Preparation and characterization of Nb2O5-Al2O3 composite oxide formed by cathodic electroplating and anodizing

Al foil was coated with niobium oxide by cathodic electroplating and anodized in a neutral boric acid solution to achieve high capacitance in a thin film capacitor. X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) revealed the niobium oxide layer on Al to be a hydroxide-rich amorphous phase. The film was crystalline and had stoichiometric stability after annealing at temperatures up to 600 °C followed by anodizing at 500 V, and the specific capacitance of the Nb₂O₅-Al₂O₃ composite oxide was approximately 27% higher than that of Al₂O₃ without a Nb₂O₅ layer. The capacitance was quite stable to the resonance frequency. Overall, the Nb₂O₅-Al₂O₃ composite oxide film is a suitable material for thin film capacitors.     

Investigation of Ti-doped Gd2O3 charge trapping layer with HfO2 blocking oxide for memory application

In this study, Ti-doped gadolinium oxide (Gd₂TiO₅) is investigated by X-ray diffraction, atomic force microscopy, and capacitance voltage curves (C-V) as the charge trapping layer in metal-oxide-high-k material-oxide-silicon structure memories. It was found that the Gd₂TiO₅ charge-trapping layer with an HfO₂ blocking layer annealed at 900 °C had a larger window of 4.8 V in the C-V hysteresis loop, a faster program/erase speed and good retention without significant drift up to 10⁴ cycles. This excellent performance was attributed to the well-crystallized Gd₂TiO₅ structure and the higher probability of charges being trapped in the deep trap energy level of the Gd₂TiO_5. This Gd₂TiO₅ memory device with post-annealing shows considerable promise for use in future flash memory applications.     

Mechanical properties and microstructure of Al2O3/TiAl in situ composites doped with Cr2O3

Al₂O₃/TiAl composites were successfully fabricated from powder mixtures of Ti, Al, TiO₂ and Cr₂O₃ by a hot-press-assisted exothermic dispersion method. The effect of the Cr₂O₃ addition on the microstructures and mechanical properties of Al₂O₃/TiAl composites was characterized, and the results showed that the Rockwell hardness, flexural strength and fracture toughness of the composites increased as the Cr₂O₃ content increased. When the Cr₂O₃ content was 2.5 wt%, the flexural strength and the fracture toughness attained peak values of 925 MPa and 8.55 MPa m^1/2, respectively. This improvement of mechanical properties was due to the more homogeneous and finer microstructure developed from the addition of Cr₂O₃ and an increase in the ratio of α₂-Ti₃Al to γ-TiAl matrix phases.     

Electrical characteristics of Ti-O/Ta2O5 thin film sputtered on Ta/Ti/Al2O3 substrate

The electrical characteristics of Ti-O/Ta₂O₅ films sputtered on Ta/Ti/Al₂O₃ substrate were investigated. Ta (tantalum) was used for the bottom and upper electrodes for the purpose of simplifying the fabrication process and Al₂O₃ substrates were used, which are needed in integral passive devices. Ta/Ti-O/Ta₂O₅/Ta/Ti/Al₂O₃ capacitors were annealed at 700 °C for 60 s in vacuum. The X-ray diffraction pattern (XRD) results showed that as-deposited Ta had a highly preferred orientation, but Ta₂O₅ film had amorphous structure, which was transformed to crystallization structure by rapid thermal heat treatment. We examined the log J-E and C-V characteristics of the dielectric thin films deposited on the Ta bottom electrode. From these results, we concluded that the leakage current could be reduced by introducing a Ti-O buffer layer. The conduction mechanisms of Ta/Ti-O/Ta₂O₅/Ta/Ti/Al₂O₃ capacitors could be interpreted appropriately by hopping conduction in lower field (E<1×10⁵ V/cm) and space-charge-limited current in higher fields (1×10⁵ V/cm<E).     

Lightweight geopolymer made of highly porous siliceous materials with various Na2O/Al2O3 and SiO2/Al2O3 ratios

The syntheses of lightweight geopolymeric materials from highly porous siliceous materials viz. diatomaceous earth (DE) and rice husk ash (RHA) with high starting SiO₂/Al₂O₃ ratios of 13.0-33.5 and Na₂O/Al₂O₃ ratios of 0.66-3.0 were studied. The effects of fineness and calcination temperature of DE, concentrations of NaOH and KOH, DE to RHA ratio; curing temperature and time on the mechanical properties and microstructures of the geopolymer pastes were investigated. The results indicated that the optimum calcination temperature of DE was 800 °C. Increasing fineness of DE and starting Na₂O/Al₂O₃ ratio resulted in an increase in compressive strength of geopolymer paste. Geopolymer pastes activated with NaOH gave higher compressive strengths than those with KOH. The optimum curing temperature and time were 75 °C and 5 days. The lightweight geopolymer material with mean bulk density of 0.88 g/cm³ and compressive strength of 15 kg/cm² was obtained. Incorporation of 40% RHA to increase starting SiO₂/Al₂O₃ and Na₂O/Al₂O₃ ratios to 22.5 and 1.7 and enhanced the compressive strength of geopolymer paste to 24 kg/cm² with only a marginal increase of bulk density to 1.01 g/cm³. However, the geopolymer materials with high Na₂O/Al₂O₃ (>1.5) were not stable in water submersion.     

Preparation and thermoelectric properties of nc-Si:(Al2O3 + SiO2) composite film

A composite film of nanocrystalline Si (nc-Si) embedded in (Al₂O₃ + SiO₂) has been prepared on a quartz substrate by thermally evaporating a 400 nm thick Al film on a quartz substrate and annealing in air at 580 °C for 1 h. During annealing, the Al reacts with the SiO₂ of the quartz substrate and produces nc-Si, which is embedded in the (Al₂O₃ + SiO₂) film. The average size of nc-Si is ~ 22 nm and the thickness of the nc-Si:(Al₂O₃ + SiO₂) composite film is ~ 810 nm. It is found that the prepared film is thermoelectric with a Seebeck coefficient of − 624 μV/K at 293 K and − 225 μV/K at 413 K.     

Characterization of Al2O3/ZrO2 nano multilayer thin films prepared by pulsed laser deposition

Microstructural characterization of pulsed laser deposited Al₂O₃/ZrO₂ multilayers on Si (1 0 0) substrates at an optimized oxygen partial pressure of 3 × 10⁻² mbar and at room temperature (298 K) has been carried out. A nanolaminate structure consisting of alternate layers of ZrO₂ and Al₂O₃ with 40 bi-layers was fabricated at different zirconia layer thicknesses (20, 15 and 10 nm). The objective of the work is to study the effect of ZrO₂ layer thickness on the stabilization of tetragonal ZrO₂ phase for a constant Al₂O₃ layer thickness of 5 nm. The Al₂O₃/ZrO₂ multilayer films were characterized using high temperature X-ray diffraction (HTXRD) in the temperature range 298–1473 K. The studies showed that the thickness of the zirconia layer has a profound influence on the crystallization temperature for the formation of tetragonal zirconia phase. The tetragonal phase content increased with the decrease of ZrO₂ layer thickness. The cross-sectional transmission electron microscope (XTEM) investigations were carried out on a multilayer thin films deposited at room temperature. The XTEM studies showed the formation of uniform thickness layers with higher fraction of monoclinic and small fraction of tetragonal phases of zirconia and amorphous alumina.     

Bond strength and microstructure investigation of Al2O3/Al/Al2O3 joints with surface modification of alumina by titanium

Joints of Al₂O₃/Al/Al₂O₃ are formed by liquid-state bonding of alumina substrates covered with thin titanium film of 800 nm thickness using an Al interlayer of 30 or 300 μm at 973 K under a vacuum of 0.2 mPa for 5 min and an applied pressure of 0.01 MPa. The bond strength of the joints is examined by a four-point bend testing at room temperature coupled with optical, scanning and transmission electron microscopy. Results show that: (i) bonding occurs due to the formation of a reactive interface on the metal side of the joint with the presence of Al₃Ti precipitates (ii) a decrease in Al layer thickness leads to stronger Al₂O₃/Al/Al₂O₃ bonds accompanied by a change of both the distribution of reaction products (Al₃Ti) in the region of the interface and the failure surface characteristics.     

Annealing temperature dependence of Er photoluminescence in alternately Er-doped Si-rich Al2O3 multilayer film

Alternately Er-doped Si-rich Al₂O₃ multilayer film, which consists of 20 layers of alternate Er-Si-codoped Al₂O₃ and Si-doped Al₂O₃ layers, has been synthesized by magnetron cosputtering. The structural and optical properties of the multilayer film as a function of annealing temperature in the range of 700-1100 °C were studied by Raman, X-ray diffraction, high-resolution transmission electron microscopy and photoluminescence (PL). The results show that Si atoms in the multilayer film cluster and have been crystallized gradually into Si nanocrystals with increasing annealing temperature to 950 °C. Upon annealing above 950 °C, however, the Er₂O₃ and Er₄Al₂O₉ phases have been formed, resulting in a rapid decrease of PL intensity. It is necessary to control the size and spatial distributions of Si-NCs and optically activate Er³⁺ ions in order to improve PL response.     

High performance self-aligned top-gate ZnO thin film transistors using sputtered Al2O3 gate dielectric

High performance self-aligned top-gate zinc oxide (ZnO) thin film transistors (TFTs) utilizing high-k Al₂O₃ thin film as gate dielectric are developed in this paper. Good quality Al₂O₃ thin film was deposited by reactive DC magnetron sputtering technique using aluminum target in a mixed argon and oxygen ambient at room temperature. The resulting transistor exhibits a field effect mobility of 27 cm²/V s, a threshold voltage of − 0.5 V, a subthreshold swing of 0.12 V/decade and an on/off current ratio of 9 × 10⁶. The proposed top-gate ZnO TFTs in this paper can act as driving devices in the next generation flat panel displays.     

Overview of optical properties of Al2O3 films prepared by various techniques

We study optical properties of Al₂O₃ films prepared by various techniques using spectroscopic ellipsometry. The film preparation techniques include conventional pulsed magnetron sputtering in various gas mixtures, high power impulse magnetron sputtering, annealing of as-deposited Al₂O₃ in an inert atmosphere and annealing of as-deposited Al in air. We focus on the effect of the preparation technique, deposition parameters and annealing temperature on the refractive index, n, and extinction coefficient, k, of stoichiometric Al₂O₃. At a wavelength of 550 nm we find n of 1.50-1.67 for amorphous deposited Al₂O₃, 1.65-1.67 for amorphous Al₂O₃ obtained by Al annealing, 1.46-1.69 for γ-Al₂O₃ and decreasing n for Al₂O₃ annealing temperature increasing up to 890 °C. The results facilitate correct interpretation of optical characterization of Al₂O₃, as well as selection of a preparation technique corresponding to a required Al₂O₃ structure and properties.     

Dielectric properties of DC reactive magnetron sputtered Al2O3 thin films

Alumina (Al₂O₃) thin films were sputter deposited over well-cleaned glass and Si < 100 > substrates by DC reactive magnetron sputtering under various oxygen gas pressures and sputtering powers. The composition of the films was analyzed by X-ray photoelectron spectroscopy and an optimal O/Al atomic ratio of 1.59 was obtained at a reactive gas pressure of 0.03 Pa and sputtering power of 70 W. X-ray diffraction results revealed that the films were amorphous until 550 °C. The surface morphology of the films was studied using scanning electron microscopy and the as-deposited films were found to be smooth. The topography of the as-deposited and annealed films was analyzed by atomic force microscopy and a progressive increase in the rms roughness of the films from 3.2 nm to 4.53 nm was also observed with increase in the annealing temperature. Al-Al₂O₃-Al thin film capacitors were then fabricated on glass substrates to study the effect of temperature and frequency on the dielectric property of the films. Temperature coefficient of capacitance, AC conductivity and activation energy were determined and the results are discussed.     

Properties of polyimide/Al2O3 and Si3N4 deposited thin films

Polyimide (PI) nanocomposites with different proportions of Al₂O₃ were prepared via two-step reaction. Silicon nitride (Si₃N₄) was deposited on PI composite films by a RF magnetron sputtering system and used as a gas barrier to investigate the water vapor transmission rate (WVTR). The thermal stability and mechanical properties of a pure PI film can be improved obviously by adding adequate content of Al₂O₃. At lower sputtering pressure (4 mTorr), the PI/Al₂O₃ hybrid film deposited with Si₃N₄ barrier film exhibits denser structure and lower root mean square (RMS) surface roughness (0.494 nm) as well as performs better in preventing the transmission of water vapor. The lowest WVTR value was obtained from the sample, 4 wt.%Al₂O₃-PI hybrid film deposited with Si₃N₄ barrier film with the thickness of 100 nm, before and after bending test. The interface bonding, Al-N and Al-O-Si, was confirmed with the XPS composition-depth profile.     

Using a slit doser to probe gas dynamics during Al2O3 atomic layer deposition and to fabricate laterally graded Al2O3 layers

A special slit doser is used to form near unit steps in the spatial profile of an Al₂O₃ ALD film thickness. The unit step is formed as the Al₂O₃ ALD occurs mainly downstream from the slit doser because the trimethylaluminum and H₂O reactants are entrained in a viscous flow carrier gas. Spectroscopic ellipsometry measurements yielded thickness profiles of Al₂O₃ ALD on samples placed at different locations relative to the exit of the slit doser and the ALD growth zone. The effects of carrier gas flow rate, reactor pressure, and reactant dose and purge times on the Al₂O₃ ALD film profile provided details about the gas dynamics around the slit doser. Experimental indications of gas turbulence were observed at the exit of the slit doser. Lateral gradients in the Al₂O₃ ALD film thickness were also formed by linear translation of the sample relative to the slit doser during ALD. Lateral gradients of various desired pitches ranging from 119 Å/in to 444 Å/in were achieved as a result of accurate control of the Al₂O₃ ALD film thickness and small sample translation steps relative to the slit doser.     

Formation process of Al2O3 thin film by reactive sputtering

Al and Al₂O₃ films were deposited by RF magnetron sputtering using a mixed gas of Ar and O₂. The surface of the Al target was changed from the metallic mode to the oxide mode at a critical O₂ flow ratio of 8%. The atomic ratio of sputtered Al atoms to supplied oxygen atoms was found to be approximately 2:3 at the critical O₂ flow ratio. The oxide layer thickness formed on the Al target was estimated to be 5-7 nm at an O₂ flow ratio of 100% by ellipsometry.     

Protection of polymer from atomic-oxygen erosion using Al2O3 atomic layer deposition coatings

Thin films of Al₂O₃ grown using atomic layer deposition (ALD) techniques can protect polymers from erosion by oxygen atoms. To quantify this protection, polyimide substrates with the same chemical repeat unit as Kapton^® were applied to quartz crystal microbalance (QCM) sensors. Al₂O₃ ALD films with varying thicknesses were grown on the polyimide substrates. The ALD-coated polyimide materials were then exposed to a hyperthermal atomic-oxygen beam. The mass loss versus oxygen-atom exposure time was measured in situ by the QCM. Al₂O₃ ALD film thicknesses of ∼ 35 Å were found to protect the polymer from erosion.     

Characterization of metal-supported Al2O3 thin films by scanning electrochemical microscopy

In this paper, physiochemical properties of amorphous alumina thin films, grown by the metal organic chemical vapour deposition process on the surface of platinum (Pt/Al₂O₃) and stainless steel (SS/Al₂O₃), were investigated in aqueous media. The study was performed by the use of scanning electrochemical microscopy (SECM), which allowed obtaining information on uniformity, topography and chemical stability/reactivity of the alumina coatings with high spatial resolution. In particular, the effects due to local acid, base and fluoride ions attack on alumina layers of thickness of about 250 nm (in the Pt/Al₂O₃ sample) and 1000 nm (in the SS/Al₂O₃ sample) were investigated. In the acid and base attack, high concentrations of H₂SO₄ and KOH were electrogenerated locally by the use of a 25 μm diameter platinum microelectrode. The latter was also used as SECM tip to monitor the chemical effect on the alumina layers. It was found that, regardless of the thickness of the film, alumina provided good resistance against local attack of concentrated H₂SO₄; instead, the film dissolved when subjected to KOH attack. The dissolution rate depended on several experimental parameters, such as SECM-tip to substrate distance, electrolysis time and alumina film thickness. The alumina layer proved also relatively poor resistance to etching in 0.1 M NaF solutions.     

The effect of bond coat on mechanical properties of plasma-sprayed Al2O3 and Al2O3-13 wt% TiO2 coatings on AISI 316L stainless steel

In this study, Al₂O₃ and Al₂O₃-13 wt% TiO₂ were plasma sprayed onto AISI 316L stainless-steel substrate with and without Ni-5 wt% Al as bond coat layer. The coated specimens were characterized by optical microscopy, metallography and X-ray diffraction (XRD). Bonding strength of coatings were evaluated in accordance with the ASTM C-633 method. It was observed that the dominant phase was Al₂O₃ for both coatings. It was also found that the hardness of coating with bond coat was higher than that of coating without bond coat. Metallographic studies revealed that coating with bond coating has three different regions, which are the ceramic layer (Al₂O₃ or Al₂O₃-13 wt% TiO₂), the bond coating, and matrix, which is not affected by coating. The coating performed by plasma-spray process without bond coating has two zones, the gray one indicating the ceramic layer and the white one characterizing the matrix. No delamination or spalling was observed in coatings. However, there are some pinholes in coating layer, but they are very rare. The bonding strength of coatings with bond coat was higher than that of coating without bond coat. The strength of adhesion and cohesion was determined by means of a planemeter. It was seen that percentage of cohesion strength was higher than that of adhesion strength.     

Single-source chemical vapor deposition of clean oriented Al2O3 thin films

Clean oriented Al₂O₃ thin film with a dominant Al₂O₃ <1 1 3> plane was deposited on Si <1 0 0> substrate at 550 °C, by single-source chemical vapor deposition (CVD) using aluminium(III) diisopropylcarbamate, Al₂(O₂CNⁱPr₂)₆. This process represents a substantial reduction in typical CVD film growth temperatures which are typically > 1000 °C. Through the studies of thermal stability of this precursor, we propose a specific β-elimination decomposition pathway to account for the low temperature of the precursor decomposition at the substrate, and for the lack of carbon impurity byproducts in the resulting alumina films that are characterized using X-ray photoelectron spectroscopy and depth profiling.     

Oxygen vacancy in Al2O3: Photoluminescence study and first-principle simulation

Broad photoluminescence (PL) band at 2.97 eV excited in the band near 6.0 eV in amorphous chemical vapor deposition films is related to the neutral oxygen vacancy by analogy with crystalline Al₂O₃. The identification of this PL band was supported by the results of first-principle quantum chemical simulation, which showed 6.3 and 6.4 eV bands in the extinction spectra for α- and γ-Al₂O₃, respectively. Other PL bands are attributed to ionized single vacancies (F⁺-centers), divacancies (F₂) and, probably, interstitial Al.