Influence of overcoat on laser-induced damage threshold of 532 and 800 nm TiO2/SiO2 high reflectors

TiO₂/SiO₂ high reflectors with and without a SiO₂ overcoat are deposited by electron-beam evaporation. The film properties are characterized by visible spectrometry measures, structure analysis, roughness and laser-induced damage threshold (LIDT) tests, surface defects and damage morphology observation. The effects of overcoats on LIDT at 532 nm, 8 ns and 800 nm, 220 ps laser pulses are investigated. The relations between film structure, roughness, surface defects, electric field and LIDT are discussed. It is found that overcoats can increase the LIDT at these two laser wavelengths. The reduction of peak temperature, the low defects density and roughness, the low intrinsic absorption of SiO₂ and its amorphous structure are the main reasons for LIDT improvement by overcoats.     

Influence of substoichiometer on the laser-induced damage characters of HfO2 thin films

HfO₂ is one of the most important high refractive index materials for depositing high power optical mirrors. In this research, HfO₂ thin films were prepared by dual-ion beam reactive sputtering method, and the laser-induced damage thresholds (LIDT) of the sample were measured in 1-on-1 mode for laser with 1064 nm wavelength. The results indicate that the LIDT of the as-grown sample is only 3.96 J/cm², but it is increased to 8.98 J/cm² after annealing under temperature of 200 °C in atmosphere. By measuring the laser weak absorption and SIMS of the samples, we deduced that substoichiometer is the main reason for the low LIDT of the as-grown sample, and the experiment results were well explained with the theory of electronic-avalanche ionization.     

Characterization of CuAlO2 thin film prepared by rapid thermal annealing of an Al2O3/Cu2O/sapphire structure

CuAlO₂ thin film was successfully prepared by rapid thermal annealing of an Al₂O₃/Cu₂O/sapphire structure in air above 1000 °C. The film was mostly with single crystalline structure as verified by X-ray diffraction methods. We found that crystal quality and electrical conductivity of the films were affected by the cooling rate after annealing. The highest conductivity obtained in this work was 0.57 S/cm. Optical gap of this film was determined to be 3.75 eV.     

High temperature annealing effect on structure, optical property and laser-induced damage threshold of Ta2O5 films

Ta₂O₅ films were deposited by conventional electron beam evaporation method and then annealed in air at different temperature from 873 to 1273 K. It was found that the film structure changed from amorphous phase to hexagonal phase when annealed at 1073 K, then transformed to orthorhombic phase after annealed at 1273 K. The transmittance was improved after annealed at 873 K, and it decreased as the annealing temperature increased further. The total integrated scattering (TIS) tests and AFM results showed that both scattering and root mean square (RMS) roughness of films increased with the annealing temperature increasing. X-ray photoelectron spectroscopy (XPS) analysis showed that the film obtained better stoichiometry and the O/Ta ratio increased to 2.50 after annealing. It was found that the laser-induced damage threshold (LIDT) increased to the maximum when annealed at 873 K, while it decreased when the annealing temperature increased further. Detailed damaged models dominated by different parameters during annealing were discussed.     

Effects of deposition parameters on laser-induced damage threshold of Ta2O5 films

Ta₂O₅ films were deposited on BK7 substrates by e-beam evaporation with different deposition parameters such as substrate temperature (323-623 K), oxygen pressure (0.5-3.0×10⁻² Pa) and deposition rate (0.2-0.5 nm/s). Absorption, scattering and chemical composition were investigated by surface thermal lensing (STL) technique, total integrated scattering (TIS) measurement and X-ray photoelectron spectroscopy (XPS), respectively. The laser-induced damage threshold (LIDT) was assessed using pulsed Nd:YAG 1064 nm laser at a pulse length of 12 ns. The results showed that optical properties, absorption and LIDT were influenced by the deposition parameters and annealing. However, scattering was little correlated with the deposition parameters. On the whole, the LIDT increased with increasing substrate temperature and oxygen pressure, whereas it increased firstly and then decreased upon increasing deposition rate. After annealing at 673 K for 12 h, the LIDT of films improved significantly. The dependence of possible damage mechanism on deposition parameters was discussed.     

Investigation of annealing effects on the laser-induced damage threshold of amorphous Ta2O5 films

Ta₂O₅ films were deposited using the conventional electron beam evaporation method and then annealed at temperatures in the range 373-673 K. Chemical composition, scattering and absorption were examined by X-ray photoelectron spectroscopy (XPS), total integrated scattering (TIS) measurement and the surface thermal lensing (STL) technique, respectively. The laser-induced damage threshold (LIDT) was assessed using the output from an Nd:YAG laser with a pulse length of 12 ns. The results showed that the improvement of the LIDT after annealing was due to the reduced substoichiometric and structural defects present in the film. The LIDT increased slightly below 573 K and then increased significantly with increase in annealing temperature, which could be attributed to different dominant defects. Moreover, the root mean square (RMS) roughness and scattering had little effect on the LIDT, while the absorption and the LIDT were in accord with a general relation.     

Microstructure and dielectric properties of La2O3 doped amorphous SiO2 films as gate dielectric material

As a potential gate dielectric material, the La₂O₃ doped SiO₂ (LSO, the mole ratio is about 1:5) films were fabricated on n-Si (0 0 1) substrates by using pulsed laser deposition technique. By virtue of several measurements, the microstructure and electrical properties of the LSO films were characterized. The LSO films keep the amorphous state up to a high annealing temperature of 800 °C. From HRTEM and XPS results, these La atoms of the LSO films do not react with silicon substrate to form any La-compound at interfacial layer. However, these O atoms of the LSO films diffuse from the film toward the silicon substrate so as to form a SiO₂ interfacial layer. The thickness of SiO₂ layer is only about two atomic layers. A possible explanation for interfacial reaction has been proposed. The scanning electron microscope image shows the surface of the amorphous LSO film very flat. The LSO film shows a dielectric constant of 12.8 at 1 MHz. For the LSO film with thickness of 3 nm, a small equivalent oxide thickness of 1.2 nm is obtained. The leakage current density of the LSO film is 1.54 × 10⁻⁴ A/cm² at a gate bias voltage of 1 V.     

Annealing temperature influence on electrical properties of ion beam sputtered Bi2Te3 thin films

Ion beam sputtering process was used to deposit n-type fine-grained Bi₂Te₃ thin films on BK7 glass substrates at room temperature. In order to enhance the thermoelectric properties, thin films are annealed at the temperatures ranging from 100 to 400 °C. X-ray diffraction (XRD) shows that the films have preferred orientations in the c-axis direction. It is confirmed that grain growth and crystallization along the c-axis are enhanced as the annealing temperature increased. However, broad impurity peaks related to some oxygen traces increase when the annealing temperature reached 400 °C. Thermoelectric properties of Bi₂Te₃ thin films were investigated at room temperature. The Bi₂Te₃ thin films, including as-deposited, exhibit the Seebeck coefficients of −90 to −168 μV K⁻¹ and the electrical conductivities of 3.92×10²-7.20×10² S cm⁻¹ after annealing. The Bi₂Te₃ film with a maximum power factor of 1.10×10⁻³ Wm⁻¹ K⁻² is achieved when annealed at 300 °C. As a result, both structural and transport properties have been found to be strongly affected by annealing treatment. It was considered that the annealing conditions reduce the number of potential scattering sites at grain boundaries and defects, thus improving the thermoelectric properties.     

Growth of high-density Ru- and RuO2-composite nanodots on atomic-layer-deposited Al2O3 film

Growth of Ru- and RuO₂-composite (ROC) nanodots on atomic-layer-deposited Al₂O₃ film has been studied for the first time using ion-beam sputtering followed by post-deposition annealing (PDA). X-ray photoelectron spectroscopy analyses reveal that RuO₂ and Ru co-exist before annealing, and around 10% RuO₂ is reduced to metallic Ru after PDA at 900 °C for 15 s. Scanning electron microscopy measurements show that well-defined spherical ROC nanodots are not formed till the PDA temperature is raised to 900 °C. The mean diameter of the nanodots enlarges with increasing PDA temperature whereas the nanodot density decreases, which is attributed to coalescence process between adjacent nanodots. It is further illustrated that the resulting nanodot size and density are weakly dependent on the annealing time, but are markedly influenced by the decomposition of RuO₂. In this article, the ROC nanodots with a high density of 1.6 × 10¹¹ cm⁻², a mean diameter of 20 nm with a standard deviation of 3.0 nm have been achieved for the PDA at 900 °C for 15 s, which is promising for flash memory application.     

Fabrication of the hydrogen resistive ferroelectric film of the (Pb0.72La0.28)Ti0.93O3/Pb(Zr0.52Ti0.48)O3/(Pb0.72La0.28)Ti0.93O3 heterostructure by a pulsed laser deposition method

(Pb_0.72La_0.28)Ti_0.93O₃ (PLT)/Pb(Zr_0.52Ti_0.48)O₃ (PZT)/PLT heterostructure was fabricated by using a pulsed laser deposition method. After depositing this structure, the hydrogen annealing process was performed in the forming gas (95% N₂ + 5% H₂) at a substrate temperature of 400 °C for 30 min to study the effects of hydrogen passivation.The heterostructure was not degraded by the hydrogen annealing in contrast with the case of PZT film without buffer layers. This heterostructure showed almost no degradation in terms of the remanent polarization even after the H₂ annealing, while the PZT film exhibited 64% reduction, which is from 20.1 to 7.3 μC/cm² after the annealing. The leakage current was decreased by an order in the case of the heterostructure, while the leakage current of the PZT film increased by an order.These can be explained that the PLT bottom buffer layer works as a seeing layer to help the PZT growth and the top PLT buffer layer acts as a barrier for penetrating hydrogen atoms.     

Preparation of sol-gel ZrO2-SiO2 highly reflective multilayer films and laser-induced damage threshold characteristic

Sol-gel (ZrO₂/SiO₂)¹² ZrO₂ films were prepared by spin coating method. The reflectivity spectrum of the films was measured with a Lambda 900 spectrometer. In order to investigate laser-induced damage threshold (LIDT) characteristic of highly reflective films, one-layer ZrO₂ and SiO₂ films, two-layer ZrO₂/SiO₂ and SiO₂/ZrO₂ films were also prepared by spin coating method. LIDT of each film was measured. Damage morphology after laser irradiation was characterized by optical microscopy (Nikon E600K). The experimental results showed that the reflectivity of (ZrO₂/SiO₂)¹² ZrO₂ film at 1064 nm and 355 nm wavelength is 99.7%. The LIDT results decreases as the number of layer of films increases. All the films have similar damage morphology. The experimental results are explained by the different temperature profiles of the films.     

Laser-induced voltage characteristics of Bi2Sr2Co2Oy thin films on LaAlO3 substrates

We report the laser-induced voltage (LIV) effects in c-axis oriented Bi₂Sr₂Co₂O_y thin films grown on (0 0 1) LaAlO₃ substrates with the title angle α of 0°, 3°, 5° and 10° by a simple chemical solution deposition method. A large open-circuit voltage with the sensitivity of 300 mV/mJ is observed for the film on 10° tilting LaAlO₃ under a 308 nm irradiation with the pulse duration of 25 ns. When the film surface is irradiated by a 355 nm pulsed laser of 25 ps duration, a fast response with the rise time of 700 ps and the full width at half maximum of 1.5 ns is achieved. In addition, the experimental results reveal that the amplitude of the voltage signal is approximately proportional to sin 2α and the signal polarity is reversed when the film is irradiated from the substrate side rather than the film side, which suggests the LIV effects in Bi₂Sr₂Co₂O_y thin films originate from the anisotropic Seebeck coefficient of this material.     

Influence of substrate temperature on properties of MgF2 coatings

Thermal boat evaporation was employed to prepare MgF₂ single-layer coatings upon both JGS1 and UBK7 substrates at different substrate temperatures. Microstructure, transmittance and residual stress of these coatings were measured by X-ray diffraction, spectrophotometer, and optical interferometer, respectively. Measurement of laser induced damage threshold (LIDT) of the samples was performed at 355 nm, 8 ns pulses. The results showed that high substrate temperature was beneficial to crystallization of the film. Above 244 °C, the refractive index increased gradually with the substrate temperature rising. Whereas, it was exceptional at 210 °C that the refractive index was higher than those deposited at 244 and 277 °C. The tensile residual stresses were exhibited in all MgF₂ films, but not well correlated with the substrate temperature. In addition, the stresses were comparatively smaller upon JGS1 substrates. A tendency could be seen that the LIDTs reached the highest values at about 244 °C, and the films upon JGS1 had higher LIDTs than those upon UBK7 substrates at the same temperature. Meanwhile, the damage morphologies showed that the laser damage of the coating resulted from an absorbing center at the film-substrate interface. The features of the damages were displayed by an absorbing center dominated model. Furthermore, the reason of the difference in LIDT values was discussed in detail.     

Effect of growth temperature on the morphology and bonded states of SnO2 nanobaskets

The nanobaskets of SnO₂ were grown on in-house fabricated anodized aluminum oxide pores of 80 nm diameter using plasma enhanced chemical vapor deposition at an RF power of 60 W. Hydrated stannic chloride was used as a precursor and O₂ (20 sccm) as a reactant gas. The deposition was carried out from 350 to 500 °C at a pressure of 0.2 Torr for 15 min each. Deposition at 450 °C results in highly crystalline film with basket like (nanosized) structure. Further increase in the growth temperature (500 °C) results in the deterioration of the basket like structure and collapse of the alumina pores. The grown film is of tetragonal rutile structure grown along the [1 1 0] direction. The change in the film composition and bonded states with growth temperature was evident by the changes in the photoelectron peak intensities of the various constituents. In case of the film grown at 450 °C, Sn 3d_5/2 is found built up of Sn⁴⁺ and O-Sn⁴⁺ and the peaks corresponding to Sn²⁺ and O-Sn²⁺ were not detected.     

Preparation of transparent conductive TiO2:Nb thin films by pulsed laser deposition

This study investigated the optical and electrical properties of Nb-doped TiO₂ thin films prepared by pulsed laser deposition (PLD). The PLD conditions were optimized to fabricate Nb-doped TiO₂ thin films with an improved electrical conductivity and crystalline structure. XRD analyses revealed that the deposition at room temperature in 0.92 Pa O₂ was suitable to produce anatase-type TiO₂. A Nb-doped TiO₂ thin film attained a resistivity as low as 6.7 × 10⁻⁴ Ω cm after annealing at 350 °C in vacuum (<10⁻⁵ Pa), thereby maintaining the transmittance as high as 60% in the UV-vis region.     

Characteristics of sandwich-structured Al2O3/HfO2/Al2O3 gate dielectric films on ultra-thin silicon-on-insulator substrates

Sandwich-structure Al₂O₃/HfO₂/Al₂O₃ gate dielectric films were grown on ultra-thin silicon-on-insulator (SOI) substrates by vacuum electron beam evaporation (EB-PVD) method. AFM and TEM observations showed that the films remained amorphous even after post-annealing treatment at 950 °C with smooth surface and clean silicon interface. EDX- and XPS-analysis results revealed no silicate or silicide at the silicon interface. The equivalent oxide thickness was 3 nm and the dielectric constant was around 7.2, as determined by electrical measurements. A fixed charge density of 3 × 10¹⁰ cm⁻² and a leakage current of 5 × 10⁻⁷A/cm² at 2 V gate bias were achieved for Au/gate stack /Si/SiO₂/Si/Au MIS capacitors. Post-annealing treatment was found to effectively reduce trap density, but increase in annealing temperature did not made any significant difference in the electrical performance.     

Auger electron spectroscopy of Au/NiOx contacts on p-GaN annealed in N2 and O2 + N2 ambients

We have designed a promising contact scheme to p-GaN. Au/NiO_x layers with a low concentration of O in NiO_x are deposited on p-GaN by reactive dc magnetron sputtering and annealed in N₂ and in a mixture of O₂ + N₂ to produce low resistivity ohmic contacts. Annealing has been studied of NiO_x layers with various contents of oxygen upon the electrical properties of Au/NiO_x/p-GaN. It has been found that the Au/NiO_x/p-GaN structure with a low content of oxygen in NiO_x layer provides a low resistivity ohmic contact even after subsequent annealing in N₂ or O₂ + N₂ ambient at 500 °C for 2 min.Auger depth profiles and transmission electron microscopy (TEM) micrographs reveal that while annealing in O₂ + N₂ ambient results in reconstruction of the initial deposited Au/NiO_x/p-GaN contact structure into a Au/p-NiO/p-GaN structure, annealing in N₂ brings about reconstruction into Au/p-NiO/p-GaN and Ni/p-NiO/p-GaN structures. Hence, in both cases, after annealing in N₂ as well as in O₂ + N₂ ambient, the ohmic properties of the contacts are determined by creation of a thin oxide layer (p-NiO) on the metal/p-GaN interface. Higher contact resistivities in the samples annealed in O₂ + N₂ ambient are most likely caused by a smaller effective area of the contact due to creation of voids.     

Effect of SiO2 protective layer on the femtosecond laser-induced damage of HfO2/SiO2 multilayer high-reflective coatings

Two kinds of HfO₂/SiO₂ 800 nm high-reflective (HR) coatings, with and without SiO₂ protective layer were deposited by electron beam evaporation. Laser-induced damage thresholds (LIDT) were measured for all samples with femtosecond laser pulses. The surface morphologies and the depth information of all samples were observed by Leica optical microscopy and WYKO surface profiler, respectively. It is found that SiO₂ protective layer had no positive effect on improving the LIDT of HR coating. A simple model including the conduction band electron production via multiphoton ionization and impact ionization is used to explain this phenomenon. Theoretical calculations show that the damage occurs first in the SiO₂ protective layer for HfO₂/SiO₂ HR coating with SiO₂ protective layer. The relation of LIDT for two kinds of HfO₂/SiO₂ HR coatings in calculation agrees with the experiment result.     

Influence of postdeposition annealing on structural properties and electrical characteristics of thin Tm2O3 and Tm2Ti2O7 dielectrics

We describe the structural properties and electrical characteristics of thin thulium oxide (Tm₂O₃) and thulium titanium oxide (Tm₂Ti₂O₇) as gate dielectrics deposited on silicon substrates through reactive sputtering. The structural and morphological features of these films were explored by X-ray diffraction, X-ray photoelectron spectroscopy, secondary ion mass spectrometry, and atomic force microscopy, measurements. It is found that the Tm₂Ti₂O₇ film annealed at 800 °C exhibited a thinner capacitance equivalent thickness of 19.8 Å, a lower interface trap density of 8.37 × 10¹¹ eV⁻¹ cm⁻², and a smaller hysteresis voltage of ∼4 mV than the other conditions. We attribute this behavior to the Ti incorporated into the Tm₂O₃ film improving the interfacial layer and the surface roughness. This film also shows negligible degrees of charge trapping at high electric field stress.     

Stabilization of a very high-k crystalline ZrO2 phase by post deposition annealing of atomic layer deposited ZrO2/La2O3 dielectrics on germanium

The impact of the ZrO₂/La₂O₃ film thickness ratio and the post deposition annealing in the temperature range between 400 °C and 600 °C on the electrical properties of ultrathin ZrO₂/La₂O₃ high-k dielectrics grown by atomic layer deposition on (1 0 0) germanium is investigated. As-deposited stacks have a relative dielectric constant of 24 which is increased to a value of 35 after annealing at 500 °C due to the stabilization of tetragonal/cubic ZrO₂ phases. This effect depends on the absolute thickness of ZrO₂ within the dielectric stack and is limited due to possible interfacial reactions at the oxide/Ge interface. We show that adequate processing leads to very high-k dielectrics with EOT values below 1 nm, leakage current densities in the range of 0.01 A/cm², and interface trap densities in the range of 2-5 × 10¹² eV⁻¹ cm⁻².