Synthesis of graphite films by electrochemical reduction of hexachlorobuta-1,3-diene

Nishihara, Hiroshi; Harada, Hiroshi; Kaneko, Shu; Teteishi, Masahiro; Aramaki, Kunitsugu

doi:10.1039/c39900000026

Cited by 9 publications

(8 citation statements)

References 3 publications

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“…The n-doping rate of electrochemical carbon from hexachlorobuta-1,3-diene 38,39,41,128 increases, as expected, with decreasing size of M + (NBu 4 + , NEt 4 + , NMe 4 + ). 40 n-Doping was also observed during electrochemical carbonization of PCTFE (δ ) 0.32), 53 Nafion 117 (δ ) 0.20), 46 PTFE-PPVE (δ ) 0.21), 53 FEP (δ ) 0.2), 66 C 6 F 6 and C 6 F 14 (δ ≈ 0.07-0.25), 47 diiodoacetylene, 34,35 and PVDF (δ ≈ 0.15).…”

Section: A Doping By Reductionsupporting

confidence: 75%

“…Hexachlorobuta-1,3-diene. Nishihara et al [38][39][40][41]127,128 reduced hexachlorobuta-1,3-diene at a carbon electrode in NBu 4 BF 4 /CH 3 CN. The product was electroactive carbon (graphite) film, and it was reversibly dopable under insertion of both cations and anions.…”

Section: B Low Molecular Weight Carbon Halidesmentioning

confidence: 99%

“…Reductive carbonization of perhalogenated hydrocarbons (eq 37) is generally accompanied by a small superstoichiometric consumption of electrons (eq 38), which is considered as n-doping of electrochemical carbon: 268 Both reactions proceed simultaneously, since the overpotential for carbonization (37) is higher (by ∼1 V) 22,40 than the overpotential for n-doping (38). Cyclic voltammetry confirms reversibility of the reaction (38), although the charge recovery upon anodic oxidation is not perfect (40-94%). 25,40 The n-doping of electrochemical carbon can also be compensated by mild reductants, e.g., I 2 .…”

Section: A Doping By Reductionmentioning

confidence: 99%

“…33 Some authors 22,25,28,40 have regarded the interaction between the inserted cations M + and C δas an intercalation into the graphite lattice. However, the potential at which the electrocarbonization 37,38 takes place (∼-2 V vs SHE) is too high to promote…”

Section: A Doping By Reductionmentioning

confidence: 99%

“…section VI). Infrared spectra of various carbons derived from PTFE, 29,64,65,191,205,225,234,272 PCTFE, 207,281 FEP, 65 hexachlorobuta-1,3-diene, 38,39 CCl 4 , 42 diiodoacetylene, 34,35 C 6 F 6 , and C 6 F 14 47 usually indicate a complicated mixture of surface oxides (sOH, dO, sCOOH, and combinations), created by air exposure during the sample preparation and/or measurement. Incomplete carbonization, impurities (adsorbed solvents), and n-doping (NR 4 + insertion) are also detectable.…”

Section: Optical Properties Spectroscopymentioning

confidence: 99%

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Electrochemical Carbon

Kavan

1997

Chem. Rev.

159

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Section: A Doping By Reductionsupporting

confidence: 75%

Section: B Low Molecular Weight Carbon Halidesmentioning

confidence: 99%

Section: A Doping By Reductionmentioning

confidence: 99%

Section: A Doping By Reductionmentioning

confidence: 99%

Section: Optical Properties Spectroscopymentioning

confidence: 99%

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Electrochemical Carbon

Kavan

1997

Chem. Rev.

159

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Room‐temperature electrosynthesis of carbonaceous fibers

et al. 1995

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Communications self-assembled thin films were fabricated by an electrostatic deposition technique similar to that described by Decher[2]; Rubner [3], and others [9]. The polymer films consist of alternating layers of a cationic poly(p-pyridiniuin vinylene) (PHPyV or Bu-PHPyV) and anionic sulfonated polyaniline (SPANI) or poly(4-styrene sulfonate) (PSS). Films are grown by first initiating ITO-coated glass substrates with positive charges. This initiation is carried out by treating the ITO-coated glass with (3-aminopropyl)triethoxysilane[7] or by depositing a thin film of polypyrrole or polyaniline directly on the substrate[3b]. In the latter case, the thickiicss of the conducting polymer film was limited to keep the total optical density of the resulting substrate below 0.1 in the visible part of the spectrum. The assembly ofthe multilayer polymer film on the cationicsubstrate was carried out by sequentially dipping the substrate into each polymer solution (alternating between anionic and cationic). Dipping time in each solution was 30 minutes. After each dip, the film was rinsed with water (for PSS or SPANI) or THF-acetone (for Bu-PHPyV) or m-cresol-acetonitrile (for PHPyV) and dried under nitrogen flow before the next deposition.The LEDs were fiiiishcd by vacuum depositing an aluminum electrode on top of the organic film. The base pressure of the chamber was mbar and the evaporating pressure was 10-' mbar The thickness of the electrode was ca.1000 a and the area of the electrode was 1 mm2. The I-Vcharacteristics of the devices were measured on an H P 414BB analyzer and the electroluminescent spectra were collected using ail EG & G nionochromator and Electriin 1000 TE CCD camera. The light intensity was detected by a calibrated broad-area silicon photodiode. ahose photocurrent was measured by H P picoampere meters.The electronic absorption spectra weremeasured on an AVIV Spectrophotometer model 14DS (modified Cary-14) and the photoluminescence spectra were taken with a Perkin-Elmer LS-50 Luminescence Spectrometer. The excitation wavelengths used were thc maximum absorption wavelengths in the electronic absorption spectra. PSS is tiansparent at both the excitation and emission wavelengths, while polypyrrole, polyaniline and SPANI have very low optical densities at these wavelengths in the samples prepared here. Photoluminescence quantum yields of Bu-PPyV and Bu-PHPyV were measured in degassed T H F solutions. typically M (based on the monomer repeat unit). The Bu-PH-PyV was made by adding stoichiometric amount methane sulfonic acid to the Bu-PPyV solution. Rhodamine B in ethanol was used as a reference (u, = 1) [11].The excitation wavelengths for the polymer solutions and Rhodamine B were 420 nm and 530 nm. respectively. The photoluminescent quantum yield of Bu-PPyV is greater than 0.9, and the quantum yield of Bu-PHPyV is ca. 0.8. M R 9357415. The authors wish to thank Victor Gruol for assistmce with the XPS measurements, and Andrew Gewirth (University of Illinois) for generous donation of the HOPG substrate. ...

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Electrochemical Methods

Kavan¹

1999

Physics and Chemistry of Materials With Low-Dimensional Structures

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Synthesis of graphite films by electrochemical reduction of hexachlorobuta-1,3-diene

Abstract: Electrochemical reduction of hexachlorobuta-l,3-diene in aprotic solvents affords mostly graphitized films which can be easily d.oped with anions and also with cations.

Cited by 9 publications

References 3 publications

Electrochemical Carbon

Electrochemical Carbon

Room‐temperature electrosynthesis of carbonaceous fibers

Electrochemical Methods

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