Techniques of vacuum pumping in multi-layer insulated cryogenic vessels

The improvement in heat transfer properties obtained by use of Multi-Layer Insulation (MLI) is reviewed. The introduction of many closely spaced layers of material increases considerably the surface exposed to vacuum and flow restrictions. Experiments have been made to demonstrate that by using correct pump-down procedures the inherent difficulties can be dealt with and the improved insulation properties of MLI can be used to full advantage in laboratory cryostats which are vented and re-pumped frequently. The test apparatus, procedure and calculation are shown in detail. Test results show that the heat losses of MLI at 10⁻⁴ torr are about 10 per cent of the losses of vacuum insulation only at 10⁻⁶ torr. Heat transfer of MLI remains constant at pressures below 10⁻³ … 10⁻⁴ torr. Recommended pump down procedures are given for equipment which is occasionally vented. The importance of cleanliness during installation of MLI, of the use of heating and getter materials is demonstrated. Pump down times to 10⁻⁴ torr of 5 … 6 h after venting were easily obtained in the test system.     

The influence of O2 and N2 on the hall and field effect mobilities in CdSe and PbTe thin films

Thin films of CdSe and PbTe were evaporated onto SiO in a vacuum system in which a pressure of less than 5 × 10⁻¹⁰ torr was available. The Hall and field effect measurements were made directly after producing the sample. Furthermore, these measurements were repeated under various partial pressures of O₂ and N₂ up to nearly 10⁺² torr. A remarkable influence of these gases on the mobilities was observed. One can understand this effect by considering that p-type regions are formed at the surface of the n-type semiconductors and thus a diminution of the measured mobilities occurs.     

Correlation of the equilibrium adsorption isotherms of low temperature cryodeposits

The applicability of several existing adsorption theories for predicting the equilibrium isotherms for. the sorption of hydrogen by carbon dioxide cryodeposits has been examined in the pressure range from 10⁻⁸ to 10⁻³ torr (1 torr = 133 N m⁻²). It is demonstrated that the H₂ sorption capacity of CO₂ frost cryosorbents at temperatures between 12 and 20 K may be accurately predicted by an equilibrium isotherm equation proposed by Dybinin and Raduschkevich. This equation is then used to calculate families of sorption isotherms for CO₂ frosts formed at various conditions and consequently having different structures. These results may be used to estimate the H₂ capacity of cryosorption pumping systems which would employ CO₂ frost as a cryosorbent. The applicability of this semi-empirical method to other frost sorbent-sorbate combinations is also reviewed.     

The cryopumping of water vapour in the continuum pressure region

Pumping speed measurements in the continuum pressure region, P>10^?3 torr, have been made for water vapour impinging on copper spheres and coils cooled to liquid nitrogen temperatures. Water vapour flow rates between 0.06 mg s^?1 and 420 mg s^?1 were used. The volumetric pumping speed was constant over the pressure range 2 × 10^?3 torr to 2 × 10^?2 torr and was, as expected, higher than that obtained in the free molecular flow region. Above 2 × 10^?2 torr the pumping speed decreased and possible reasons for this were investigated and are discussed. These included the effects of inadequate heat transfer from the liquid nitrogen refrigerant to the cryopump, a poor thermal conductivity of the cryodeposit, and an impurity, nitrogen gas, in the water vapour.     

A study on the interface and bulk charge density of AlN films with sputtering pressure

An attempt to correlate deposition-induced effects and the morphological properties with the electrical properties of the aluminum nitride (AlN) films have been made. The AlN film was sputter deposited on silicon while increasing the pressure in steps from 2×10⁻³ to 8×10⁻³ mbar. An X-ray diffractogram revealed that the intensity of (0 0 2) orientation increased till 6×10⁻³ mbar pressure, but it changed to (1 0 0) orientation of the AlN film at 8×10⁻³ mbar. The FTIR spectra of the absorption band of the films were observed around 682 cm⁻¹ and became prominent at 6×10⁻³ mbar. A decrease in the grain size was seen by SEM images at 8×10⁻³ mbar. The AFM measurements revealed that the surface roughness varied from 1.56 to 3.24 nm with pressure. It was found that the insulator charge density (Q_in) increased from 1.4×10¹¹ cm⁻² to 1.3×10¹² cm⁻² with increase in pressure. On the other hand, the interface state density (D_it) was found minimum (7.3×10¹¹ eV⁻¹ cm⁻²) at 6×10⁻³ mbar. It is found that presence of the Q_in and D_it are primarily governed by the sputtering pressure of the AlN film.     

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.     

Thermal stability of the Mobil Five type metallosilicate molecular sieves—An in situ high temperature X-ray diffraction study

We have carried out in situ high temperature X-ray diffraction (HTXRD) studies of silicalite-1 (S-1) and metallosilicate molecular sieves containing iron, titanium and zirconium having Mobil Five (MFI) structure (iron silicalite-1 (FeS-1), titanium silicalite-1 (TS-1) and zirconium silicalite-1 (ZrS-1), respectively) in order to study the thermal stability of these materials. Isomorphous substitution of Si⁴⁺ by metal atoms is confirmed by the expansion of unit cell volume by X-ray diffraction (XRD) and the presence of Si-O-M stretching band at ∼960 cm⁻¹ by Fourier transform infrared (FTIR) spectroscopy. Appearance of cristobalite phase is seen at 1023 and 1173 K in S-1 and FeS-1 samples. While the samples S-1 and FeS-1 decompose completely to cristobalite at 1173 and 1323 K, respectively, the other two samples are thermally stable upto 1623 K. This transformation is irreversible. Although all materials show a negative lattice thermal expansion, their lattice thermal expansion coefficients vary. The thermal expansion behavior in all samples is anisotropic with relative strength of contraction along ‘a’ axes is more than along ‘b’ and ‘c’ axes in S-1, TS-1, ZrS-1 and vice versa in FeS-1. Lattice thermal expansion coefficients (α_v) in the temperature range 298-1023 K were −6.75 × 10⁻⁶ K⁻¹ for S-1, −12.91 × 10⁻⁶ K⁻¹ for FeS-1, −16.02 × 10⁻⁶ K⁻¹ for TS-1 and −17.92 × 10⁻⁶ K⁻¹ for ZrS-1. The highest lattice thermal expansion coefficients (α_v) obtained were −11.53 × 10⁻⁶ K⁻¹ for FeS-1 in temperature range 298-1173 K, −20.86 × 10⁻⁶ K⁻¹ for TS-1 and −25.54 × 10⁻⁶ K⁻¹ for ZrS-1, respectively, in the temperature range 298-1623 K. Tetravalent cation substitution for Si⁴⁺ in the lattice leads to a high thermal stability as compared to substitution by trivalent cations.     

8. A specimen-exchange device for an ultra-high vacuum atom-probe field-ion microscope

A specimen-exchange device is described for an ultra-high vacuum field-ion microscope (FIM). This device completely eliminates the long pump-down period that is required if the FIM chamber is brought back to atmospheric pressure. The pressure in an air-lock is reduced to 10^?6 torr before the exchange takes place and the pressure in the FIM chamber remains below 10^?7 torr during the exchange and it drops to less than 3 × 10^?9 torr within 15 min after the exchange.     

Influence of Mn-site doped with Ru on the high-temperature thermoelectric performance of CaMnO3−δ

Thermoelectric properties were measured from room temperature to 1000 K to study the effects of doping of Ru for Mn-site on the thermoelectric performance of CaMnO_3−δ. The electrical resistivity shows a sharp decrease upon Ru doping. The Seebeck coefficients of all the samples are negative, and their absolute values remain fairly large even after Ru doping. Among the samples of CaMn_1−xRu_xO_3−δ (x=0.02, 0.04, 0.06, 0.08, 0.10, 0.12, 0.15, 0.18), CaMn_0.96Ru_0.04O_3−δ has the largest power factor, 1.85×10⁻⁴ W/mK² at 1000 K. An increase or a decrease of x value results in a marked decrease of the power factor. The thermal conductivity and the figure of merit Z of CaMn_0.96Ru_0.04O_3−δ is 2.88 W/mK and 0.64×10⁻⁴ K⁻¹ at 1000 K, respectively.     

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.     

Influence of tetramethylammonium hydroxide treatment on the electrical characteristics of Ni/Au/GaN Schottky barrier diode

The effect of tetramethylammonium hydroxide (TMAH) treatment on the electrical properties of Ni/Au/GaN Schottky diodes have been investigated by current–voltage (I–V) and capacitance–voltage (C–V) techniques. The barrier heights and ideality factors measured from I–V characteristics are found to be 0.70 eV and 1.32 for without TMAH treatment, and 0.78 eV and 1.14 for with TMAH treatment, respectively. Cheung method is used to measure the series resistance and barrier height of the Schottky diodes, and the barrier height consistency is checked using the Norde method. The magnitude of interface state density for the diodes without and with TMAH treatment are varied from 7.45 × 10¹³ eV⁻¹ cm⁻² to 6.09 × 10¹² eV⁻¹ cm⁻² and 4.03 × 10¹³ eV⁻¹ cm⁻² to 1.79 × 10¹² eV⁻¹ cm⁻² in the below the conduction band from E_C-0.19 eV to E_C-0.63 eV and E_C-0.22 eV to E_C-0.73 eV. Based on the results, the TMAH treatment effectively removes of surface oxide (Ga_xO_y) layer, formed due to the incorporation of the residual oxygen with Ga atom at the GaN surface during the plasma etching. The decrease in interface state density at the Ni/Au/GaN interface could be the reason for the improvement in the electrical properties.     

Structural and electrical properties of chromium and nickel films evaporated in the presence of oxygen

Electron-optical investigations of Cr films evaporated in the presence of oxygen (1 × 10^-7 to 5 × 10^-7 torr) have shown that the negative temperature coefficient of resistivity (TCR) is caused by small amounts of an amorphous oxide. On annealing these films in a vacuum of better than 5 × 10^-9 torr (e.g. for 140 h at 395°C) the amorphous phase crystallized and could be identified as Cr₂O₃. When Ni is evaporated in the presence of oxygen the TCR changes from positive to negative values at about 5 × 10^-5 torr. Since the negative TCR of oxygen-doped Cr-Ni (60/40) films did not change after annealing these films in a hydrogen atmosphere at 300°C (reduction of Ni oxide) it becomes plausible that the negative TCR of the Cr-Ni films, too, is caused by an amorphous Cr oxide surrounding the metal crystals.     

The determination of interface state energy distribution of the H-terminated Zn/p-type Si Schottky diodes with high series resistance by the admittance spectroscopy

Analysis of Zn/p-Si Schottky diodes (SDs) with high resistivity has been given by admittance spectroscopy. The importance of the series resistance in the determination of energy distribution of interface states and especially their relaxation time in the SDs with high resistivity has been considered. The effect of the series resistance on capacitance-conductance/frequency characteristics has been given by comparing experimental data with theoretical data. The interface state density N_ss from the admittance spectroscopy ranges from 1.0×10¹² cm⁻² eV⁻¹ in 0.720-E_v eV to 2.03×10¹² cm⁻² eV⁻¹ in 0.420-E_v eV. Furthermore, the relaxation time ranges from 4.20×10⁻⁵ s in (0.420-E_v) eV to 3.20×10⁻⁴ s in (0.720-E_v) eV. It has been seen that the interface state density has a very small distribution range (1.0-2.03×10¹² cm⁻² eV⁻¹) that is ascribed to the predominant termination with hydrogen of the silicon surface after HF treatment.     

SrSn1−xFexO3−δ (0≤x≤1) perovskites: a novel mixed oxide ion and electronic conductor

The electrical conductivity of SrSn_1−xFe_xO_3−δ increases with the Fe content and reaches a value of ∼10⁻¹ S/cm at 25°C at x=1. Compounds with low Fe content exhibit both ionic and electronic conductivity, while the higher Fe content perovskites are mainly electronic conductors with a conductivity independent of the oxygen partial pressure over a wide range from 0.21 to 10⁻²² atm.     

XAFS and CEMS study of dilute magneto-optical semiconductor, Fe doped TiO2 films

TiO₂ films doped with 6% Fe were prepared by pulsed laser deposition (PLD) under different oxygen pressures, and characterized by X-ray absorption fine spectra (XAFS) and conversion electron Mössbauer spectra (CEMS). The edge energy and spectrum profiles of Fe- and Ti K X-ray absorption showed only Fe³⁺ and Ti⁴⁺ states for rutile TiO₂ films prepared under 10^− 1 Torr, the metallic Fe and Ti⁴⁺ for rutile TiO₂ films prepared in 10^− 6 Torr, and the metallic Fe and the average valance of less than “4+” for Ti in Ti_nO_2n−x films prepared by the PLD under 10^− 8 Torr. The metallic Fe clusters are also found in the TEM images of Ti_nO_2n−x film. Magnetic property of Fe doped TiO₂ films prepared by PLD at high vacuum (10^− 6 and 10^− 8 Torr) is considered to originate mainly from the magnetic metal iron clusters.     

High temperature thermoelectric properties of (Ca, Ce)4Mn3O10

Thermoelectric (TE) properties such as resistivity (ρ), Seebeck coefficient (S), and thermal conductivity (κ) of Ca_4−3xCe_3xMn₃O₁₀ (0<x≤0.03) polycrystalline samples were measured from room temperature to 1000 K. ρ shows an obvious decrease with the increment of Ce content. The hopping conduction mechanism is used to explain the conduction behavior of these samples. The negative S values indicate that these materials are n-type. The sample of x=0.03 has the largest power factor, 0.52×10⁻⁴ Wm⁻¹ K⁻² at 1000 K. The value of κ and the dimensionless figure of merit of this sample is 1.51 Wm⁻¹ K⁻¹ and 0.034 at 1000 K, respectively.     

Effect of an organic compound (Methyl Red) interfacial layer on the calculation of characteristic parameters of an Al/Methyl Red/p-Si sandwich Schottky barrier diode

An Al/Methyl Red/p-Si sandwich Schottky barrier diode (SBD) has been fabricated by adding a solution of the organic compound Methyl Red in chloroform onto a p-Si substrate, and then evaporating the solvent. Current-voltage (I-V) measurements of the Al/Methyl Red/p-Si sandwich SBD have been carried out at room temperature and in the dark. The Al/Methyl Red/p-Si sandwich SBD demonstrated rectifying behavior. Barrier height (BH) and ideality factor values of 0.855 eV and 1.19, respectively, for this device have been determined from the forward-bias I-V characteristics. The Al/Methyl Red/p-Si sandwich SBD showed non-ideal I-V behavior with the value of ideality factor greater than unity. The energy distribution of the interface state density determined from I-V characteristics increases exponentially with bias from 3.68 × 10¹² cm^− 2 eV^− 1 at (0.81 − E_v) eV to 9.99 × 10¹³ cm^− 2 eV^− 1 at (0.69 − E_v) eV.     

Structural, optical, and nonlinear optical absorption/refraction studies of the manganese nanoparticles prepared by laser ablation in ethanol

The structural, optical, and nonlinear optical properties of the manganese nanoparticles prepared by laser ablation in various liquids were investigated using the 532 and 1064 nm, 50 ps laser pulses. The TEM and spectral measurements showed temporal dynamics of size distribution of Mn nanoparticles in solutions. The nonlinear absorption (β = 2 × 10⁻¹⁰ and 4 × 10⁻¹¹ cm W⁻¹) and positive nonlinear refraction (γ = 8 × 10⁻¹⁵ and 2 × 10⁻¹⁴ cm² W⁻¹) of picosecond radiation were observed in the Mn colloidal suspensions using the 1064 and 532 nm radiation, respectively     

Synthesis of three dimensional photoluminescent [In10S20 − xSex] supertetrahedral clusters: (x < 0.3)

Two strong solid state luminescence peaks, centered at 457 nm and 538 nm, were observed from the newly synthesized ternary [In₁₀S_20 − xSe_x]¹⁰⁻ T3 clusters, under excitation by UV radiation (λ = 360 nm). The 457 nm peak is due to the porosity property of T3 clusters. Nevertheless, the 538 nm peak has not been reported for the T3 clusters before. In this letter, we demonstrate that the 538 nm peak is attributed to the trace Se atoms confined in the [In₁₀S_20 − xSe_x]¹⁰⁻ clusters. The luminescent output from the ternary [In₁₀S_20 − xSe_x]¹⁰⁻ T3 clusters is independent of temperature from 298 K until 77 K.