Coupled thermogravimetry, mass spectrometry, and infrared spectroscopy for quantification of surface functionality on single-walled carbon nanotubes

Kingston, Christopher T.; Martinez‐Rubi, Yadienka; Guan, Jingwen; Barnes, Michael; Scriver, Christine; Sturgeon, Ralph E.; Simard, Benoît

doi:10.1007/s00216-009-3205-y

Cited by 15 publications

(13 citation statements)

References 27 publications

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“…TGA in desorption mode can be used to estimate degree of functionalization. 48,49 A larger mass loss in desorption was seen for the SWCNT-OH paper, which again is consistent with the functionalization chemistry employed. Quantitative analysis of functionalization from TGA has a high uncertainty for small functional groups (in this case CH 2 OH) at typical degrees of functionalization of a few percent.…”

Section: Modified Buckypaperssupporting

confidence: 83%

3D chemically cross-linked single-walled carbon nanotube buckypapers

et al. 2014

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Single-walled carbon nanotubes (SWCNTs) covalently modified with OH functional groups were assembled into buckypapers through solvent dispersion and vacuum filtration. These SWCNT-OH buckypaper sheets were subsequently crosslinked by wetting with bifunctional linkers followed by hot compression causing reaction between the functional groups of the reagent and OH functional groups on the side-walls of SWCNTs to create three-dimensional (3D) covalently cross-linked buckypapers. Cross-linking also was performed using SWCNTs encapsulated with a functionalized polymer wrapping in a core-shell structure, where OH or/and NH 2 groups are available on the surface of the polymeric shell for reaction. The 3D cross-linked SWCNT buckypapers retain the porous character typical of buckypaper, and were characterized for their tensile properties and thermal and electrical conductivities. Several cross-linking approaches dramatically improved the mechanical properties. The strongest and stiffest papers (32 MPa, E = 3.1 GPa), which approach 10× stronger and stiffer than the pristine non-crosslinked buckypaper, were obtained at the expense of a loss of electrical conductivity. In other cases, such as cross-linking using a high-performance epoxy resin monomer, improvements in strength and stiffness of ~5× were obtained while retaining electrical and thermal conductivity. Therefore, the optimal crosslinking approach would be determined by the desired, multifunctional properties. Additionally, the approach can be used in the preparation buckypaper composites and it is demonstrated that cross-linking using a multifunctional epoxy resin prior to impregnation with the same epoxy resin results in substantially better mechanical properties than comparison to just epoxy-impregnation of pristine buckypaper.

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Section: Modified Buckypaperssupporting

confidence: 83%

3D chemically cross-linked single-walled carbon nanotube buckypapers

et al. 2014

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“…While negative ion SIMS of CNTs has been reported, there does not appear to have been any recognition or discussion of this effect, although odd–even effects of secondary ions from other carbon‐containing materials are known The valence band spectrum of CNTs taken with X‐radiation (Al Kα) does not appear to have been reported.As has previously been reported for highly ordered pyrolytic graphite and CNTs, the C 1 s peak is asymmetric . We similarly observe this asymmetry, which can be confused with oxidized carbon moieties.…”

Section: Discussionsupporting

confidence: 47%

“…291 eV is the π → π * transition or shake‐up peak. Both of these features are common in graphitic carbon and CNTs . The valence band (VB) region consists of a signal that increases steadily with increasing binding energy to ca.…”

Section: Resultsmentioning

confidence: 99%

Multi‐instrument characterization of the surfaces and materials in microfabricated, carbon nanotube‐templated thin layer chromatography plates. An analogy to ‘The Blind Men and the Elephant’

Jensen

Kanyal

Madaan

et al. 2013

Surface & Interface Analysis

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We apply a suite of analytical tools to characterize materials created in the production of microfabricated thin layer chromatography plates. Techniques used include X-ray photoelectron spectroscopy (XPS), valence band spectroscopy, time-of-flight secondary ion mass spectrometry (ToF-SIMS) in both positive and negative ion modes, Rutherford backscattering spectroscopy (RBS), and helium ion microscopy. Materials characterized include: the Si(100) substrate with native oxide: Si/SiO 2 , alumina (35 nm) deposited as a diffusion barrier on the Si/SiO 2 : Si/SiO 2 /Al 2 O 3 , iron (6 nm) thermally evaporated on the Al 2 O 3 : Si/SiO 2 /Al 2 O 3 /Fe, the iron film annealed in H 2 to make Fe catalyst nanoparticles: Si/SiO 2 /Al 2 O 3 /Fe(NP), and carbon nanotubes (CNTs) grown from the Fe nanoparticles: Si/SiO 2 /Al 2 O 3 /Fe(NP)/CNT. The Fe films and nanoparticles appear in an oxidized state. Some of the analyses of the CNTs/CNT forests appear to be unique: (i) the CNT forest appears to exhibit an interesting 'channeling' phenomenon by RBS, (ii) we observe an odd-even effect in the SIMS spectra of C n -species for n = 1 -6, with the n ≥ 6 ions showing a steady decrease in intensity, and (iii) valence band characterization of CNTs using X-radiation is reported. Initial analysis of the CNT forest by XPS shows that it is 100 at.% carbon. After one year, only ca. 0.25 at.% oxygen is observed. The information obtained from the combination of the different analytical tools provides a more complete understanding of our materials than a single technique, which is analogous to the story of 'The Blind Men and the Elephant'. The raw XPS and ToF-SIMS spectra from this study will be submitted to Surface Science Spectra for archiving.

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“…Transfer lines between the TG instrument and FTIR spectrometer were heated to a temperature of 200 °C. The detailed experimental conditions of the measurement have been reported previously [29].…”

Section: Characterizationmentioning

confidence: 99%

Tailored SWCNT functionalization optimized for compatibility with epoxy matrices

et al. 2012

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We have modified single walled carbon nanotubes (SWCNTs) with well defined matrix-based architectures to improve interface interaction in SWCNT/epoxy composites. The hardener and two pre-synthesized oligomers containing epoxy and hardener moieties were covalently attached to the SWCNT walls by in situ diazonium or carboxylic coupling reactions. In this way, SWCNTs bearing amine or epoxide-terminated fragments of different molecular weights, which resemble the chemical structure of the cured resin, were synthesized. A combination of characterization techniques such as Raman and infrared absorption (FTIR) spectroscopy, elemental analysis and coupled thermogravimetry-FTIR spectroscopy were used to identify both the functional groups and degree of functionalization of SWCNTs synthesized by the laser ablation and arc-discharge methods. Depending on the type of reaction employed for the chemical functionalization and the molecular weight of the attached fragment, it was possible to control the degree of functionalization and the electronic properties of the functionalized SWCNTs. Improved dispersion of SWCNTs in the epoxy matrix was achieved by direct integration without using solvents, as observed from optical microscopy and rheology measurements of the SWCNT/epoxy mixtures. Composite materials using these fillers are expected to exhibit improved properties while preserving the thermosetting architecture.

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Coupled thermogravimetry, mass spectrometry, and infrared spectroscopy for quantification of surface functionality on single-walled carbon nanotubes

Cited by 15 publications

References 27 publications

3D chemically cross-linked single-walled carbon nanotube buckypapers

3D chemically cross-linked single-walled carbon nanotube buckypapers

Multi‐instrument characterization of the surfaces and materials in microfabricated, carbon nanotube‐templated thin layer chromatography plates. An analogy to ‘The Blind Men and the Elephant’

Tailored SWCNT functionalization optimized for compatibility with epoxy matrices

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