Observation of triangular terraces and triangular craters of CaF2 film on Si(1 1 1) substrate

We have investigated the growth mode and surface morphology of CaF₂ film on Si(1 1 1)7×7 substrate by reflection high-energy electron diffraction (RHEED) using very weak electron beam and atomic force microscopy (AFM). It was found by RHEED intensity oscillation measurements and AFM observations that three-dimensional (3D) islands grow at RT; however, rather flat surface appears with two-dimensional (2D) islands around 300 °C. Especially, at high temperature of 700 °C, characteristic equilateral triangular terraces (or islands) with flat and wide shape grow with the tops directed toward [1 1 −2] of substrate Si(1 1 1). On the other hand, the desorption process of the CaF₂ film due to electron stimulated desorption (ESD) was also examined. It was found that the ESD process at 300 °C forms characteristic equilateral triangular craters on the film surface with the tops (or corners) directed toward [−1 −1 2] of substrate Si(1 1 1), provided that the film was grown at 700 °C.     

Elemental steps in the growth of thin β-Ga2O3 films on CoGa(1 0 0)

The oxidation of CoGa(1 0 0) at 700 K was studied by means of high resolution electron energy loss spectroscopy (EELS), scanning tunneling microscopy, low energy electron diffraction and Auger electron spectroscopy (AES). At 700 K, thin well-ordered β-Ga₂O₃ films grow on CoGa(1 0 0). The EEL spectrum of the Ga-oxide films exhibit Fuchs–Kliewer phonons at 305, 455, 645, and 785 cm⁻¹. For low oxygen exposure (<0.2 L), the growth of oxide-islands starts at step edges and on defects. The oxide films have the shape of long, rectangular islands and are oriented in the [1 0 0] and [0 1 0] directions of the substrate. For higher oxygen exposure, islands of β-Ga₂O₃ are found also on the terraces. After an exposure of 200 L O₂ at 700 K, the CoGa(1 0 0) surface is homogeneously covered with a thin film of β-Ga₂O₃.     

High-resolution electron microscopy study of Ni81Fe19 film with Co33Cr67 buffer layer

The anisotropic magnetoresistance (AMR) in permalloy Ni₈₁Fe₁₉ film deposited on a 1.2 nm Co₃₃Cr₆₇ buffer layer was significantly enhanced. The high-resolution electron microscopy was used to study the microstructure of Ni₈₁Fe₁₉ film with and without Co₃₃Cr₆₇ buffer layer. It was found that Co₃₃Cr₆₇ buffer layer can induce good (1 1 1) texture, while without Co₃₃Cr₆₇ buffer layer, Ni₈₁Fe₁₉ film show randomly oriented grain structure. The Δρ/ρ enhancement is attributed to the decrease in the resistivity ρ of the Ni₈₁Fe₁₉ film due to the formation of the large (1 1 1) textured grains in Ni₈₁Fe₁₉ film with Co₃₃Cr₆₇ buffer layer. However, the surface roughness of substrate may limit the (1 1 1) textured grain size and induce additional grain boundaries in Ni₈₁Fe₁₉ film with Co₃₃Cr₆₇ buffer layer, limit the enhancement of the AMR effect.     

Auger electron spectroscopy and electron energy loss spectroscopy studies on carbonization of Si(100) and (111) surfaces with ethylene

The reactions of Si(100) and Si(111) surfaces at 700 °C (973 K) with ethylene (C₂H₄) at a pressure of 1.3×10⁻⁴ Pa for various periods of time were studied by using Auger electron spectroscopy (AES) and electron energy loss spectroscopy (ELS). For a C₂H₄ exposure level, the amount of C on the (111) surface was larger than that on the (100) surface. The formation of β-SiC grain was deduced by comparing the C_KLL spectra from the sample subjected to various C₂H₄ exposure levels, and from β-SiC crystal.     

Growth of β-MnO2 films on TiO2(110) by oxygen plasma assisted molecular beam epitaxy

We have used oxygen plasma assisted MBE to grow epitaxial films of pyrolusite (β-MnO₂) on TiO₂(110) for thicknesses of one to six bilayers (BL). We define a bilayer to be a layer of Mn and lattice O and an adjacent layer of bridging O within the rutile structure. The resulting surfaces have been characterized in situ by reflection high-energy electron diffraction, low-energy electron diffraction, X-ray photoelectron spectroscopy and diffraction, and atomic force microscopy. Well-ordered, pseudomorphic overlayers form for substrate temperatures between 400 and 500°C. Mn–Ti intermixing occurs over the time scale of film growth (1 BL/min) for substrate temperatures in excess of 500°C. Films grown at 400–500°C exhibit island growth, whereas intermixed films grown at temperatures of 500–600°C are more laminar. 1 BL films grown at 450°C are more laminar than multilayer films grown at the same temperature, and form a well-ordered surface cation layer of Mn on the rutile structure with at most 10% indiffusion to the second cation layer.     

A study on the reaction between chlorine trifluoride gas and glass-like carbon

The reaction between glass-like carbon (GC) and chlorine trifluoride (ClF₃) gas was investigated with weight measurements, surface analysis, and gas desorption measurements, where the ClF₃ gas is used for the in situ cleaning of tubes in silicon-related fabrication equipment. From Auger electron spectroscopy and X-ray photoelectron spectroscopy measurements, a carbon mono-fluoride, –(CF)_n–, film near the surface of GC is considered to be grown onto the GC surface above 400 °C by the chemical reaction with ClF₃, and this thickness of the fluoride film depends on the temperature. The grown fluoride film desorbs by annealing in a vacuum up to 600 °C. Although GC is apparently etched by ClF₃ over 600 °C, the etch rate of GC is much lower than that of SiC and quartz.     

LEED structure determination of the Ni(1 1 1)(√3×√3)R30°-Sn surface

Quantitative low energy electron diffraction has been used to determine the structure of the Ni(1 1 1)(√3×√3)R30°-Sn surface phase. The results confirm that the surface layer comprises a substitutional alloy of composition Ni₂Sn as previously found by low energy ion scattering (LEIS), and also shows that there is no stacking fault at the substrate/alloy interface as has been found in (√3×√3)R30°-Sb surface alloys on Ag and Cu(1 1 1). The surface alloy layer is rumpled with the Sn atoms 0.45 ± 0.03 Å higher above the substrate than the surrounding Ni atoms. This rumpling amplitude is almost identical to that previously reported on the basis of the LEIS study. Comparison with similar results for Sn-induced surface alloy phases on Ni(1 0 0) and Ni(1 1 0) shows a clear trend to reduced rumpling with reduced surface atomic layer density, an effect which can be rationalised in terms of the different effects of valence electron charge smoothing at the surface.     

Surface deformation phenomena induced by electron-beam irradiation in strained InGaAs/AlGaAs layers on GaAs (1 0 0) and (3 1 1)B substrates

The strained InGaAs/AlGaAs layer structures have been grown on GaAs ( 10 0) and (3 1 1)B substrates in a horizontal low-pressure metalorganic vapor-phase epitaxy system at a temperature of 800°C. In the surface observation using a high-resolution scanning electron microscope, we have found that surface deformation phenomena induced by electron-beam irradiation in strained In_0.36Ga_0.64As,/Al_0.3Ga_0.7As layers on GaAs (1 0 0) and (3 1 1)B substrates. The change of the surface morphology was observed in real time on the display of SEM with the accelerating voltage of 30 kV and the irradiated time of 60–120 s. The surface deformation through mass transport seems to be the cause of the residual strain relaxation due to electron-beam irradiation.     

Structural comparison of gadolinium and lanthanum silicate films on Si(1 0 0) by HRTEM, EELS and SAED

High-resolution transmission electron microscopy (HRTEM), electron energy loss spectroscopy (EELS) and selected area electron diffraction (SAED) were used to study gadolinium and lanthanum silicate films deposited on Si(1 0 0) substrates using electron-beam evaporation from pressed-powder targets. As-deposited films consist of an amorphous silicate layer without an interfacial layer. After annealing at 900 °C in oxygen for 2 min, an interfacial SiO₂ layer is formed in the gadolinium silicate film, while this interfacial layer is a SiO₂-rich lanthanum silicate layer in the lanthanum silicate film. The formation of interfacial silicate layers is thermodynamically more favorable for the lanthanum films than for the gadolinium films. The gadolinium silicate films crystallize at a temperature between 1000 and 1050 °C, while the crystallization temperature for the lanthanum silicate films is between 900 and 950 °C.     

RF-sputtered CrB2 diffusion barrier for Ni/Au Ohmic contacts on p-CuCrO2

Ohmic contacts to p-type CuCrO₂ using Ni/Au/CrB₂/Ti/Au contact metallurgy are reported. The samples were annealed in the 200–700 °C range for 60 s in flowing oxygen ambient. A minimum specific contact resistance of 2 × 10⁻⁵ Ω cm² was obtained after annealing at 400 °C. Further increase in the annealing temperature (>400 °C) resulted in the degradation of contact resistance. Auger Electron Spectroscopy (AES) depth profiling showed that out-diffusion of Ti to the surface of the contact stacks was evident by 400 °C, followed by Cr at higher temperature. The CrB₂ diffusion barrier decreases the specific contact resistance by almost two orders of magnitude relative to Ni/Au alone.     

Enhanced magnetic properties of Nd–Fe–B thin films crystallized by heat treatment

Nd₂Fe₁₄B Φ phase crystallites were formed in Nd_16.7Fe_65.5B_17.8 thin films prepared by RF sputtering with subsequent heat treatment. The 2 μm-thick films were deposited onto 0.1 mm Mo sheets at an average substrate temperature (T_s) of 365°C. The enhanced magnetic properties of the magnetically anisotropic thin films were investigated using different heating rates (h_r) of 10°C, 20°C, 50°C and 100°C/min in an annealing experiment. Transformation from the amorphous phase to the crystalline phase is clearly manifested by the formation of fine crystallites embedded as a columnar matrix of Nd₂Fe₁₄B phase. High-resolution scanning electron microscope data of the cross-section of the annealed films show columnar stacking of Nd₂Fe₁₄B crystallites with sizes <500 nm. Transmission electron microscope observations revealed that the microstructure of these films having out-of-plane magnetization consists of uniformly distributed Φ phase with grain size around 400 nm together with small Nd rich particles. This grain size of Φ phase is comparable to the single domain particle diameter of Nd₂Fe₁₄B. Significant change in _iH_c, 4πM_r and 4πM_s with h_r was confirmed. Annealing conditions with a heating rate of 50°C/min to an annealing temperature (T_a) of 650°C for 30 min was consequently found to give optimum properties for the NdFeB thin films. The resulting magnetic properties, considered to be the effect of varying h_r were _iH_c= 1307–1357 kA/m, 4πM_r=0.78–1.06 T and 4πM_s=0.81–1.07 T.     

Electrode contact study for SiGe thin film operated at high temperature

A study on the electrode contact of the sputtered SiGe thin film is reported for application of devices working at high temperature. Surface morphological characterization with optical microscope and AFM (atomic force microscope) together with the electrical characterization by TLM measurements (transmission line method) were performed before and after aging at 500 °C for 24 h using various sputtered multilayer electrodes, Ti/Au/Ti, Ta/Pt/Ta and Ti/Pt/Ti, on 300-nm B-doped SiGe thin film deposited by magnetron sputtering and furnace crystallisation at high temperature. After aging at 500 °C for 24 h, the Ti/Au/Ti multilayer electrodes seriously degraded to be non-ohmic contact, showing rough surface morphology. The Ti/Pt/Ti metal layers showed the lowest specific contact, resistivity before and after aging, 1.46 × 10⁻³ Ω cm² and 1.68 × 10² Ω cm² respectively.     

Superconducting Nd1.85Ce0.15CuO4 films grown by the pulsed electron deposition technique

Nd_1.85Ce_0.15CuO_4−δ superconducting thin films were prepared on (1 0 0) SrTiO₃ substrates by pulsed electron deposition technique without reducing atmosphere. Oxygen content is finely controlled by high temperature vacuum annealing, and optimal superconductivity has been obtained. The deposition conditions of the film are discussed in details. Higher deposition temperature and lower gas pressure result in the loss of copper and the appearance of the foreign phase Ce_0.5Nd_0.5O_1.75. High quality Nd_1.85Ce_0.15CuO_4−δ epitaxial films are deposited at 840–870 °C in the mixed gas with a ratio of O₂:Ar = 1:3.     

Hydroxyapatite coating on porous silicon substrate obtained by precipitation process

Hydroxyapatite Ca₁₀(PO₄)₆(OH)₂ (HAP) is known as a bioactive and biocompatible material, HAP coatings were used to improve the biocompatible of substrate by many researcher, In this work, HAP thin films on porous silicon (PS) substrates have been prepared by aqueous precipitation method with rapid thermal annealing (RTA) processes. The HAP films had been prepared under the annealing temperature ranging from 300 to 1000 °C. By the measurement of X-ray diffraction (XRD), it was found that for the crystallinity optimization, the heat-treatment at 850–950 °C for 1 h would be favorable. Atomic force microscopy (AFM) and scanning electron microscope (SEM) measurements reveal a dense and smooth surface of the HAP film, and tightly adherence of the coating on porous silicon substrate after sintered. Thus, by this method, porous silicon could be increased its bioactivity and so that could be used in the biomedical area.     

Synthesis and physical behaviour of In2S3 films

In₂S₃ layers have been grown by close-spaced evaporation of pre-synthesized In₂S₃ powder from its constituent elements. The layers were deposited on glass substrates at temperatures in the range, 200–350 °C. The effect of substrate temperature on composition, structure, morphology, electrical and optical properties of the as-grown indium sulfide films has been studied. The synthesized powder exhibited cubic structure with a grain size of 63.92 nm and S/In ratio of 1.01. The films grown at 200 °C were amorphous in nature while its crystallinity increased with the increase of substrate temperature to 300 °C. The films exhibited pure tetragonal β-In₂S₃ phase at the substrate temperature of 350 °C. The surface morphological analysis revealed that the films grown at 300 °C had an average roughness of 1.43 nm. These films showed a S/In ratio of 0.98 and a lower electrical resistivity of 1.28 × 10³ Ω cm. The optical band gap was found to be direct and the layers grown at 300 °C showed a higher optical transmittance of 78% and an energy band gap of 2.49 eV.     

Preparation of tantalum oxide thin films by photo-assisted atomic layer deposition

Tantalum oxide thin films were prepared by photo-assisted atomic layer deposition (Photo-ALD) in the substrate temperature range of 170–400 °C using Ta(OC₂H₅)₅ and H₂O as precursors. The constant growth rates of 0.42 and 0.47 Å per cycle were achieved for the films grown by normal ALD and Photo-ALD, respectively. The increased growth rate in Photo-ALD is probably due to the reactive surface by photon energy and faster surface reaction. In Photo-ALD, however, the constant growth rate started at lower temperature of 30 °C and one cycle time shortened up to 5.7 s than that of normal ALD. The films grown by normal ALD and Photo-ALD were amorphous and very smooth (0.21–0.35 nm) as examined by X-ray diffractometer and atomic force microscopy, respectively. Also, the refractive index was found to be 2.12–2.16 at the substrate temperature of 190–300 °C, similar to that of the film grown by normal ALD. However, the remarkably low leakage current density of 0.6×10⁻⁶ A/cm² to 1×10⁻⁶ A/cm² at applied field of 1 MV/cm is several order of magnitude smaller than that of normal ALD, probably due to the presence of reactive atom species.     

The effect of a nitrogen-rich surface layer on the sub-surface deuterium (hydrogen) concentration distribution in titanium

Deuterium and nitrogen depth profiles in Ti with modified surfaces have been measured with Auger electron spectroscopy, secondary ion mass spectroscopy, and D(³He,p)⁴He nuclear reaction analysis. Nitrogen-rich surfaces layers of varying thicknesses were created on Ti by exposure to N₂ gas at 650°C. Deuterium loading was performed by exposure to 1 Torr of D₂ gas at 500°C. The deuterium distribution was influenced by nitrogen in the near-surface regions of all samples. Specifically, deuterium solubility was suppressed in surface regions of high (greater than 1%) nitrogen concentration. The deuterium solubility also remained low within the first few microns, well beyond the region of high nitrogen concentration. This effect is attributed to internal elastic stresses imposed by the non-deuterium absorbing nitrogen-rich layer on the Ti. These stresses prohibit the volume expansion associated with deuterium absorption. We estimate stresses on the order of 3–4 GPa are required to suppress the deuterium solubility to the values observed. The deuterium absorption kinetics were observed to depend systematically on the thickness of the nitrogen-rich layer. This is consistent with limited solubility near the surface or a surface poisoning effect influencing the overall deuterium diffusion from the gas phase into the Ti bulk.     

Increased surface roughness by oxygen plasma treatment of graphite/polymer composite

The technology of selective plasma etching was applied to increase the surface roughness of graphite/polymer composite. Etching was performed with a low pressure weakly ionised oxygen plasma created with a RF generator of the output power of 200 W and frequency of 27.12 MHz. The density of charged particles, density of neutral oxygen atoms and the electron temperature was about 1×10¹⁶ m⁻³, 4×10²¹ m⁻³, and 5 eV, respectively. The effects of plasma treatment were observed by scanning electron microscope (SEM), electron microprobe (EMPA) and Talysurf. It was found that the surface roughness was increased by approximately 15 times, from a virgin sample at the roughness of R_a=0.27 μm to a very rough surface with R_a=4 μm. The roughness increased with increasing plasma exposure time. The EMPA results showed that the amount of sulphur in the surface layer decreased with increasing etching time indicating that PPS polymer was the material etched preferentially.     

The effect of annealing on the MR and exchange bias characteristics in dual spin valve with nano-oxide layer

We investigated magnetoresistance (MR) and exchange bias properties by annealing in the dual spin valve (SV) with nano-oxide layer (NOL). By analyzing effects of NOL in top and bottom pinned simple SVs, MR enhancement effect of NOL inserted in the bottom pinned layer was higher than that of NOL in the top pinned layer with annealing. By the enhanced specular scattering of electrons by NOL, the MR ratio of dual SV with NOL was increased to 15.5–15.9% with an annealing of 200–250°C. Exchange coupling constant J_ex was improved rapidly as 0.13–0.16 erg/cm² by annealing in the bottom pinned layer, whereas the effect of annealing was not large in the top pinned layer with J_ex of about 0.09–0.116 erg/cm².     

Effect of annealing temperature on microstructure of chemically deposited calcium modified lead titanate thin films

Thin ferroelectric films of calcium modified lead titanate Pb_1−xCa_xTiO₃(PCT) have been prepared by chemical deposition process. The as deposited amorphous films were thermally treated for crystallization and formation of perovskite structure. Characterization of these films by X-ray diffraction (XRD) have been carried out for various amounts of calcium (Ca)-doping (0.20, 0.24, and 0.28) on indium tin oxide (ITO) coated corning glass substrates. For a better understanding of the crystallization mechanism, the investigations were carried out at various annealing temperatures (450, 550, and 650 °C). Characterization of these films by XRD shows that the films exhibit tetragonal phase with perovskite structure. Atomic force microscope images (AFM) are characterized by slight surface roughness with a uniform crack-free, densely-packed structure. Also, Fourier transform infrared spectra (FT-IR) of the as deposited film and annealed thin films (x=0.24) at 650 °C on silicon (Si) substrates were taken to get more information about the film formation. Dielectric studies of the films were carried out and reported.