An experimental investigation of the effect of biaxial loading on the master curve transition temperature in RPV steels

During the 1990s considerable work was conducted to characterize the effect of biaxial loading on the ductile to brittle transition temperature. The work centered on a series of tests using large cruciform bend specimens from an experimental A533B test plate denoted as HSST Plate 14 (Heavy Section Steel Technology Plate 14). Recently a series of similar biaxial cruciform tests has been conducted on the steel used for an extensive European Round Robin that investigated the ductile-to-brittle transition master curve and associated T₀ reference temperature. The results of these tests have been used to promote the concept of a “Biaxial Effect” which corresponds to a shift in the shallow crack transition master curve of +20 °C or more when biaxial stresses are present, in comparison with the master curve for uniaxially loaded shallow crack specimens. A comprehensive analysis of the all of the available HSST Plate 14 data and data from two other structural steels was performed to investigate the extent of a biaxial effect on the reference temperature, T₀. The analysis included many additional biaxial cruciform test results on three different materials. The results of all three materials discussed in this paper fail to clearly demonstrate that biaxial loading, imposed through the use of a cruciform specimen geometry, has an effect on the fracture toughness, characterized using a master curve approach and reference temperature T₀. The analysis utilized in this paper assumes that the toughness distribution and temperature dependence of shallow cracked specimens can be modeled by using the master curve approach. This assumption has not been rigorously validated and would benefit from further study. Additional detailed stress analysis of the constraint evolution in the cruciform specimens may better define the precise conditions under which a biaxial effect on the fracture toughness could be realized.     

Synthesis and mechanical properties of high-purity Cr2AlC ceramic

High-purity and dense Cr₂AlC has been successfully fabricated by hot-pressing, using Cr, Al and graphite as raw materials. Delamination, kink bands, monolamellar kink, transgranular crack and transgranular fracture of bulk Cr₂AlC are found during the room-temperature test. The density, Vickers hardness, flexural strength, Young's modulus, compressive strength and fracture toughness of the Cr₂AlC are 5.17 g/cm³, 4.9 GPa, 469 ± 27 MPa, 282 GPa, 949 ± 22 MPa and 6.22 ± 0.26 MPa m^1/2, respectively. The strength of Cr₂AlC could be greatly improved by second phase of Cr₇C₃. And the slipping of basal planes and slip system cold be hindered by Cr₇C₃, thus resulting in a lower toughness.     

Diffusion of Pb in carbon ion-implanted silicon: Discovery of a new crystalline phase after electron beam annealing

A novel phase has been discovered by dual low-energy ion implantation and high vacuum electron beam annealing. (100) p-type Si was implanted with (a) 20 keV ¹²C⁺ ions to the fluence of 6 × 10¹⁶ cm⁻² and (b) 7 keV Pb⁺ ions to the fluence of 4 × 10¹⁵ cm⁻². The ¹²C ion implantation results in an understoichiometric shallow SiC_x layer that intersects with the surface. The implanted Pb ions decorate a shallow subsurface region. High vacuum electron beam annealing at 1000 °C for 15 s using a temperature gradient of 5 °C s⁻¹ leads to the formation of large SiC nanocrystals on the surface with RBS measurements showing Pb has diffused into the deeper region affected by the ¹²C implantation. In this region, a new crystalline phase has been discovered by XRD measurements.     

Fracture behavior and mechanism of 2D C/SiC-BCx composite at room temperature

2D C/SiC composite was modified with partial BC_x matrix by low pressure chemical vapor infiltration technique (LPCVI), which was named as 2D C/SiC-BC_x composite. The flexural fracture behavior, mechanism, and strength distribution of 2D C/SiC-BC_x composite are investigated. The results indicate that the flexural strength, fracture toughness, and fracture work are 442.1 MPa, 22.84 MPa m^1/2, and 19.2 kJ m⁻², respectively. The flexural strength of C/SiC-BC_x composite decrease about 20% than that of C/SiC composite. However, the fracture toughness and fracture work increase about 19% and 18.5%, respectively. The properties varieties between C/SiC-BC_x composite and C/SiC composite can be attributed to the weak-bonding interface between BC_x/SiC matrices according to the results of detailed microstructure analysis. The strength distribution of 2D C/SiC-BC_x composite follows as Normal distribution or Weibull distribution with σ_u = 0, and m = 8.1393. The mean value of flexural strength for 2D C/SiC-BC_x composite is 443 MPa obtained by theory calculation, which is consistent with experiment result (442.1 MPa) very well.     

Preparation and characterization of CuIn1 − xGaxSe2 − ySy thin film solar cells by rapid thermal processing

This paper describes the synthesis and characterization of CuIn_1 − xGa_xSe_2 − yS_y (CIGSeS) thin-film solar cells prepared by rapid thermal processing (RTP). An efficiency of 12.78% has been achieved on ~ 2 µm thick absorber. Materials characterization of these films was done by SEM, EDS, XRD, and AES. J-V curves were obtained at different temperatures. It was found that the open circuit voltage increases as temperature decreases while the short circuit current stays constant. Dependence of the open circuit voltage and fill factor on temperature has been estimated. Bandgap value calculated from the intercept of the linear extrapolation was 1.1-1.2 eV. Capacitance-voltage analysis gave a carrier density of 4.0 × 10¹⁵ cm^− 3.     

Crack arrest testing of high strength structural steels for naval applications

The crack arrest fracture toughness of two high strength steel alloys used in naval construction, HSLA-100, Composition 3 and HY-100, was characterized in this investigation. A greatly scaled-down version of the wide-plate crack arrest test was developed to characterize the crack arrest performance of these tough steel alloys in the upper region of the ductile-brittle transition. The specimen is a single edge-notched, 152 mm wide by 19 mm thick by 910 mm long plate subjected to a strong thermal gradient and a tensile loading. The thermal gradient is required to arrest the crack at temperatures high in the transition region, close to the expected service temperature for crack arrest applications in surface ships. Strain gages were placed along the crack path to obtain crack position and crack velocity data, and this data, along with the applied loading is combined in a “generation mode” analysis using finite element analysis to obtain a dynamic analysis of the crack arrest event. Detailed finite element analyses were conducted to understand the effect of various modeling assumptions on the results and to validate the methodology compared with more conventional crack arrest tests.Brittle cracks initiation, significant cleavage crack propagation and subsequent crack arrest was achieved in all 15 of the tests conducted in this investigation. A crack arrest master curve approach was used to characterize and compare the crack arrest fracture toughness. The HSLA-100, Comp. 3 steel alloy had superior performance to the HY-100 steel alloy. The crack arrest reference temperature was T_KIA = −136 °C for the HSLA-100 plate and T_KIA = −64 °C for the HY-100 plate.     

Structure and negative thermal expansion of Pb1 −xBixTiO3

Pb_1-xBi_xTiO₃ (x = 0.0-0.1) compounds were prepared to study the unique dopant effect of bismuth in PbTiO₃. Their thermal expansions and structures were investigated by high-temperature X-ray diffraction and X-ray Rietveld method. The results indicated that Bismuth substitution evidently weakened the tetragonality of PbTiO₃ solid solution, but increased the spontaneous polarization. Both the enhanced spontaneous polarization and the decreased tetragonality led to small volume shrinkage with temperature rising, where the average volumetric thermal expansion coefficient changed from − 1.99 × 10^− 5/°C for pure PbTiO₃ to − 0.56 × 10^− 5/°C for Pb_0.90Bi_0.10TiO₃. The Curie point of Pb_1 − xBi_xTiO₃ was slightly raised compared to PbTiO₃ and permitted one to use it in a wide temperature range.     

Structural, electrical and optical properties of transparent Zn1 − xMgxO nanocomposite thin films

Zn_1 − xMg_xO thin films of various Mg compositions were deposited on quartz substrates using inexpensive ultrasonic spray pyrolysis technique. The influence of varying Mg composition and substrate temperature on structural, electrical and optical properties of Zn_1 − xMg_xO films were systematically investigated. The structural transition from hexagonal to cubic phase has been observed for Mg content greater than 70 mol%. AFM images of the Zn_1 − xMg_xO films (x = 0.3) deposited at optimized substrate temperature clearly reveals the formation of nanorods of hexagonal Zn_1 − xMg_xO. The variation of the cation-anion bond length to Mg content shows that the lattice constant of the hexagonal Zn_1 − xMg_xO decreases with corresponding increase in Mg content, which result in structure gradually deviating from wurtzite structure. The tuning of the band gap was obtained from 3.58 to 6.16 eV with corresponding increase in Mg content. The photoluminescence results also revealed the shift in ultraviolet peak position towards the higher energy side.     

Composition dependent thermoelectric properties of sintered Mg2Si1−xGex (x = 0 to 1) initiated from a melt-grown polycrystalline source

Fabrication of Mg₂Si_1−xGe_x (x = 0-1.0) was carried out using a spark plasma sintering technique initiated from melt-grown polycrystalline Mg₂Si_1−xGe_x powder. The thermoelectric properties were evaluated from RT to 873 K. The power factor of Mg₂Si_1−xGe_x with higher Ge content (x = 0.6-1.0) tends to decrease at higher temperatures, and the maximum value of about 2.2 × 10^− 5 Wcm^− 1K^− 2 was observed at 420 K for Mg₂Si and Mg₂Si_0.6Ge_0.4. The coexistence of Si and Ge gave rise to a decrease in the thermal conductivity in the Mg₂Si_1−xGe_x. The values close to 0.02 Wcm^− 1K^− 1 were obtained for Mg₂Si_1−xGe_x (x = 0.4-0.6) over the temperature range from 573 to 773 K, with the minimum value being about 0.018 Wcm^− 1K^− 1 at 773 K for Mg₂Si_0.4Ge_0.6. The maximum dimensionless figure of merit was estimated to be 0.67 at 750 K for samples of Mg₂Si_0.6Ge_0.4.     

Influence of strontium substitution on the dielectric properties of Ca(1 − x)SrxTi0.9Zr0.1O3 solid solutions

A conventional solid-state reaction has been used to synthesize the perovskite Ca_(1 − x)Sr_xTi_(1 − y)Zr_yO₃ (y = 0.1). The aim of this study is focused on the development of new materials with complex perovskite structure and on their dielectric property improvement. The temperature and substitutional ratio effects on the different phase evolutions is investigated by X-ray diffraction (XRD) and scanning electron microscope observations. These ceramics sintered at 1500 °C, present a density higher than 95% and their dielectric properties are significantly affected by the substitution. The CaTiO₃ ceramic present a relative permittivity of 190 and the temperature coefficient of the permittivity of − 1828 ppm/C°. The substitution with zirconium (for x = 0 and y = 0.1: Σ = 145; |Σ = − 917 ppm/C°). Both permittivity and temperature coefficient values decrease; however, an opposite effect is observed when substituting with the strontium. With increasing an x value and maintaining a y value constant (y = 0.1), the dielectric constant increases and the temperature coefficient remains constant. Therefore, the dielectric properties of CaTiO₃ ceramics are improved with the combined substitution.     

Enhanced thermoelectric properties of NaCo2O4 by adding ZnO

The primary phase present in the as-sintered Na(Co_1 − xZn_x)₂O₄ (0 ≤ x ≤ 0.1) bodies was the solid solution of the constituent oxides with a bronze-type layered structure. The electrical conductivity of the Na(Co_1 − xZn_x)₂O₄ samples significantly increased with an increase in ZnO content. The sign of the Seebeck coefficient for all samples was positive over the whole temperature range (723-1073 K), i.e., p-type conduction. The power factor of Na(Co_0.95Zn_0.05)₂O₄ showed an outstanding power factor (1.7 × 10^− 3Wm^− 1 K^− 2) at 1073 K. The power factor was above four times superior to that of ZnO-free NaCo₂O₄ (0.4 × 10^− 3Wm^− 1 K^− 2). This originates from an unusually large Seebeck coefficient (415 μVK^− 1) accompanied with high conductivity (127Ω^− 1 cm^− 1) at 1073 K.     

Structure and thermal conductivity of Gd2(TixZr1 − x)2O7 ceramics

The Gd₂(Ti_xZr_1 − x)₂O₇ (x = 0, 0.25, 0.50, 0.75, 1.00) ceramics were synthesized by solid state reaction at 1650 °C for 10 h in air. The relative density and structure of Gd₂(Ti_xZr_1 − x)₂O₇ were analyzed by the Archimedes method and X-ray diffraction. The thermal diffusivity of Gd₂(Ti_xZr_1 − x)₂O₇ from room temperature to 1400 °C was measured by a laser-flash method. The Gd₂Zr₂O₇ has a defect fluorite-type structure; however, Gd₂(Ti_xZr_1 − x)₂O₇ (0.25 ≤ x ≤ 1.00) compositions exhibit an ordered pyrochlore-type structure. Gd₂Zr₂O₇ and Gd₂Ti₂O₇ are infinitely soluable. The thermal conductivity of Gd₂(Ti_xZr_1 − x)₂O₇ increases with increasing Ti content under identical temperature conditions. The thermal conductivity of Gd₂(Ti_xZr_1 − x)₂O₇ first decreases gradually with the increase of temperature below 1000 °C and then increases slightly above 1000 °C. The thermal conductivity of Gd₂(Ti_xZr_1 − x)₂O₇ is within the range of 1.33 to 2.86 W m^− 1 K^− 1 from room temperature to 1400 °C.     

Tuning the optical properties of alloyed CdSexS1 − x nanoparticles by changing the constituent stoichiometry

The spherical particles CdSe_xS_1 − x with 30-80 nm in radius have been successfully prepared by the hydrothermal reaction at 200 °C. The structure characterization which has been carried out using X-ray diffraction (XRD) shows hexagonal crystal structure. Novel properties have been observed via UV-visual absorption spectra and photoluminescence (PL) spectra. The absorption shoulder and the luminescence emission peaks have been tuned by changing the mole ratio of Se in the CdSe_xS_1 − x samples.     

Thermal and FTIR spectral characterization of diammonium tetrachloromanganate (II) monohydrate crystals

Crystals of the new compound, diammonium tetrachloromanganate (II) monohydrate, were grown by slow evaporation solution growth method at room temperature. The compound was characterized through thermogravimetric, low temperature differential scanning calorimetric methods and Fourier Transform infrared spectroscopy. The elemental analysis and the thermal studies confirm the stoichiometry of the compound. The thermal anomalies observed in differential scanning calorimetric curve at − 9.8 °C and − 20.4 °C in the cooling cycle indicate a first order transition. The phase transition is attributed to the gradual ordering of NH₄⁺ and MnCl₄²⁻ ions at low temperatures. The infrared spectrum of the compound characterizes the various chemical bonding and water molecules in the compound.     

Enhanced ferromagnetic properties of multiferroic BiCoxFe1 − xO3 synthesized by hydrothermal method

The BiCo_xFe_1 − xO₃ samples have been successfully synthesized by hydrothermal process. The resulting products were characterized by X-ray powder diffraction (XRD), energy dispersive X-ray (EDS), differential thermal analysis (DTA), and physical property measurement system (PPMS).It was found that the magnetization of the obtained products was greatly enhanced by Co substituting for Fe ions. Furthermore, the value of magnetism of BiCo_xFe_1 − xO₃ samples can be adjusted by Fe doping concentration. DTA curve indicates the ferroelectric properties of the obtained BCFO samples are not affected by Co substitution. Therefore, it would be interesting to realize thin films with similar compositions and study their properties in the interest of device applications.     

Characterization of N-doped TiO2 films prepared by reactive sputtering using air/Ar mixtures

Nitrogen-doped titanium dioxide (TiO_2 − xN_x) thin films desirable for visible light photocatalysts were prepared by reactive sputtering using air/Ar mixtures. Using air as the reactive gas allows the process to conduct at high base pressures (low vacuum), which reduces substantially the processing time. The obtained films transformed from mixed phases to anatase phase as the air/Ar flow ratio increased. Substitutional doping of nitrogen verified by X-ray photoelectron spectroscopy accounts for the red-shift of absorption edge in the absorption spectra. Anatase TiO_2 − xN_x films could incorporate up to about 7.5 at.% substitutional nitrogen and a maximum of 23 at.% nitrogen was determined in the films with mixed phases. The optical band gaps of the TiO_2 − xN_x films calculated from Tauc plots varied from 3.05 to 3.11 eV and those of the mixed phase ranged from 2.77 to 3.00 eV, which are all lower than that for pure anatase TiO₂ and fall into the visible light regime.     

Structural,optical and electrical properties of In4Sn3O12 films prepared by pulsed laser deposition

Highly conducting (σ ∼ 2.6 × 10³ Ω⁻¹ cm⁻¹) In₄Sn₃O₁₂ films have been deposited using pulsed laser deposition (PLD) on glass and quartz substrates held at temperatures between 350 and 550 °C under chamber pressures of between 2.5 and 15 mTorr O₂. The crystallinity and the surface roughness of the films were found to increase with increasing substrate temperature. Electron concentrations of the order of 5 × 10²⁰ cm⁻³ and mobilities as high as 30 cm² V⁻¹ s⁻¹ were determined from Hall effect measurements performed on the films. Fitting of the transmission spectral profiles in the ultra-violet–visible spectrum has allowed the determination of the refractive index and extinction coefficient for the films. A red-shift in the frequency of plasmon resonance is observed with both increasing substrate temperature and oxygen pressure. Effective masses have been derived from the plasma frequencies and have been found to increase with carrier concentration indicating a non-parabolic conduction band in the material In₄Sn₃O₁₂. The optical band-gap has been determined as 3.8 eV from the analysis of the absorption edge in the UV. These results highlight the potential of these films as lower In-content functional transparent conducting materials.     

Preparation of inorganic solid state thin film for electrochromic application

All oxide solid state ITO (indium tin oxide)/Li_yWO_3−x/Li_1−zMn₂O₄/ITO stacked structure was deposited on a silica glass substrate by pulsed laser deposition for its electrochromic application. The Li doped amorphous tungsten trioxide Li_yWO_3−x thin film prepared at room temperature and in oxygen pressure of 7 Pa got the color of blue due to the mixture valence state of tungsten. We found that the amorphous Li_1−zMn₂O₄ thin film was suitable for the electrochromic application in spite of the low ion conductivity along in-plane direction. The ITO electrode thin film deposited at room temperature showed the relatively high transmittance and the usable conductivity. The transmittance at a wavelength of 750 nm for the ITO/Li_yWO_3−x/Li_1−zMn₂O₄/ITO stacked film changed from 50% to 80% by the applied voltage, while the transmittance at around 450 nm did not change. The blue-colored electrochromic property could be observed for the all oxide solid state film.     

Regulate the content of magnesium in MgxZn1−xO films by vacuum anneal

Mg_xZn_1−xO thin films were grown on c-sapphire substrates by metal-organic chemical vapor deposition (MOCVD), followed by annealing in vacuum at different temperatures for 1 h. The UV emission peak was blue shifted in the photoluminescence (PL) spectra and a dramatic shift of (0 0 2) diffraction peak to higher angle was observed in X-ray diffraction (XRD) pattern with increasing anneal temperature. This suggested the band gap and the lattice parameter of Mg_xZn_1−xO had been affected by annealing in vacuum. Furthermore, the structure of the film became sparser due to annealing in vacuum. From the X-ray photoelectron spectroscopy (XPS) and ICP of the Mg_xZn_1−xO film, we can find that the anneal temperature have an effect on the content of each element in Mg_xZn_1−xO quantitatively. In addition, the value of x in Mg_xZn_1−xO varied slightly as the annealing temperature increased. The above phenomena indicated that annealing in vacuum could slightly adjust the percentage of Mg indirectly in Mg_xZn_1−xO film and offer a good idea in Mg_xZn_1−xO devices facture.