KATRIN NEG pumping concept investigation

The Karlsruhe Tritium Neutrino experiment (KATRIN) is going to use a very large electro-static tandem spectrometer to measure the electron spectrum from the tritium beta decay, where several kilometers of non-evaporable getter (NEG) strips (type ST707) are to be used to achieve the UHV requirements. Different geometrical configurations of the NEG strips have been studied by Monte Carlo simulations. It is shown that the resulting pumping speed of the getter pumps will allow to get a pressure below 10⁻¹¹ mbar in the huge vessel with a volume of 1400 m³. By systematic assessment of the statistics of the pumping surfaces, it could be demonstrated that the design is sound.     

Test Particle Monte-Carlo modelling of installations for NEG film pumping properties evaluation

Two installations were built in the ASTeC vacuum science laboratory to investigate the pumping properties of non-evaporable getter (NEG) films. An important parameter to characterise the pumping properties is the film sticking probability (α). Test Particle Monte-Carlo (TPMC) models were used for accurate evaluation of NEG film sticking probability from pressure readings during gas injection. The results of these models were used for interpreting the results of measurements in different experimental configurations: planar, cup and tubular samples. It was shown that there is a difference between simple formulas used in vacuum technique and TPMC results which is significant for α > 0.1 with planar samples, for α > 0.01 with cup samples, and in the full range of α for tubular samples. It was also shown that the gauge positions are very important, the exact position of the gauge or RGA ionisation chamber should be used in the modelling.     

Residual surface oxide on ZrV getter—XPS, LEIS and SIMS study

The activated ZrV non-evaporable getter (NEG) film has been studied by means of X-ray photoelectron spectroscopy, low-energy ion scattering and secondary ion mass spectrometry. In this work, we found that the first atomic layer of the thermally activated ZrV NEG consists mainly of zirconium atoms, which are partly oxidized. The residual zirconium suboxides observed on thermally activated ZrV NEG diminish during ion sputtering of NEG surface. It indicates that residual suboxides are located mainly in the top surface layer.     

Measuring volume ratios of vacuum vessels using non-evaporable getters

Several methods have been used in vacuum metrology for volume determination. Volume ratios can be determined by different gas expansion methods, which were primarily developed for the precise determination of expansion ratios in static expansion systems. Measurements of the volume ratios using the gas expansion methods below 10⁻² Pa are influenced by outgassing from chamber walls. To reduce outgassing in the expansion chambers during measurements at low pressures, we have installed non-evaporable getter (NEG) pumps, which pump hydrogen and other active gases but have a negligible pumping speed for inert gases. The volume ratio of two chambers of an experimental static expansion system has thus been measured using the inert gases argon, helium and krypton. The obtained results were compared with the measurements without the use of an NEG pump. Measurements of the pressure ratios were performed with a spinning rotor gauge (SRG).     

LHC: The world's largest vacuum systems being operated at CERN

With the successful circulation of beams in the Large Hadron Collider (LHC), its vacuum system becomes the world's largest vacuum system under operation. This system is composed of 54 km of ultra high vacuum (UHV) for the two circulating beams and about 50 km of insulation vacuum around the cryogenic magnets and the liquid helium transfer lines (QRL). The LHC complex is completed by 7 km of high vacuum transfer lines for the injection of beams from the SPS and their dumping.Over the 54 km of UHV beam vacuum, 48 km are at cryogenic temperature (1.9 K), the remaining 6 km are at ambient temperature and use extensively non-evaporable getter (NEG) coatings, a technology that was born and industrialised at CERN.The cryogenic insulation vacuum systems, less demanding technically, impress by their size and volume: 50 km and 15,000 m³. Once cooled at 1.9 K, the cryopumping allows pressure in the 10⁻⁴ Pa range to be attained.     

Surface characterization of activated Ti-Zr-V NEG coatings

The thermally activated Ti-Zr-V non-evaporable getter (NEG) film has been studied by means of X-ray photoelectron spectroscopy (XPS) and low energy ion scattering (LEIS). Depth profiling technique has been used to establish the location of different components in the near-surface region. It was found that the top surface layer of the activated Ti-Zr-V NEG film is zirconium and titanium enriched. Residual oxide observed even on fully activated NEG surface consists mostly of zirconium and titanium low valence suboxides that are located mainly in the top surface layer. Carbides formed during the activation process remain on the surface and their concentration drops strongly with depth.     

Influence of oxygen pressure on the structural, electrical and optical properties of VO2 thin films deposited on ZnO/glass substrates by pulsed laser deposition

The influence of oxygen pressure on the structural and electrical properties of vanadium oxide thin films deposited on glass substrates by pulsed laser deposition, via a 5-nm thick ZnO buffer, was investigated. For the purposes of comparison, VO₂ thin films were also deposited on c-cut sapphire and glass substrates. During laser ablation of the V metal target, the oxygen pressure was varied between 1.33 and 6.67 Pa at 500 °C, and the interaction and reaction of the VO₂ and the ZnO buffer were studied. X-ray diffraction studies showed that the VO₂ thin film deposited on a c-axis oriented ZnO buffer layer under 1.33 Pa oxygen had (020) preferential orientation. However, VO₂ thin films deposited under 5.33 and 6.67 Pa were randomly oriented and showed (011) peaks. Crystalline orientation controlled VO₂ thin films were prepared without such expensive single crystal substrates as c-cut sapphire. The metal-insulator transition properties of the VO₂/ZnO/glass samples were investigated in terms of electrical conductivity and infrared reflectance with varying temperatures, and the surface composition was investigated by X-ray photoelectron spectroscopy.     

Corrosion protection of ENIG surface finishing using electrochemical methods

Four types of thin film coating were carried out on copper for electronic materials by the electroless plating method at a pH range from 3 to 9. The coating performance was evaluated by electrochemical impedance spectroscopy and potentiodynamic polarization testing in a 3.5 wt.% NaCl solution. In addition, atomic force microscopy and X-ray diffraction were also used to analyze the coating surfaces. The electrochemical behavior of the coatings was improved using the electroless nickel plating solution of pH 5. The electroless nickel/immersion gold on the copper substrate exhibited high protective efficiency, charge transfer resistance and very low porosity, indicating an increase in corrosion resistance. Atomic force microscopy and X-ray diffraction analyses confirmed the surface uniformity and the formation of the crystalline-refined NiP {1 2 2} phase at pH 5.     

Novel Ga-doped ZnO nanocrystal ink: Synthesis and characterization

Ga-doped ZnO (GZO) nanocrystals were synthesized via the hot-injection method for the first time. The characterizations of its structure, composition, morphology, and absorption properties were conducted by using powder X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM) and UV-vis absorption spectroscopy. The results indicated that GZO nanocrystals were single phase polycrystalline within a range of 5―10 nm. Optical measurements illustrated that GZO nanocrystals have a tunable band gap from 3.35 to 3.81 eV, depending on the Ga doping level. GZO nanocrystals were dispersed in nonpolar solvents to form a nanocrystal ink which could remain stable after a month of storage. The GZO thin film was fabricated by spin coating the GZO nanocrystal ink and annealing in air. The electrical resistivity of the film was measured to be 7.5 × 10⁻² Ω cm. This method, which eliminated the requirement of high vacuum and high temperature, was a promising alternative for transparent conducting oxide (TCO) fabrication.     

Influence of ambient air exposure on surface chemistry and electronic properties of thin copper phthalocyanine sensing layers

In this paper we present photoemission studies of the influence of 12-hour exposure to the ambient air on the chemical and electronic properties of thin 16-nm copper phthalocyanine (CuPc) sensing layers deposited on n- and p-type silicon Si(111) substrates covered with the native oxide. The surface chemistry and electronic parameters of organic thin film including surface band bending, work function, electron affinity and their variations upon the exposure have been monitored with X-ray photoemission spectroscopy and ultraviolet photoemission spectroscopy techniques. We found that after the exposure, the surface chemistry of CuPc remained unaffected, however the work function and surface band bending increased by 0.55 eV and 0.45 eV for the layers on n-Si and by 0.25 eV and 0.30 eV for those on p-Si. Additionally, we detected a slight surface dipole at CuPc on n-Si manifested by a small shift in electron affinity of 0.10 eV. In order to explain these changes we developed a model basing on the interaction of ionic species with the phthalocyanine surface.     

A comparative study on the NO2 gas sensing properties of ZnO thin films, nanowires and nanorods

ZnO thin films were fabricated using the spin coating method, ZnO nanowires by cathodically induced sol-gel deposition by the means of an anodic aluminum oxide (AAO) template, and ZnO nanorods with the hydrothermal technique. For thin film preparation, a clear, homogeneous and stable ZnO solution was prepared by the sol-gel method using zinc acetate (ZnAc) precursor which was then coated on a glass substrate with a spin coater. Vertically aligned ZnO nanowires which were approximately 65 nm in diameter and 10 μm in length were grown in an AAO template by applying a cathodic voltage in aqueous zinc nitrate solution at room temperature. For fabrication of the ZnO nanorods, the sol-gel ZnO solution was coated on glass substrate by spin coating as a seed layer. Then ZnO nanorods were grown in zinc nitrate and hexamthylenetetramine aqueous solution. The ZnO nanorods are approximately 30 nm in diameter and 500 nm in length. The ZnO thin film, ZnO nanowires and nanorods were characterized by X-ray diffraction (XRD) analysis and scanning electron microscope (SEM). The NO₂ gas sensing properties of ZnO thin films, nanowires and nanorods were investigated in a dark chamber at 200 °C in the concentration range of 100 ppb-10 ppm. It was found that the response times of both ZnO thin films and ZnO nanorods were approximately 30 s, and the sensor response was depended on shape and size of ZnO nanostructures and electrode configurations.     

Design of the vacuum system for Diamond, the UK third generation light source

The Diamond synchrotron, which is due to come into operation with beam for users in 2007, is being constructed at the Rutherford Appleton Laboratory, Oxford. The design status of the vacuum system of the storage ring as at 31st December 2002 will be reported.Diamond is based on a 24 cell 3 GeV electron storage ring of 561.6 m circumference. As is the case for most such machines, the operational pressure has been specified as 10⁻⁹ mbar to give a beam lifetime >10 h at the design current of 300 mA. The storage ring vacuum system will use conventional technology and most of the vacuum vessels will be constructed of stainless steel. With the exception of the insertion device (ID) vacuum chambers, the ring has not been designed to be baked in situ, but all components will be vacuum baked as sub assemblies before installation. The vacuum system is designed to achieve the required pressure after 100 A h of beam conditioning using the pumping scheme, which will be described.Twenty-one ID straights are available for ID, of which seven will be installed at the start of operations. Three types of vacuum vessel will be used in these straights, a stainless-steel make-up pipe, a NEG coated narrow-gap vacuum chamber for conventional IDs and a wider vacuum chamber to house in vacua IDs. The ID straights have an isolation valve installed at each end, and in situ baking can be used in these restricted locations, for example to activate the NEG coatings.The vacuum system for the beam line front ends has been designed to provide good vacuum isolation between the storage ring and the experimental beam lines, whether or not an interposing window is fitted.Pumping schemes, pressure measurement and calculated pressure profiles will be described.     

The effect of sputtering pressure on electrical, optical and structure properties of indium tin oxide on glass

Indium tin oxide (ITO) thin layers were deposited onto glass substrates by RF magnetron sputtering using different pressures. Subsequently, the films were annealed in a reducing atmosphere at 500 °C for 30 min. Electrical properties were measured by Hall Effect analysis and four-point probe measurements. Optical properties were determined by UV-Vis spectrophotometery. Film structures and compositions were analyzed by X-ray diffractometry and X-ray photoelectron spectroscopy, respectively. The effect of sputter pressure and additional anneals was investigated. The results revealed that the lowest resistivity of 1.69 × 10^− 4 Ω cm was achieved at low pressure (1.2 Pa) and the highest transmittance of ~ 90% was obtained after a second anneal. However, the second anneal decreased the mobility and the conductivity especially for high sputtering pressures. This study also describes the effect of Sn defect clustering on electrical properties of the ITO films.     

Operational experience and relation to deposition process for NEG-coated chambers installed on the ESRF electron storage ring

A majority of the ESRF insertion device sections have been equipped with NEG-coated low gap vacuum chambers made of extruded aluminium and PVD coated with a low-temperature non-evaporable getter coating at ESRF. The low initial outgassing and quick conditioning allowed some modifications for chamber installation and accelerator restart procedures. The operational behaviour of those chambers has been studied not only by means of vacuum gauges but also with ionisation chambers measuring the bremsstrahlung sent to the connected synchrotron beamlines. The NEG-coating film thickness was optimised taking into account vacuum performance and also coating process parameters and duration. The 2nd more flexible and powerful NEG-coating device is under commissioning in the NEG-coating facility at ESRF.     

Chemical vapor deposition and characterization of nitrogen doped TiO2 thin films on glass substrates

Photocatalytically active, N-doped TiO₂ thin films were prepared by low pressure metalorganic chemical vapor deposition (MOCVD) using titanium tetra-iso-propoxide (TTIP) as a precursor and NH₃ as a reactive doping gas. We present the influence of the growth parameters (temperature, reactive gas phase composition) on the microstructural and physico-chemical characteristics of the films, as deduced from X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), secondary ion mass spectrometry (SIMS) and ultra-violet and visible (UV/Vis) spectroscopy analysis. The N-doping level was controlled by the partial pressure ratio R = [NH₃]/[TTIP] at the entrance of the reactor and by the substrate temperature. For R = 2200, the N-doped TiO₂ layers are transparent and exhibit significant visible light photocatalytic activity (PA) in a narrow growth temperature range (375-400 °C). The optimum N-doping level is approximately 0.8 at.%. However, the PA activity of these N-doped films, under UV light radiation, is lower than that of undoped TiO₂ films of comparable thickness.     

Further studies on the lithium phosphorus oxynitride solid electrolyte

First step in the way to the fabrication of an all-solid microbattery for autonomous wireless sensor node, amorphous thin solid films of lithium phosphorus oxynitride (LiPON) were prepared by radio-frequency sputtering of a mixture target of P₂O₅/Li₂O in ambient nitrogen atmosphere. The morphology, composition, and ionic conductivity were characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, and A.C. impedance spectroscopy. With a thickness of 1.4 μm, the obtained LiPON amorphous layer provided an ionic conductivity close to 6 × 10⁻⁷ S cm⁻¹ at room temperature. MicroRaman UV spectroscopy study was successfully carried out for the first time on LiPON thin films to complete the characterization and bring further information on LiPON structure.     

Photoinduced hydrophobic surface of graphene oxide thin films

Graphene oxide (GO) thin films were deposited on transparent conducting oxide substrates and glass slides by spin coating method at room temperature. The wettability of GO thin films before and after ultraviolet (UV) irradiation was characterized with water contact angles, which increased from 27.3° to 57.6° after 3 h of irradiation, indicating a photo-induced hydrophobic surface. The UV-vis absorption spectra, Raman spectroscopy, X-ray photoelectron spectroscopy, and conductivity measurements of GO films before and after UV irradiation were taken to study the mechanism of photoinduced hydrophobic surface of GO thin films. It is demonstrated that the photoinduced hydrophobic surface is ascribed to the elimination of oxygen-containing functional groups on GO molecules. This work provides a simple strategy to control the wettability properties of GO thin films by UV irradiation.     

Optimization of thermoelectric properties on Bi2Te3 thin films deposited by thermal co-evaporation

The optimization of the thermal co-evaporation deposition process for n-type bismuth telluride (Bi₂Te₃) thin films deposited onto polyimide substrates and intended for thermoelectric applications is reported. The influence of deposition parameters (evaporation rate and substrate temperature) on film composition and thermoelectric properties was studied for optimal thermoelectric performance. Energy-dispersive X-ray spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy and Raman spectroscopy confirmed the formation of Bi₂Te₃ thin films. Seebeck coefficient (up to 250 μV K^− 1), in-plane electrical resistivity (≈10 μΩ m), carrier concentration (3×10¹⁹-20×10¹⁹ cm^− 3) and Hall mobility (80-170 cm² V⁻¹ s^− 1) were measured at room temperature for selected Bi₂Te₃ samples.     

Synthesis, crystal structure and thermal decomposition of [La2(CH3CH2COO)6·(H2O)3]·3.5H2O precursor for high-k La2O3 thin films deposition

Lanthanum acetylacetonate La(C₅H₇O₂)₃·xH₂O has been used in the preparation of the precursor solution for the deposition of polycrystalline La₂O₃ thin films on Si(1 1 1) single crystalline substrates. The precursor chemistry of the as-prepared coating solution, precursor powder and precursor single crystal have been investigated by Fourier Transformed Infrared Spectroscopy (FTIR), differential thermal analysis coupled with quadrupole mass spectrometry (TG-DTA-QMS) and X-ray diffraction. The FTIR and X-ray diffraction analyses have revealed the complex nature of the coating solution due to the formation of a lanthanum propionate complex. The La₂O₃ thin films deposited by spin coating on Si(1 1 1) substrate exhibit good morphological and structural properties. The films heat treated at 800 °C crystallize in a hexagonal phase with the lattice parameters a = 3,89 Å and c = 6.33 Å, while at 900 °C the films contain both the hexagonal and cubic La₂O₃ phase.     

Characterization of electrochemically deposited Cu-Ni black coatings

Electrochemically deposited Cu-Ni black coatings on molybdenum substrate from ethylenediaminetetraacetic acid (EDTA) bath solution are shown to exhibit good optical properties (α=0.94, ε = 0.09). The deposit is characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). Cu is present in metallic and +2 oxidation states in the as-prepared Cu-Ni black coating, whereas Ni²⁺ as well as Ni³⁺ species are observed in the same coating. Cu and Ni are observed in their metallic state after 10 and 20 min sputtering. X-ray initiated Auger electron spectroscopy (XAES) of Cu and Ni also agrees well with XPS investigations.