Preparation and characterization of biocompatible carbon electrodes

Electron transfer in microbial fuel cell and biosensors could be facilitated through high conductive materials with enhanced active surface area and appropriate redox potential suited to microbial metabolism. In the first strategy based on bulk doping, graphite/epoxy composite electrode (GECE) bulk was modified with six types of metal ion which were prepared through a wet impregnation procedure. In the second strategy, immobilization of redox dye on carbon cloth and graphite sheet was carried out using N,N′-dicyclohexylcarbodiimide for surface modification. Crystallinity, morphology, surface chemistry and electrochemical properties of all modified electrodes were investigated. Influence of redox behavior of electrodes suited to microbial metabolism and conducive to biofilm formation have been examined. It was observed that the Fe³⁺ doped GECE surfaces exhibited significantly high biofilm formation of 1.10(±0.18) × 10⁷ CFU/cm² as compared to other dopants. The microbial growth on the carbon cloth electrode and carbon fiber reinforced plate were found to be less (2.6(±0.97) × 10⁴, 4.8(±1.8) × 10³ CFU/cm² respectively) compared to GECEs.     

碳纤维表面磁控溅射镀铜研究

以碳纤维T- 700为原料,对其进行低温等离子预处理,实验表明,尽管预处理对碳纤维拉伸强度有一定影响,但表面粗糙度增加.经预处理后的碳纤维在室温下采用磁控溅射法在其表面溅射镀铜,利用扫描电子显微镜( SEM)、原子力显微镜(AFM)分别对镀铜碳纤维的表面形态进行表征,用VC9804A+型万用电表测量了碳纤维的导电性能....     

氯化铜/活性炭复合电极的制备及性能的研究

以酚醛树脂为活性炭基体,采用化学掺杂法掺杂氯化铜,制备氯化铜／活性炭复合电极材料。通过物理吸附考察了金属氯化铜的存在下不同活化时间对金属复合活性炭孔径分布的影响,实验表明活化时间越长,比表面积越大,中孔含量越高。通过透射电镜和X射线衍射对复合电极的微观结构进行了研究,表明金属铜以纳米级均匀分散在活性炭中。通过比较活性炭电极和复合电极的电化学性能,说明掺杂金属铜可以有效提高比电容,并对充放电机理进行了探讨。     

Electroactive coating of stimulating electrodes

Electrophysiologic examinations as well as the electrotherapy of heart diseases require electrodes which distinguish themselves by outstanding sensing and pacing performance. Both, the sensing and the stimulation behaviour are determined by the interface between electrode and tissue. To avoid energy losses and distortions of heart signals having components down to 1 Hz, the interface's impedance has to be very small in the corresponding frequency range. Towards this goal a new coating has been developed: electrolytically deposited electroactive iridium oxide. On the electrode's surface iridium oxide forms a long-term stable reversible redox system which changes its oxidation state according to the applied potential. The decrease of impendance is demonstrated by impedance spectroscopy: the low-frequency limit is lowered by more than three orders of magnitude to a value of 0.4 Hz. The reason is the electroactivity of this material which is caused by reversible proton incorporation into the coating, as is proven by cyclic voltammetry. Due to the low interface impedance well below 1 Hz, the coated electrodes fulfil the requirements for medical applications. Outstanding sensing behaviour was shown by measuring the monophasic action potential in dogs, which is possible without any distortions.This paper was accepted for publication after the 1995 Conference of the European Society of Biomaterials, Oporto, Portugal, 10–13 September.     

双电层电容器用中孔活性炭电极的电化学性能

选用中孔活性炭作为双电层电容器的电极材料，实验发现，中孔活性炭电化学性能优异，比表面积利用率高达93．5％，用水蒸气活化可以增加活性炭的比表面积，随着活化时间的延长，活性炭收率降低，活化2h收率仅为26．5％,同时比表面积从原来的760m^2/g增加到1480m^2/g，且主要在2nm附近孔结构分布强度增强，比电容随活化时间的延长而增加，但增速低于比表面积的增加幅度。     

Carbon nanotube purification: preparation and characterization of carbon nanotube paste electrodes

Paste electrodes have been constructed using single-wall carbon nanotubes mixed with mineral oil. The electrochemical behavior of such electrodes prepared with different percentages of carbon nanotubes has been compared with that of graphite paste electrodes and evaluated with respect to the electrochemistry of ferricyanide with cyclic voltammetry. Carbon nanotubes were purified by a treatment with concentrated nitric acid, then oxidized in air. In addition, electrochemical pretreatments were carried out to increase the selectivity of carbon nanotube electrodes. Performances of carbon nanotube paste and carbon paste electrodes were evaluated by studying such parameters as current peak, deltaEp, anodic and cathodic current ratio, and charge density toward several different electroactive molecules. Data interpretation based on the carbon nanotubes and carbon surface area is presented. Carbon nanotube paste and carbon paste electrodes were tested as H2O2 and NADH probes, and several analytical parameters were evaluated. The oxidative behavior of dopamine was examined at these electrodes. The two-electron oxidation of dopamine to dopaminequinone showed an excellent reversibility in cyclic voltammetry that was significantly better than that observed at carbon paste electrodes.     

Mechanical characterization of copper coated carbon nanotubes reinforced aluminum matrix composites

In this investigation, carbon nanotube (CNT) reinforced aluminum composites were prepared by the molecular-level mixing process using copper coated CNTs. The mixing of CNTs was accomplished by ultrasonic mixing and ball milling. Electroless Cu-coated CNTs were used to enhance the interfacial bonding between CNTs and aluminum. Scanning electron microscope analysis revealed the homogenous dispersion of Cu-coated CNTs in the composite samples compared with the uncoated CNTs. The samples were pressureless sintered under vacuum followed by hot rolling to promote the uniform microstructure and dispersion of CNTs. In 1.0 wt.% uncoated and Cu-coated CNT/Al composites, compared to pure Al, the microhardness increased by 44% and 103%, respectively. As compared to the pure Al, for 1.0 wt.% uncoated CNT/Al composite, increase in yield strength and ultimate tensile strength was estimated about 58% and 62%, respectively. However, in case of 1.0 wt.% Cu-coated CNT/Al composite, yield strength and ultimate tensile strength were increased significantly about 121% and 107%, respectively.     

Fabrication, characterization, and potential application of carbon fiber cone nanometer-size electrodes

A novel method has been developed for the fabrication of carbon fiber cone nanometer-size ultramicroelectrodes (nanoelectrodes) with overall tip dimensions as small as 50 nm in diameter. In this method, carbon fibers were initially etched by an argon ion beam thinner. Afterward, a single etched carbon fiber was inserted into a glass capillary, which was then sealed by heating the glass/fiber interface in a vacuum; thus, no epoxy resin is involved. The success rate of our fabrication route for the electrodes with overall tip diameters of up to 500 nm was about 80%; for those with tip diameters of up to 100 nm, it was about 50%. The fabricated carbon fiber cone nanoelectrodes (CFCNEs) were inspected by optical and scanning electron microscopy. Their electrochemical behavior was examined by cyclic and linear sweep voltammetric measurements of ferricyanide and ferrocene ions in aqueous and nonaqueous media. The potential analytical applicability of the CFCNEs was tested by differential pulse voltammetric measurements of two well-known neurotransmitters, dopamine (DA) and 5-hydroxytryptamine (5-HT), and the results achieved were highly satisfactory. The calibration plots obtained were linear over the ranges from 5.0 × 10(-7) to 1.0 × 10(-4) and from 2.0 × 10(-6) to 1.0 × 10(-4) mol/L, with limits of detection of 1.0 × 10(-7) and 5.0 × 10(-7) mol/L for DA and 5-HT, respectively. Some advantages and improvements of the proposed CFCNE fabrication method, especially with respect to smoothness of the fiber (electrode) surface, strength, and control over the fiber tip dimensions, are also discussed.     

Electrochemical characterization of carbon nanotube forests grown on copper foil using transition metal catalysts

Growth of vertical, multiwalled carbon nanotubes (CNTs) on bulk copper foil substrates can be achieved by sputtering either Ni or Inconel thin films on Cu substrates followed by thermal chemical vapor deposition using a xylene and ferrocene mixture. During CVD growth, Fe nanoparticles from the ferrocene act as a vapor phase delivered catalyst in addition to the transition metal thin film, which breaks up into islands. Both the thin film and iron are needed for dense and uniform growth of CNTs on the copper substrates. The benefits of this relatively simple and cost effective method of directly integrating CNTs with highly conductive copper substrates are the resulting high density of nanotubes that do not require the use of additional binders and the potential for low contact resistance between the nanotubes and the substrate. This method is therefore of interest for charge storage applications such as double layer capacitors. Inconel thin films in conjunction with Fe from ferrocene appear to work better in comparison to Ni thin films in terms of CNT density and charge storage capability. We report here the power density and specific capacitance values of the double layer capacitors developed from the CNTs grown directly on copper substrates.     

Structural characteristics of titanium coating on copper substrates

The growth characteristics of titanium films deposited on glass, silicon (100) and oxygen free high purity copper substrate using magnetron sputtering have been investigated using X-ray diffraction, electron microscopy and scratch indentation techniques. The study of interface between the titanium film and the substrate was carried out to determine coating thickness, as well as intermixing of the elements at the interface. Studies revealed that the interface is free from voids and intermixing of the film and the substrate. Microstructural and diffraction analysis showed that the Ti coating was polycrystalline and exhibited columnar growth. The Ti crystallite size varied between 24 and 58 nm depending on the substrate. The thickness of the films were typically about 4 μm. Scratch test indicated that the films are adherent and the first critical load to failure was observed to be 4·5 N ± 2 N.     

Cell attachment on diamond-like carbon coating

Preliminary results of diamond-like carbon (DLC) coating with its novel properties with no toxicity have caused a strong interest of commercial manufacturers of surgical implants. DLC coatings were prepared on polymethylmethacrylate (PMMA) at room temperature using ion beam assisted deposition (IBAD). It could be shown by X-ray photoelectron spectroscopy, Auger electron spectroscopy, and Raman spectroscopy that DLC coating prepared by 800 eV CHⁿ⁺ beam bombardment possessed a higher fraction ofsp ³ bonds in the structure of mixedsp ⁿ³ +sp ⁿ² bonding, resulting in a higher hydrophobicity. The results of the cell attachment tests indicated that DLC coatings exhibited low macrophage attachment and provided desirable surface for the normal cellular growth and morphology of the fibroblasts. At the same time, the number of both neutral granulocytes and platelets adhering to DLC coatings decreased significantly. These findings showed that DLC was a better coating with desirable tissue and blood compatibility.     

Preliminary study of iridium coating on carbon/carbon composites

Iridium coating was deposited on as-received, polished and chemical vapour deposited (CVD) pyro carbon-coated carbon/carbon composite by d.c. sputtering. The as-received surface of the carbon/carbon composite was not fully covered by an iridium coating up to 12 m thick, whereas better deposition and surface coverage with the iridium coating were obtained on the polished surface and CVD pyro carbon-coated carbon/carbon composite surface. After heat treatment at 2000 K for 1.2 ks, interconnected islands of iridium were formed on three surfaces of the carbon/carbon composite. Iridium neither reacted with nor dissolved the carbon/carbon composite, it had some penetration but did not react to form an interfacial compound, and the boundary between the iridium and carbon/carbon composite was distinct.     

炭气凝胶为电极的超级电容器的研究

采用低分子线性酚醛树脂-糠醛为原料通过溶液．溶胶-凝胶途径成功合成了炭气凝胶．探讨了结构对电化学性能的影响。采用直流循环法测定炭气凝胶为电极的超级电容器的电化学性能,结果表明,炭气凝胶电极在0．5mA充放电时电极的比电容为121F／g．充放电效率为95％．具有性能稳定、充放电效率高等优良性能。     

Enzymatic genosensor on streptavidin-modified screen-printed carbon electrodes

Voltammetric enzyme genosensors on streptavidin-modified screen-printed carbon electrodes (SPCEs) for the detection of virulence nucleic acid determinants of pneumolysin and autolysin genes, exclusively present on the genome of the human pathogen Streptococcus pneumoniae, were described. Alkaline phosphatase (AP) and 3-indoxyl phosphate were used as the enzymatic label and substrate, respectively. The oligonucleotide probes were immobilized on electrochemically pretreated SPCEs through the streptavidin/biotin reaction. The adsorption of streptavidin was performed by deposition of a drop of a streptavidin solution overnight at 4 degrees C on the surface of the SPCEs. After the hybridization reaction with FITC-labeled complementary targets, the enzyme is captured using an anti-FITC antibody conjugated to AP. In nonstringent experimental conditions, these genosensors can detect 0.49 fmol of 20-mer oligonucleotide target and discriminate between a complementary oligo and an oligo with a three-base mismatch. In the presence of 25% formamide in the hybridization buffer, a single-base mismatch on the oligonucleotide target can be detected.     

Fabrication and textural characterization of nanoporous carbon electrodes embedded with CuO nanoparticles for supercapacitors

Abstract

We introduce a novel strategy of fabricating nanoporous carbons loaded with different amounts of CuO nanoparticles via a hard templating approach, using copper-containing mesoporous silica as the template and sucrose as the carbon source. The nature and dispersion of the CuO nanoparticles on the surface of the nanoporous carbons were investigated by x-ray diffraction (XRD), high-resolution scanning electron microscopy (HRSEM) and high-resolution transmission electron microscopy (HRTEM). XRD results reveal that nanoporous carbons with embedded CuO nanoparticles exhibit a well-ordered mesoporous structure, whereas the nitrogen adsorption measurements indicate the presence of excellent textural characteristics such as high surface area, large pore volume and uniform pore size distribution. The amount of CuO nanoparticles in the nanochannels of the nanoporous carbon could be controlled by simply varying the Si/Cu molar ratio of the mesoporous silica template. Morphological characterization by SEM and TEM reveals that high-quality CuO nanoparticles are distributed homogeneously within the nanoporous carbon framework. The supercapacitance behavior of the CuO-loaded nanoporous carbons was investigated. The material with a small amount of CuO in the mesochannels and high surface area affords a maximum specific capacitance of 300 F g^-1 at a 20 mV s^-1 scan rate in an aqueous electrolyte solution. A supercapacitor containing the CuO-loaded nanoporous carbon is highly stable and exhibits a long cycle life with 91% specific capacitance retained after 1000 cycles.     

Adherent diamond coating on copper using an interlayer

With a titanium interlayer, adherent diamond coating on copper is obtained. The diamond nucleation density is enhanced significantly by scratching the substrate with diamond powder and is influenced by the deposition conditions. It is found that the diamond growth rate increases with microwave power, gas pressure and methane concentration. However, a higher methane concentration results in increased growth defects and non-diamond phases. Under typical deposition conditions, the diamond crystals exhibit a (111) face dominating. The coating adhesion is accessed by pull-off tests and scratch tests. The former indicates that the coating adhesion is better than the strength of the adhesive, at ca 13 MPa. The latter shows a critical load about 8 N.