Thermal desorption spectroscopy as a quantitative tool to determine the hydrogen content in solids

Thermal desorption spectroscopy (TDS) utilising a quadrupolar mass spectrometer is a highly sensitive and selective method to study the hydrogen desorption of hydrogen storage materials. For a quantitative analysis of the hydrogen storage capacity, the TDS apparatus can be consistently calibrated by using hydrogenated PdGd alloys or TiH2 as standards. Owing to its hygroscopic nature, the use of CaH2 as calibration standard leads to erroneous results. The chemical reactions during the thermal desorption of CaH2 are analysed in detail

Mixed state parameters of single crystalline Rb3C60 fullerene superconductors

We report on detailed magnetic investigations of big Rb3C60 single crystals with sizes of ~1 mm. The Rb3C60 crystals were prepared by doping C60 crystals in rubidium vapor. Experiments with different annealing times and various annealing temperatures and temperature gradients were made to assess the optimal conditions for homogeneous doping. The crystals were characterized by ac magnetization measurements. Doping at 463 K with 10% excess of rubidium and annealing at 685 K for 27 days was found to produce the best crystals with almost 100% of the pure Rb3C60 phase. The temperature dependence of the upper and lower critical fields was obtained, the latter by the trapped magnetic moment method. The coherence length and the penetration depth at T=0 and close to the transition temperature were evaluated and the irreversibility line was determined. The results are compared to those obtained on powder and polycrystalline samples

Closed-loop control of laser assisted chemical vapor deposition growth of carbon nanotubes

Laser-assisted chemical vapor deposition growth is an attractive mask-less process for growing locally aligned nanotubes in selected places on temperature sensitive substrates. An essential parameter for a successful and reproducible synthesis of nanotubes is the temperature during growth. Here, we demonstrate a temperature feedback control mechanism based on the dynamic, in situ monitoring of the infrared radiation coupled with reflectivity information. With the information provided by these sensors, an infrared laser, focused on a silicon substrate covered with aluminum-oxide and iron catalyst layers, can be controlled. The growth takes place in a gaseous mixture of argon (carrier gas), hydrogen (process gas), and ethylene (carbon-containing gas). Scanning electron microscopy and Raman spectroscopy analysis demonstrate the excellent reproducibility of the closed-loop control process over multiple experiments. Furthermore, we developed a unique method to identify the onset for catalyst formation and activation by monitoring the fluctuation of the reflected laser beam

Effects of charge impurities and laser energy on Raman spectra of graphene

The position and width of the Raman G-line was analyzed for unintentionally doped single-layered graphene samples. Results indicate a significant heating of the monolayer by the laser beam. Moreover, a weak additional component was resolved in the G-band. The position of the line is independent of the level of doping of the sample. We conclude that this new component is due to the phonons coupled to the intraband electronic transitions

Closed-loop control of laser assisted chemical vapor deposition growth of carbon nanotubes

Laser-assisted chemical vapor deposition growth is an attractive mask-less process for growing locally aligned nanotubes in selected places on temperature sensitive substrates. An essential parameter for a successful and reproducible synthesis of nanotubes is the temperature during growth. Here, we demonstrate a temperature feedback control mechanism based on the dynamic, in situ monitoring of the infrared radiation coupled with reflectivity information. With the information provided by these sensors, an infrared laser, focused on a silicon substrate covered with aluminum-oxide and iron catalyst layers, can be controlled. The growth takes place in a gaseous mixture of argon (carrier gas), hydrogen (process gas), and ethylene (carbon-containing gas). Scanning electron microscopy and Raman spectroscopy analysis demonstrate the excellent reproducibility of the closed-loop control process over multiple experiments. Furthermore, we developed a unique method to identify the onset for catalyst formation and activation by monitoring the fluctuation of the reflected laser beam. © 2012 American Institute of Physics

Carbon:nickel nanocomposite templates-predefined stable catalysts for diameter-controlled growth of single-walled carbon nanotubes

Carbon : nickel (C : Ni) nanocomposite templates (NCTs) were used as catalyst precursors for diameter-controlled growth of single-walled carbon nanotubes (SWCNTs) by chemical vapor deposition (CVD). Two NCT types of 2 nm thickness were prepared by ion beam co-sputtering without (type I) or with assisting Ar+ ion irradiation (type II). NCT type I comprised Ni-rich nanoparticles (NPs) with defined diameter in an amorphous carbon matrix, while NCT type II was a homogenous C : Ni film. Based on the Raman spectra of more than 600 individual SWCNTs, the diameter distribution obtained from both types of NCT was determined. SWCNTs with a selective, monomodal diameter distribution are obtained from NCT type I. About 50% of the SWCNTs have a diameter of (1.36 ± 0.10) nm. In contrast to NCT type I, SWCNTs with a non-selective, relatively homogeneous diameter distribution from 0.80 to 1.40 nm covering 88% of all SWCNTs are obtained from NCT type II. From both catalyst templates predominantly separated as-grown SWCNTs are obtained. They are free of solvents or surfactants, exhibit a low degree of bundling and contain negligible amounts of MWCNTs. The study demonstrates the advantage of predefined catalysts for diameter-controlled SWCNT synthesis in comparison to in situ formed catalysts.ISSN:2040-3364ISSN:2040-337

Closed-loop control of laser assisted chemical vapor deposition growth of carbon nanotubes

Laser-assisted chemical vapor deposition growth is an attractive mask-less process for growing locally aligned nanotubes in selected places on temperature sensitive substrates. An essential parameter for a successful and reproducible synthesis of nanotubes is the temperature during growth. Here, we demonstrate a temperature feedback control mechanism based on the dynamic, in situ monitoring of the infrared radiation coupled with reflectivity information. With the information provided by these sensors, an infrared laser, focused on a silicon substrate covered with aluminum-oxide and iron catalyst layers, can be controlled. The growth takes place in a gaseous mixture of argon (carrier gas), hydrogen (process gas), and ethylene (carbon-containing gas). Scanning electron microscopy and Raman spectroscopy analysis demonstrate the excellent reproducibility of the closed-loop control process over multiple experiments. Furthermore, we developed a unique method to identify the onset for catalyst formation and activation by monitoring the fluctuation of the reflected laser beam

Topochemical polymerization of C70 controlled by monomer crystal packing

Polymeric forms of C60 are now well known, but numerous attempts to obtain C70 in a polymeric state have yielded only dimers. Polymeric C70 has now been synthesized by treatment of hexagonally packed C70 single crystals under moderate hydrostatic pressure (2 gigapascals) at elevated temperature (300¡C), which conÞrms predictions from our modeling of polymeric structures of C70. Single-crystal x-ray diffraction shows that the molecules are bridged into polymeric zigzag chains that extend along the c axis of the parent structure. Solid-state nuclear magnetic resonance and Raman data provide evidence for covalent chemical bonding between the C70 cages.Upprättat; 2001; 20061110 (ysko)</p

Carbon : nickel nanocomposite templates – predefined stable catalysts for diameter-controlled growth of single-walled carbon nanotubes

Carbon : nickel (C : Ni) nanocomposite templates (NCTs) were used as catalyst precursors for diameter-controlled growth of single-walled carbon nanotubes (SWCNTs) by chemical vapor deposition (CVD). Two NCT types of 2 nm thickness were prepared by ion beam co-sputtering without (type I) or with assisting Ar+ ion irradiation (type II). NCT type I comprised Ni-rich nanoparticles (NPs) with defined diameter in an amorphous carbon matrix, while NCT type II was a homogenous C : Ni film. Based on the Raman spectra of more than 600 individual SWCNTs, the diameter distribution obtained from both types of NCT was determined. SWCNTs with a selective, monomodal diameter distribution are obtained from NCT type I. About 50% of the SWCNTs have a diameter of (1.36 ± 0.10) nm. In contrast to NCT type I, SWCNTs with a non-selective, relatively homogeneous diameter distribution from 0.80 to 1.40 nm covering 88% of all SWCNTs are obtained from NCT type II. From both catalyst templates predominantly separated as-grown SWCNTs are obtained. They are free of solvents or surfactants, exhibit a low degree of bundling and contain negligible amounts of MWCNTs. The study demonstrates the advantage of predefined catalysts for diameter-controlled SWCNT synthesis in comparison to in situ formed catalysts.ISSN:2040-3364ISSN:2040-337