versions. We have executed photoelectron, absorption, and X-ray emission spectroscopy (XES) measurements in the soft X-ray regime providing chemical and structural information with high energy resolution and throughput. We observed that the nitric acid treatment did not significantly alter the chemical state of the carbon matrix, whereas the oxygen plasma treatment was associated with strong effects and chemical conversions toward oxygen-functionalized groups such as carboxyl. Additionally, an Fe catalyst was present before and after the oxidizing treatments at considerable concentrations as detected by both X-ray absorption spectroscopy and XES, with a near complete conversion of Fe 2+ to Fe 3+. Additional minor elements (metals <0.1 at. %) were detected only with XES. With thismore » combined approach, we can study the effect of different treatments on application-ready carbon nanomaterials’ physicochemical and structural properties with unmatched precision, which helps understand the nature of these materials.« less

Authors:
ORCiD logo [1];  [2]; ORCiD logo [3]; ORCiD logo [2];  [2];  [4];  [4];  [4];  [3];  [5]; ORCiD logo [5];  [5];  [6];  [2]; ORCiD logo [2];  [2]
  1. Aalto Univ., Aalto (Finland); SLAC National Accelerator Lab., Menlo Park, CA (United States)
  2. Aalto Univ., Aalto (Finland)
  3. Stanford Univ., Stanford, CA (United States)
  4. SLAC National Accelerator Lab., Menlo Park, CA (United States)
  5. National Institute of Standards and Technology, Boulder, CO (United States)
  6. National Institute of Standards and Technology, Boulder, CO (United States); Univ. of Colorado, Boulder, CO (United States)
Publication Date:
Research Org.:
SLAC National Accelerator Lab., Menlo Park, CA (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1529087
Grant/Contract Number:  
AC02-76SF00515; 211637
Resource Type:
Accepted Manuscript
Journal Name:
Journal of Physical Chemistry. C
Additional Journal Information:
Journal Volume: 123; Journal Issue: 10; Journal ID: ISSN 1932-7447
Publisher:
American Chemical Society
Country of Publication:
United States
Language:
English

Citation Formats

Sainio, Sami, Wester, Niklas, Titus, Charles J., Liao, Yongping, Zhang, Qiang, Nordlund, Dennis, Sokaras, Dimosthenis, Lee, Sang-jun, Irwin, Kent D., Doriese, William B., O’Neil, Galen C., Swetz, Daniel S., Ullom, Joel N., Kauppinen, Esko I., Laurila, Tomi, and Koskinen, Jari. Hybrid X-ray Spectroscopy-Based Approach To Acquire Chemical and Structural Information of Single-Walled Carbon Nanotubes with Superior Sensitivity. United States: N. p., 2019. Web. doi:10.1021/acs.jpcc.9b00714.
Sainio, Sami, Wester, Niklas, Titus, Charles J., Liao, Yongping, Zhang, Qiang, Nordlund, Dennis, Sokaras, Dimosthenis, Lee, Sang-jun, Irwin, Kent D., Doriese, William B., O’Neil, Galen C., Swetz, Daniel S., Ullom, Joel N., Kauppinen, Esko I., Laurila, Tomi, & Koskinen, Jari. Hybrid X-ray Spectroscopy-Based Approach To Acquire Chemical and Structural Information of Single-Walled Carbon Nanotubes with Superior Sensitivity. United States. doi:10.1021/acs.jpcc.9b00714.
Sainio, Sami, Wester, Niklas, Titus, Charles J., Liao, Yongping, Zhang, Qiang, Nordlund, Dennis, Sokaras, Dimosthenis, Lee, Sang-jun, Irwin, Kent D., Doriese, William B., O’Neil, Galen C., Swetz, Daniel S., Ullom, Joel N., Kauppinen, Esko I., Laurila, Tomi, and Koskinen, Jari. Wed . "Hybrid X-ray Spectroscopy-Based Approach To Acquire Chemical and Structural Information of Single-Walled Carbon Nanotubes with Superior Sensitivity". United States. doi:10.1021/acs.jpcc.9b00714.
@article{osti_1529087,
title = {Hybrid X-ray Spectroscopy-Based Approach To Acquire Chemical and Structural Information of Single-Walled Carbon Nanotubes with Superior Sensitivity},
author = {Sainio, Sami and Wester, Niklas and Titus, Charles J. and Liao, Yongping and Zhang, Qiang and Nordlund, Dennis and Sokaras, Dimosthenis and Lee, Sang-jun and Irwin, Kent D. and Doriese, William B. and O’Neil, Galen C. and Swetz, Daniel S. and Ullom, Joel N. and Kauppinen, Esko I. and Laurila, Tomi and Koskinen, Jari},
abstractNote = {High-resolution nondestructive chemical analysis of both bulk and surface of application-ready carbon nanomaterials is needed to connect the material properties to the observed performance. This is needed to enable application-specific tailoring of carbon nanomaterials. However, detailed studies of effects of oxidizing treatments on the chemical composition and structural integrity of carbon and on the metal seed materials are rare. Here we show a hybrid X-ray-based study retrieving this hard-to-access chemical and structural information of application-ready ferrocene-grown single-walled carbon nanotubes and their nitric acid- and oxygen plasma-treated versions. We have executed photoelectron, absorption, and X-ray emission spectroscopy (XES) measurements in the soft X-ray regime providing chemical and structural information with high energy resolution and throughput. We observed that the nitric acid treatment did not significantly alter the chemical state of the carbon matrix, whereas the oxygen plasma treatment was associated with strong effects and chemical conversions toward oxygen-functionalized groups such as carboxyl. Additionally, an Fe catalyst was present before and after the oxidizing treatments at considerable concentrations as detected by both X-ray absorption spectroscopy and XES, with a near complete conversion of Fe2+ to Fe3+. Additional minor elements (metals <0.1 at. %) were detected only with XES. With this combined approach, we can study the effect of different treatments on application-ready carbon nanomaterials’ physicochemical and structural properties with unmatched precision, which helps understand the nature of these materials.},
doi = {10.1021/acs.jpcc.9b00714},
journal = {Journal of Physical Chemistry. C},
number = 10,
volume = 123,
place = {United States},
year = {2019},
month = {2}
}

Journal Article:
Free Publicly Available Full Text
This content will become publicly available on February 20, 2020
Publisher's Version of Record

Save / Share: