The exceptional physical properties of carbon nanotubes (CNTs) have the potential to transform materials science and various industrial applications. However, to exploit their unique properties in carbon-based electronics, CNTs regularly need to be chemically interfaced with metals. Although CNTs can be directly synthesized on metal substrates, this process typically requires temperatures above 350 °C, which is not compatible for many applications. Additionally, the CNTs employed here were highly densified, making them suitable as interconnecting materials for electronic applications. This paper reports a method for the chemical bonding of vertically aligned CNTs onto metal substrates that avoids the need for high temperatures and can be performed at temperatures as low as 80 °C. Open-ended CNTs were directly bonded onto Cu and Pt substrates that had been functionalized using diazonium radical reactive species, thus allowing bond formation with the open-ended CNTs. Careful control during grafting of the organic species onto the metal substrates resulted in functional group uniformity, as demonstrated by FT-IR analysis. Scanning electron microscopy images confirmed the formation of direct connections between the vertically aligned CNTs and the metal substrates. Furthermore, electrochemical characterization and application as a sensor revealed the nature of the bonding between the CNTs and the metal substrates.
Self-assembled monolayers (SAMs) of alkanethiols on gold have become a central focus of controllable surface chemistry because they can be easily formed from the solution phase and characterized using various techniques. Understanding the formation processes occurring at a nanoscale level is crucial to form defect-free SAMs for tailored applications in bio- and nanotechnology. Although many reports study and characterize SAMs after they are formed on gold surfaces, typical methods have not extensively studied the SAM formation process at the nanoscale. This paper focuses on the formation of defect-free SAMs and elucidates the formation mechanism occurring at the nanoscale level during the formation process. Exploiting the strength of scanning electrochemical cell microscopy, we monitored SAM formation via a soluble redox reporter on a polycrystalline gold foil using voltammetric and amperometric techniques. We formed SAMs by varying the concentration of 3-mercapto-1-propanol [HS(CH2)3OH], 6-mercapto-1-hexanol [HS(CH2)6OH], and 9-mercapto-1-nonanol [HS(CH2)9OH] to determine the effects of the thiol chain length, concentration, and location on the substrate (grain boundaries) on monolayer formation. We observed real-time changes in the quasisteady-state current of our redox reporter during the self-assembly process. Importantly, we formed defect-free SAMs at the nanoscale level using different concentrations of HS(CH2)6OH and HS(CH2)9OH and found that SAM formation at the nanoscale is concentration-dependent and varies when at a boundary between two crystal grains.
Carbon nanotubes (CNTs) offer unique properties that have the potential to address multiple issues in industry and material sciences. Although many synthesis methods have been developed, it remains difficult to control CNT characteristics. Here, with the goal of achieving such control, we report a bottom-up process for CNT synthesis in which monolayers of premade aluminum oxide (Al2O3) and iron oxide (Fe3O4) nanoparticles were anchored on a flat silicon oxide (SiO2) substrate. The nanoparticle dispersion and monolayer assembly of the oleic-acid-stabilized Al2O3 nanoparticles were achieved using 11-phosphonoundecanoic acid as a bifunctional linker, with the phosphonate group binding to the SiO2 substrate and the terminal carboxylate group binding to the nanoparticles. Subsequently, an Fe3O4 monolayer was formed over the Al2O3 layer using the same approach. The assembled Al2O3 and Fe3O4 nanoparticle monolayers acted as a catalyst support and catalyst, respectively, for the growth of vertically aligned CNTs. The CNTs were successfully synthesized using a conventional atmospheric pressure-chemical vapor deposition method with acetylene as the carbon precursor. Thus, these nanoparticle films provide a facile and inexpensive approach for producing homogenous CNTs.
Implantable neural electrodes are generally used to record the electrical activity of neurons and to stimulate neurons in the nervous system. Biofouling triggered by inflammatory responses can dramatically affect the performance of neural electrodes, resulting in decreased signal sensitivity and consistency over time. Thus, long-term clinical applications require electrically conducting electrode materials with reduced dimensions, high flexibility, and antibiofouling properties that can reduce the degree of inflammatory reactions and increase the lifetime of neural electrodes. Carbon nanotubes (CNTs) are well known to form flexible assemblies such as CNT fibers. Herein, we report the covalent functionalization of predefined CNT fiber and film surfaces with hydrophilic, antibiofouling phosphorylcholine (PC) molecules. The electrochemical and spectroscopic characteristics, impedance properties, hydrophilicity, and in vitro antifouling nature of the functionalized CNT surfaces were evaluated. The hydrophilicity of the functionalized CNT films was demonstrated by a decrease in the static contact angle from 134.4°± 3.9°before to 15.7°± 1.5°after one and fully wetting after three functionalization cycles, respectively. In addition, the extent of protein absorption on the functionalized CNT films was significantly lower than that on the nonfunctionalized CNT film. Surprisingly, the faradic charge-transfer properties and impedance of the CNT assemblies were preserved after functionalization with PC molecules. These functionalized CNT assemblies are promising for the development of low-impedance neural electrodes with higher hydrophilicity and protein-fouling resistance to inhibit inflammatory responses.
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