Advertisement

Evaluation of edges for carbon materials via temperature-programmed desorption and temperature-programmed oxidation

  • Kazuki Matsumura
  • Taro Kinumoto
  • Tomoki Tsumura
  • Masahiro ToyodaEmail author
Note

Abstract

Herein, the edges in carbon materials were quantitatively evaluated by summing the amount of hydrogen and the amount of functional groups without hydrogen in the material. The amount of hydrogen in the carbon material was quantitated via temperature-programmed oxidation (TPO) under an oxygen atmosphere, whereas the amount of functional groups was determined via temperature-programmed desorption (TPD) of the sample under an inert atmosphere. Consequently, the amount of edges in exfoliated carbon fibers prepared from polyacrylonitrile (PAN) (referred to as PAN-1000) was 9.4 mmol g−1. In addition, Ketjen Black (KB) and activated carbon (AC) had edge content of 1.3 and 3.6 mmol g−1, respectively. Because the total amount of functional groups of PAN-1000, KB and AC were estimated to be 8.18, 0.082 and 1.02 mmol g−1 via TPD, the total amount of edges and oxygen-containing functional groups of each sample could be quantified. The difference between amount of edges and the amount of functional groups is speculated to correspond to the amount of edges terminated with hydrogen. This study revealed that detailed information about the edges such as their proportion terminated with oxygen-containing functional groups, the species and amount of oxygen-containing functional groups via a combination of TPO and TPD.

Keywords

Edge site Oxygen-containing functional groups Temperature-programmed oxidation Temperature-programmed desorption 

Supplementary material

42823_2019_6_MOESM1_ESM.docx (67 kb)
Supplementary material 1 (DOCX 66 kb)

References

  1. 1.
    Horita K, Fujita T (1989) Wettability of activated carbon for using as an oxygen electrode. TANSO 140:228 (in Japanese) CrossRefGoogle Scholar
  2. 2.
    Tamai H, Sasaki M, Yasuda H (1998) Surface charge of activated carbon and its characteristics for adsorption. TANSO 184:219 (in Japanese) CrossRefGoogle Scholar
  3. 3.
    Boehm HP (1994) Some aspects of the surface chemistry of carbon blacks and other carbons. Carbon 32:759CrossRefGoogle Scholar
  4. 4.
    Figueiredo JL, Pereira MFR, Freitas MMA, Orfao JJM (1999) Modification of the surface chemistry of activated carbons. Carbon 37:1379CrossRefGoogle Scholar
  5. 5.
    Yamabe K, Takahashi H (1980) The surface oxygen on activated carbons. TANSO 102:106 (in Japanese) CrossRefGoogle Scholar
  6. 6.
    Takagi H (2009) Analysis of surface structure of carbon materials by using temperature-programmed desorption method. TANSO 237:67 (in Japanese) CrossRefGoogle Scholar
  7. 7.
    Ishii T, Kashihara S, Hoshikawa Y, Ozaki J, Kannari N, Takai K, Enoki T, Kyotani T (2014) A quantitative analysis of carbon edge sites and an estimation of graphene sheet size in high-temperature treated, non-porous carbons. Carbon 80:135CrossRefGoogle Scholar
  8. 8.
    Aso H, Matsuoka K, Sharma A, Tomita A (2004) Structural analysis of PVC and PFA carbons prepared at 500–1000°C based on elemental composition, XRD, and HRTEM. Carbon 42:2963CrossRefGoogle Scholar
  9. 9.
    Matsuoka K, Akahane T, Aso H, Sharma A, Tomita A (2008) The size of polyaromatic layer of coal char estimated from elemental analysis data. Fuel 87:539CrossRefGoogle Scholar
  10. 10.
    Kashihara S, Otani S, Orikasa H, Hoshikawa Y, Ozaki J, Kyotani T (2012) A quantitative analysis of a trace amount of hydrogen in high temperature heat-treated carbons. Carbon 50:3310CrossRefGoogle Scholar
  11. 11.
    Toyoda M, Shimizu A, Iwata H, Inagaki M (2001) Exfoliation of carbon fibers through intercalation compounds synthesized electrochemically. Carbon 39:1697CrossRefGoogle Scholar
  12. 12.
    Toyoda M, Katoh H, Shimizu A, Inagaki M (2003) Exfoliation of nitric acid intercalated carbon fibers: effects of heat-treatment temperature of pristine carbon fibers and electrolyte concentration on the exfoliation behavior. Carbon 41:731CrossRefGoogle Scholar
  13. 13.
    Toyoda M, Katoh M, Tanigawa H, Inagaki M (2004) Intercalation and exfoliation behavior of carbon fibers during electrolysis in H2SO4. J Phys Chem Solids 65:257CrossRefGoogle Scholar
  14. 14.
    Hara H, Kinumoto T, Tsumura T, Toyoda M (2012) Appearance of edges of miniaturized carbon fibers prepared by electrochemical processing and their evaluation. TANSO 255:245 (in Japanese) CrossRefGoogle Scholar
  15. 15.
    Matsumura K, Hara H, Kinumoto T, Tsumura T, Toyoda M (2016) Analysis of structural changes in and gas evolution from carbon materials during TPD, TPR and TPO. TANSO 274:125 (in Japanese) CrossRefGoogle Scholar
  16. 16.
    Calo JM, Cazorla-Amoros D, Linares-Solano A, Roman-Martinez MC, Salinas-Martinez C (1997) The effects of hydrogen on thermal desorption of oxygen surface complexes. Carbon 35:543CrossRefGoogle Scholar

Copyright information

© Korean Carbon Society 2019

Authors and Affiliations

  • Kazuki Matsumura
    • 1
  • Taro Kinumoto
    • 1
  • Tomoki Tsumura
    • 1
  • Masahiro Toyoda
    • 1
    Email author
  1. 1.Graduate School of EngineeringOita UniversityOita-shiJapan

Personalised recommendations