Intercomparison of gas flow-rate measurements at IMGC, Italy, and UASG, Germany, in the range from 10 to 10 Pa m/s

Primary standard gas flow meters are developed for various applications such as calibration of leak artefacts, generation of calibration pressures by dynamic gas expansion and calibration of secondary standard gas flow meters. The Istituto di Metrologia “G. Colonnetti” (IMGC), Italy, and the University of Applied Sciences Giessen-Friedberg (UASG), Germany, maintain primary flow meters based on different principles in order to measure small gas flows delivered either to vacuum (i.e. practically zero pressure) or to atmosphere (ambient pressure). The principle, design and properties of these flow meters are described. Comparison of the primary standard flow meters maintained at these laboratories was performed over a range from 3×10⁻⁸ to 7×10⁻⁴ Pa m³/s with nitrogen, using a crimped capillary leak as a transfer standard. IMGC was the pilot laboratory. During the intercomparison, the transfer standard changed by ca. −2% for flow to vacuum and by ca. −4% for flow to atmosphere without obvious reason. The results of the intercomparison show that the laboratories agree within their expanded uncertainties over the measured range of gas flows.     

New leak element using sintered stainless steel filter for in-situ calibration of ionization gauges and quadrupole mass spectrometers

A new leak element using a sintered stainless steel filter with a pore size of less than 1 μm has been developed for in-situ calibrations of ionization gauges (IGs) and quadruple mass spectrometers (QMSs). The gas flow through this leak element realizes molecular flow at an upstream pressure of less than 10⁴ Pa. This new leak element, which is a kind of open-type standard leak, has four advantages. (1) Calibrations for various gas species are available only with this single leak element because the conductance is easily compensated for gas species by molecular mass. (2) Calibrations with multiple pressure points are easily available because the conductance is constant against changing upstream pressure. (3) Calibrations for a gas mixture are available because the interference effect between gas molecules in a gas mixture is negligible. (4) The dependence of flow rate on temperature is small and is compensated theoretically. These advantages were experimentally demonstrated. The stability and uncertainty of the leak element were also evaluated. The changes in the conductance of this leak element were less than 3% over one year. Since the conductance is typically 10⁻¹⁰ · m³/s, the reference gas flow in the range from 10⁻⁸ Pa · m³/s to 10⁻⁶ Pa m³ is obtained by changing the upstream pressure from 10² Pa to 10⁴ Pa with an uncertainty of approximately 6%.     

Microstructure tuning of epitaxial BaTiO3 − x thin films grown using laser molecular-beam epitaxy by varying the oxygen pressure

Microstructural properties are found to be variant in the BaTiO_3 − x films grown on SrTiO₃(001) substrate under various oxygen pressures from 2 × 10^− 2 Pa to 2 × 10^− 5 Pa by laser molecular-beam epitaxy. Transmission electron microscopic studies reveal that the predominant defects in the films change from threading dislocations into (111) planar defects (i.e. stacking faults and nanotwins) by lowering the oxygen pressure. High density of these defects was observed in the BaTiO_3 − x film prepared at the oxygen pressure of 2 × 10^− 5 Pa, which shows metallic behavior. The relationships between oxygen pressure, microstructure, and electrical properties are established on the basis of oxygen deficiency. The formation of nanotwins in highly oxygen-deficient BaTiO_3 − x epitaxial thin films results from accommodating excess oxygen vacancies induced by lowering oxygen pressure.     

High-speed pumping to UHV

Development of a high-speed pumping system for ultra high vacuum (UHV) process dose not reduce only cost and waiting time for experiment and production, but also reduces CO₂ emission that is known as one of the serious causes in the global warming problem. Reduction of vapor water concentration in a purge gas line would be one of the most effective measures to reduce pumping time to UHV. We carried out control of water vapor in a nitrogen gas purge line in addition to surface treatments of chambers using buff polishing and electrolytic polishing, followed by measurement of outgassing rate of the chambers. Under the reasonable control of the water vapor, the pumping time to reach the pressure of 1 × 10⁻⁶ Pa was able to be shortened with two orders of the magnitude. And it was also found that the main residual gas in the chamber was hydrogen after pumping down with the low concentration of water vapor. The quality of residual gas was equivalent to the quality in a baked UHV system. The introduction of well controlled nitrogen gas to the vacuum system which was not baked out during its pumping has proved a pressure of 3 × 10⁻⁸ Pa for 24 h in the chamber without orifice.     

Calibration of ultrahigh vacuum gauge from 10 Pa to 10 Pa by the two-stage flow-dividing system

A new two-stage flow-dividing system has been developed for the calibration of ultrahigh vacuum gauges from 10⁻⁹ Pa to 10⁻⁵ Pa for N₂, Ar, and H₂. This system is designed based on the techniques for our previously developed calibration system in the range from 10⁻⁷ Pa to 10⁻² Pa. Three modifications were performed to extend the calibration pressure to a lower range. The relative standard uncertainty of the generated pressure (k = 1) is in the range from 2.3% to 2.6%, from 10⁻⁹ Pa to 10⁻⁵ Pa. The characteristics of ultrahigh vacuum gauges were also examined by using this system. The stabilities of the pressure reading, the linearity, the temperature dependence, and the long-term stability were examined. These results show that the calibration of ultrahigh vacuum gauges is possible in the range from 10⁻⁹ Pa to 10⁻⁵ Pa for N₂, Ar, and H₂ with the uncertainty of about 6.0% (k = 2) by this new system.     

Effects of oxygen pressure on the growth of pulsed laser deposited ZnO films on Si(0 0 1)

ZnO thin films were prepared on Si(0 0 1) substrates using a pulsed laser deposition (PLD) technique and then their growth and properties were investigated particularly as a function of ambient O₂ pressure during film growth. It was found that the microstructure, crystallinity, orientation and optical properties of the films grown are strongly dependent on the O₂ pressures used. Completely c-axis oriented ZnO films are grown in a low O₂ pressure regime (5×10⁻⁴-5×10⁻² Torr), whereas a randomly oriented film with a much lower crystallinity and a rougher grained-surface is grown at an O₂ pressure of 5×10⁻¹ Torr. This deterioration in film quality may be associated with the kinetics of atomic arrangements during deposition. Our results suggest that ambient O₂ pressure is an important processing parameter and should be optimized in a narrow regime in order to grow a ZnO film of good properties in PLD process.     

Oxide-ion conductivity in CuxCe1−xO2−δ (0 ≤ x ≤ 0.10)

Up to 10 at.% of copper readily substitutes for cerium in ceria. It is found that at oxygen partial pressures between 0.21 atm and 10⁻⁵ atm, Cu_xCe_1−xO_2−δ (0 ≤ x ≤ 0.10) solid solution behave as an oxide-ion electrolyte. Interestingly, Cu_0.10Ce_0.90O_2−δ exhibits the oxide-ion conductivity of ca. 10⁻⁴ Ω⁻¹ cm⁻¹ at 600 °C at an oxygen partial pressure of 10⁻⁵ atm.     

Forbidden energy band gap in diluted a-Ge1 − xSix:N films

By means of electron gun evaporation Ge_1 − xSi_x:N thin films, in the entire range 0 ≤ x ≤ 1, were prepared on Si (100) and glass substrates. The initial vacuum reached was 6.6 × 10^− 4 Pa, then a pressure of 2.7 × 10^− 2 Pa of high purity N₂ was introduced into the chamber. The deposition time was 4 min. Crucible-substrate distance was 18 cm. X-ray diffraction patterns indicate that all the films were amorphous (a-Ge_1 − xSi_x:N). The nitrogen concentration was of the order of 1 at% for all the films. From optical absorption spectra data and by using the Tauc method the energy band gap (E_g) was calculated. The Raman spectra only reveal the presence of SiSi, GeGe, and SiGe bonds. Nevertheless, infrared spectra demonstrate the existence of SiN and GeN bonds. The forbidden energy band gap (E_g) as a function of x in the entire range 0 ≤ x ≤ 1 shows two well defined regions: 0 ≤ x ≤ 0.67 and 0.67 ≤ x ≤ 1, due to two different behaviors of the band gap, where for x > 0.67 exists an abruptly change of E_g(x). In this case E_g(x) versus x is different to the variation of E_g in a-Ge_1 − xSi_x and a-Ge_1 − xSi_x:H. This fact can be related to the formation of Ge₃N₄ and GeSi₂N₄ when x ≤ 0.67, and to the formation of Si₃N₄ and GeSi₂N₄ for 0.67 ≤ x.     

Influence of SnO2 addition on the thermoelectric properties of Zn1 − xSnxO (0.01 ≤ x ≤ 0.05)

The grain size and the density of the Zn_1 − xSn_xO (0 ≤ x ≤ 0.05) samples decreased with increasing SnO₂ content. The addition of a small amount of SnO₂ (x ≤ 0.01) to ZnO led to an increase in both the electrical conductivity and the absolute value of the Seebeck coefficient, resulting in a significant increase in the power factor. The thermoelectric power factor was maximized to a value of 1.25 × 10⁻³ Wm⁻¹ K⁻² at 1073 K for the Zn_0.99Sn_0.01O sample.     

Ionization vacuum gauge with a carbon nanotube field electron emitter combined with a shield electrode

The applicability of carbon nanotubes to an electron source for a Bayard-Alpert type vacuum gauge has been investigated. Three gauge configurations are designed to optimize the gauge performance. The optimized gauge, in which an additional shield electrode is fixed on a gate electrode, exhibits good measurement of linearity between ion current and system pressure from 10⁻⁷ to 10⁻² Pa. A gauge sensitivity of 0.05 Pa⁻¹ has been achieved under 100 μA emission current for nitrogen, comparable with 0.07 Pa⁻¹ of commercial ionization gauges.     

Fabrication and infiltration kinetics analysis of Ti-coated diamond/copper composites with near-net-shape by pressureless infiltration

The Ti-coated diamond/copper composites with near-net-shape are manufactured by pressurelessly infiltrating liquid copper into porous Ti-coated diamond preforms. The contact angle between diamond and copper, relative density, thermal conductivity (TC), coefficient of thermal expansion (CTE), leak rate and microstructure are evaluated and characterized. In addition, the numerical analysis of the pressureless infiltration kinetics is also discussed. The results indicate that the relative density, TC and CTE of composites are 99.3%, 385 Wm⁻¹ k⁻¹ and 3–8 × 10⁻⁶ K⁻¹, respectively. It can meet heat-sink package requirement of high-power electronic devices as LED, insulated gate bipolar transistor (IGBT), etc. The liquid copper exhibits a turbulent flow with the Reynolds number in the range of 27.83–49.7. The porosity ? and the pressure drop Δp are the main influence factors controlling the velocity of liquid copper. Moreover, under vacuum condition of 8.7 × 10⁻³ Pa, the maximum theoretical infiltration length L_max of Ti-coated diamond/copper composites is found to be 552 mm.     

Hot-wire chemical vapor deposition of silicon nanoparticles on fused silica

Silicon nanoparticles on fused silica have potential as recombination centers in infrared detectors due quantum confinement effects that result in a size dependent band gap. Growth on fused silica was realized by etching in HF, annealing under vacuum at 700-750 °C, and cooling to ambient temperature before ramping to the growth temperature of 600 °C. Silicon particles could not be grown in a thermal chemical vapor deposition (CVD) process with adequate size uniformity and density. Seeding fused silica with Si adatoms in a hot-wire chemical vapor deposition (HWCVD) process at a disilane pressure of 1.1 × 10^− 5 Pa followed by thermal CVD at a disilane pressure of 1.3 × 10^− 2 Pa, or direct HWCVD at a disilane pressure of 2.1 × 10^− 5 Pa led to acceptable size uniformity and density. Dangling bonds at the surface of the as-grown nanoparticle were passivated using atomic H formed by cracking H₂ over the HWCVD filament.     

Negative thermal expansion and electrical properties of Mn3(Cu0.6NbxGe0.4 − x)N (x = 0.05-0.25) compounds

Bulk materials with the general formula of Mn₃(Cu_0.6Nb_xGe_0.4 − x)N (x = 0.05, 0.1, 0.15, 0.2, 0.25), Mn₃(Cu_0.6Ge_0.4)N and Mn₃(Cu_0.7Ge_0.3)N were fabricated by mechanical ball milling and solid state sintering. Their thermal expansion coefficients and electrical conductivities were investigated in the temperature range of 80-300 K. It is found that the temperature interval of negative temperature expansion behavior is about 95 K in the samples of Mn₃(Cu_0.6Nb_0.15Ge_0.25)N and Mn₃(Cu_0.6 Nb_0.2Ge_0.2)N, which is twice as large as that of Mn₃(Cu_0.7Ge_0.3)N. The negative thermal expansion of Mn₃(Cu_0.6Nb_0.15Ge_0.25)N can reach to − 19.5 × 10⁻⁶ K^− 1 in the temperature range of 165 to 210 K. The electrical conductivity of this series materials is in a level of about 2.5 × 10⁶ (Ω m)^− 1.     

Effect of base and oxygen partial pressures on the electrical and optical properties of indium molybdenum oxide thin films

Indium molybdenum oxide thin films were RF sputtered at room temperature on glass substrates with a reference base pressure of 7.5 × 10^− 4 Pa. The electrical and optical properties of the films were studied as a function of oxygen partial pressures (OPP) ranging from 1.5 × 10^− 3 Pa to 3.5 × 10^− 3 Pa. The obtained data show that the bulk resistivity of the films increased by about 4 orders of magnitude (from 7.9 × 10^− 3 to 7.6 × 10¹ Ω-cm) when the OPP increased from 1.5 × 10⁻³ to 3.5 × 10^− 3 Pa, and the carrier concentration decreased by about 4 orders (from 1.77 × 10²⁰ to 2.31 × 10¹⁶ cm^− 3). On the other hand, the average visible transmittance of 30.54% of the films (brown colour; OPP = 1.5 × 10^− 3 Pa) was increased with increasing OPP to a maximum of 80.47% (OPP = 3.5 × 10^− 3 Pa). The optical band gap calculated from the absorption edge of the transmittance spectra ranges from 3.77 to 3.88 eV. Further, the optical and electrical properties of the films differ from those deposited at similar conditions but with a base pressure lower than 7.5 × 10^− 4 Pa.     

Low-resistance p-type ohmic contacts for high-power InGaAs/GaAs-980 nm CW semiconductor lasers

In this paper, the optimization of ohmic contacts for semiconductor lasers based on InGaAs/GaAs/GaAlAs layers is reported. Transmission electron microscopy (TEM) and electrical methods were used to study extensively the Pt/Ti/Pt/Au metallization system. The contact fabrication technology was optimized towards achieving the lowest electrical resistance. The technological control and optimization concerned the contact annealing temperature and thickness of metallic layers that form the contact. The average specific contact resistance was below 5×10⁻⁶ Ω cm² (with the record value of 8×10⁻⁷ Ω cm²) for the 10 nm Pt/20 nm Ti/30 nm Pt/150 nm Au system. The presented system was used in fabrication of continuous wave (CW) operated laser diodes. The chips mounted on passively cooled copper block achieved optical powers over 1 W, threshold current density values of 140-160 A/cm² and differential efficiencies above 1 W/A. The value of the characteristic temperature T₀ for discussed lasers varied in the range of 180-200 K.     

Stability tests of ionization gauges using two-stage flow-dividing system

Stability tests of four ionization gauges (a BA gauge, an extractor gauge, an AT gauge, and a BA gauge with a heating electrode) were performed using a two-stage flow-dividing system from four viewpoints: (1) the fluctuation and drift of pressure readings, (2) the repeatability of pressure readings, (3) the change in sensitivity owing to prior conditions of use and (4) long-term stability. These tests were performed at pressures from 8 × 10⁻⁶ Pa to 8 × 10⁻⁴ Pa using N₂ gas under tightly controlled conditions.The fluctuation and drift of the four IGs were within 1% over 1 h. Their repeatability was also within 1% during eight cycles with an interval of 1 h between each cycle. Although changes in sensitivity of several percent owing to prior conditions of use were observed, the sensitivity was recovered to within 1% of its original values after operation in ultrahigh vacuum for one day. The result of a long-term stability test over a year showed that the sensitivity of the four IGs tended to decrease by 2.6-5.4% due to aging, depending on the gauge.     

Hydrogen atom density in a solar plasma reactor

A density of neutral hydrogen atoms was systematically measured in the MESOX solar plasma reactor at different MW powers and flow rates. The H-atom density was measured by a gold fibre optics catalytic probe. The H-atom density was in general increasing with increasing MW power. At a pressure of 40 Pa and a power of 500 W it was about 3.5 × 10²¹ m⁻³ and at a power of 1000 W it was about 4.1 × 10²¹ m⁻³. A degree of dissociation of hydrogen molecules was between 3% and 20% depending on pressure and power. A maximum degree of dissociation was obtained at a pressure of 40 Pa and 1000 W, while the lowest one at 130 Pa and 500 W.     

Applicability of self-consistent global model for characterization of inductively coupled Cl2 plasma

Investigations of the influence of gas pressure and input power on the Cl₂ plasma parameters in the inductively coupled plasma system were carried out. The investigations combined plasma diagnostics by Langmuir probe with plasma modeling represented by the self-consistent global model with Maxwellian approximation for the electron energy distribution function. From the experiments, it was found that the increase of gas pressure in the range of 0.27-3.33 Pa for 400-700 W of input power results in a decrease in both electron temperature (3.3-2.0 eV) and density (6.5×10¹⁶−3.0×10¹⁶ m⁻³ for 400 W and 1.2×10¹⁷-6.7×10¹⁶ m⁻³ for 700 W). For the given range of experimental conditions, the model showed an outstanding agreement with the experiments and provided the data on kinetics of plasma active species, their densities and fluxes.     

A low-voltage Penning cell for vacuum measurement and vacuum technology

This paper presents new results on the performance of a special cold-cathode gauge. The use of an AC and DC voltage simultaneously as the power source makes it possible to ignite and sustain a discharge at a significantly lower voltage than normal over a wide pressure range (from 5 to 3×10⁻⁶ Pa). The Penning discharge voltage can be as low as 20 V at a pressure of 0.3 Pa and 300 V in high vacuum. For low values of pressure, the discharge current has a monotonously increasing dependence on the gas pressure. If a low RF voltage is applied to a high-voltage DC discharge, the discharge current increases in many times. These discharge properties can be used to improve the performance of devices that use the Penning and other magnetic discharges (total and partial pressure gauges, leak detectors, ion pumps, ion sources and hot plasma sources). A vacuum gauge of this type combines the best features of magnetic discharge and hot cathode ionization gauges.     

Optimization of sputtering parameters for deposition of Al-doped ZnO films by rf magnetron sputtering in Ar + H2 ambient at room temperature

The effects of sputtering pressure and power on structural and optical-electrical properties of Al-doped ZnO films were systemically investigated at substrate temperature of room temperature and H₂/(Ar + H₂) flow ratio of 5%. The results show that carrier concentration and mobility of the films show nonmonotone change due to the evolution of microstructure and lattice defect of the films caused by introduction of H₂ with increasing sputtering pressure and power. The transmittance of the films is also found to be related to the introduction of H₂ in addition to usually considered surface roughness and crystallinity. Finally, optimized sputtering pressure and power are 0.8 Pa and 100 W, respectively, and obtained minimum resistivity and highest transmittance are 1.43 × 10^− 3 Ω·cm and 90.5%, respectively. In addition, it is found that E_g of the films is mainly controlled by the carrier concentration, but crystallite size and stress should also be considered for the films deposited at different powers.