Electrochemical machining of super-hydrophobic Al surfaces and effect of processing parameters on wettability

Super-hydrophobic aluminum (Al) surfaces were successfully fabricated via electrochemical machining in neutral NaClO₃ electrolyte and subsequent fluoroalkylsilane (FAS) modification. The effects of the processing time, processing current density, and electrolyte concentration on the wettability, morphology, and roughness were studied. The surface morphology, chemical composition, and wettability of the Al surfaces were investigated using scanning electron microscopy (SEM) equipped with energy-dispersive spectroscopy (EDS), white-light interferometry, roughness measurements, X-ray diffraction (XRD), Fourier-transform infrared spectrometry (FTIR), and optical contact angle measurements. The results show that hierarchical rough structures and low surface energy films were present on the Al surfaces after electrochemical machining and FAS modification. The combination of the rough structures and the low surface energy materials plays a crucial role in achieving super-hydrophobicity. Compared with the anodic oxidation and chemical etching method, the method proposed in our work does not require strong acid or alkali, and causes less harm to the environment and operators but with high processing efficiency. The rough structures required by the super-hydrophobic surfaces were obtained at 30-s processing time and the best super-hydrophobicity with 164.6^° water contact angle and 2^° tilting angle was obtained at 360 s. The resulting super-hydrophobic Al surfaces have a long-time stability in air and an excellent resistance to corrosive liquids.     

Effect of Cr and V dopants on the chemical stability of AZO thin film

The effect of the dopants of Cr and V on the optoelectronic properties of AZO thin film by pulsed DC magnetron sputtering has been investigated. We also use HCl and KOH solutions to conduct the chemical stability of AZO:Cr:V thin film. The experimental results show that the optimum AZO optoelectronic properties without Cr and V doping obtain the resistivity of 9.87 × 10⁻⁴ Ω cm, optical transmittance of 84% and surface roughness rms value of 2.6 nm. The chemical stability of AZO will increase after Cr and V doping. Under the added V = 0.19 wt.%, Cr = 0.56 wt.%, AZO:Cr:V thin film showed 52% increased chemical stability and 128% decrease in surface roughness after etching (the resistivity was 3.62 × 10⁻³ Ω cm and optical transmittance 81%). From the experimental results, the higher resistivity obtained after KOH etching compared with after HCl etching. The reason is that the Zn/Al ratio will reduce after etching and cause the AZO film carrier density to reduce as well. However, the optical transmittance obtained after KOH etching will be higher than that after HCl etching. This is because that a better surface roughness after KOH etching obtained than after HCl etching.     

A study on the wet etching behavior of AZO (ZnO:Al) transparent conducting film

This paper studies the wet etching behavior of AZO (ZnO:Al) transparent conducting film with tetramethylammonium hydroxide (TMAH). The optimum optoelectronic film is prepared first using designated RF power, film thickness and controlled annealing heat treatment parameters. The AZO film is then etched using TMAH etchant and AZ4620 photoresist with controlled etchant concentration and temperature to examine the etching process effect on the AZO film optoelectronic properties. The experimental results show TMAH:H₂O = 2.38:97.62 under 45 °C at the average etch rate of 22 nm/min as the preferred parameters. The activation energy drops as the TMAH concentration rises, while the etch rate increases along with the increase in TMAH concentration and temperature. After lithography, etching and photoresist removal, the conductivity of AZO film dramatically drops from 2.4 × 10⁻³ Ω cm to 3.0 × 10⁻³ Ω cm, while its transmittance decreases from 89% to 83%. This is due to the poor chemical stability of AZO film against AZ4620 photoresist, leading to an increase in surface roughness. In the photoresist postbaking process, carbon atoms diffused within the AZO film produce poor crystallinity. The slight decreases in zinc and aluminum in the thin film causes a carrier concentration change, which affect the AZO film optoelectronic properties.     

Preparation and rapid thermal annealing of AlN thin films grown by molecular beam epitaxy

AlN films were grown at 785 ^°C on (0001) sapphire substrates by radio-frequency assisted molecular beam epitaxy. Post-growth rapid thermal annealing (RTA) was carried out from 900 to 1200 ^°C for 10 s in flowing N₂. The morphological and structural properties of the AlN epilayers before and after the RTA were studied by atomic force microscopy, x-ray diffraction and transmission electron microscopy. It is found that the threading dislocations can be decreased to an order of magnitude by using an interlayer growth method. The surface roughness (RMS) of the AlN thin films becomes larger with the increase of annealing temperature. The full width at half maximum of AlN (0002) rocking curve reaches its minimum after the RTA at 1000 ^°C.     

Growth and high-temperature electromechanical properties of Ca3NbX3Si2O14 (X=Ga and Al) piezoelectric crystals

Piezoelectric single crystals of Ca₃NbX₃Si₂O₁₄ (CNXS, X=Ga and Al) with ordered langasite structure were successfully grown using the Czochralski technique. The structure was analyzed by X-ray powder diffraction, and the lattice parameters for CNAS were found to decrease slightly when compared to CNGS, due to the smaller ion radius of Al. The dielectric, piezoelectric and electromechanical properties were studied as function of temperature from 30 ^°C to 900 ^°C, showing a stable temperature-dependent behavior. Of particular significant is their high mechanical quality factor and electrical resistivity at elevated temperature, demonstrating CNXS crystals to be promising candidates for high-temperature applications.     

Transparent conductive ZnO:Al films grown by atomic layer deposition for Si-wire-based solar cells

Structural, electrical, and optical properties of atomic layer-controlled Al-doped ZnO (ZnO:Al) films grown by atomic layer deposition (ALD) on glass substrates were characterized at various growth temperatures for use as transparent electrodes. The Al atomic content in ZnO:Al films increased due to the reduced ZnO film growth rate with increasing temperature. The preferred orientation of ZnO:Al films was changed, and the optimum condition for best crystallinity was identified by varying the growth temperature. Furthermore, the carrier concentration of free electron was increased by substituting the Zn sites with Al atoms in the crystal, resulting from monolayer growth based on alternate self-limiting surface chemical reactions. The electrical resistivity of ZnO:Al film grown by ALD at 225 °C reached the lowest value of 8.45 × 10⁻⁴ Ω cm, with a carrier mobility of 9.00 cm² V⁻¹ s⁻¹ and optical transmittance of ∼93%. This result demonstrates that ZnO:Al films grown by ALD possess excellent potential for applications in electronic devices and displays as transparent electrodes and surface passivation layers.     

Influence of post-annealing conditions on properties of ZnO:Ag films

Silver-doped ZnO films were grown on glass substrates by RF reactive magnetron sputtering. The as-grown ZnO:Ag film is insulating but behaves as p-type conduction with a resistivity of 152 Ω cm, a carrier concentration of 2.24×10¹⁶ cm^?3 and a Hall mobility of 1.83 cm²/V s after annealing in O₂ atmosphere at 600 ^°C for 1 h. The influence of post-annealing temperature and ambience on the electrical, structural and optical properties of the films was investigated.     

High work function of Al-doped zinc-oxide thin films as transparent conductive anodes in organic light-emitting devices

Deposition of Al-doped ZnO (AZO) films with various film thicknesses on glass substrates was performed to investigate the feasibility of using AZO films as anode electrodes in organic light-emitting devices (OLEDs). The electrical resistivity of the AZO films with a 180-nm thickness was 4.085 × 10⁻² Ω cm, and the average optical transmittance in the visible range was 80.2%. The surface work function for the AZO films, determined from the secondary electron emission coefficients obtained with a focused ion beam, was as high as 4.62 eV. These results indicate that AZO films grown on glass substrates hold promise for potential applications as anode electrodes in high-efficiency OLEDs.     

MAPLE deposition of PEG:PLGA thin films

We report on MAPLE deposition of thin films of PEG:PLGA blends. The films were analyzed in terms of morphology, chemical composition, wettability, and optical constants. These properties were particularly discussed in correlation with film thickness. The film thickness was increased by increasing the deposition rate (i.e., laser fluence). This method was effective for fluences up to 1 J/cm², above which the efficiency of the deposition leveled off. Moreover, with increasing fluence above 1 J/cm², important changes in the polymeric films were noticed: the surface roughness increased abruptly (up to ∼200 nm), the polymers lost their chemical integrity and their optical constants underwent significant changes. In addition, surface wettability decreased considerably, water contact angle reaching ∼90°; this was attributed to increased surface roughness and to orientation of the hydrophobic groups toward the surfaces of the films. An alternative method for obtaining thicker films was employed, by prolonging the deposition time while maintaining a constant, relatively low, deposition rate (i.e., fluence). In this case, the properties of the films were significantly less affected.     

AlN thin films fabricated by ultra-high vacuum electron-beam evaporation with ammonia for silicon-on-insulator application

The application of silicon-on-insulator (SOI) substrates to high-power integrated circuits is hampered by the self-heating effect due to the poor thermal conductivity of the buried SiO₂ layer. We introduce aluminum nitride (AlN) thin films formed by ultra-high vacuum electron-beam evaporation with ammonia as an alternative. The chemical composition, surface morphology, and electrical properties of these films were investigated. The film synthesized at 800 °C shows a high AlN content, low surface roughness with a root-mean-square value of 0.46 nm, and high electrical resistivity. Based on thermodynamic analysis and our experimental results, the mechanism of AlN formation is proposed.     

Influence of deposition temperature on the crystallinity of Al-doped ZnO thin films at glass substrates prepared by RF magnetron sputtering method

Al-doped ZnO (AZO) transparent conducting films were successfully prepared on glass substrates by RF magnetron sputtering method under different substrate temperatures. The microstructural, electrical and optical properties of AZO films were investigated in a wide temperature range from room temperature up to 350 °C by X-ray Diffraction (XRD), Field-Emission Scanning Electron Microscopy (FESEM), High-Resolution Transmission Electron Microscopy (HRTEM), Hall measurement, and UV–visible meter. The nature of AZO films is polycrystalline thin films with hexagonal wurtzite structure and a preferred orientation along c-axis. The crystallinity and surface morphologies of the films are strongly dependent on the growth temperature, which in turn exerts a great effect on microstructural, electrical and optical properties of the AZO films. The atomic arrangement of AZO film having an wurtzite structure was indeed identified by the HRTEM as well as the Selected Area Electron Diffraction (SAED). The defect density of AZO film was investigated by HRTEM. The film deposited at 100 °C exhibited the relatively well crystallinity and the lowest resistivity of 3.6 × 10⁻⁴ Ω cm. The average transmission of AZO films in the visible range is all over 85%. More importantly, the low-resistance and high-transmittance AZO film was also prepared at a low temperature of 100 °C.     

The reason of degradation in electrical properties of ZnO:Al thin films annealed with various post-annealing temperature

ZnO:Al (AZO) thin films were deposited on glass substrates by RF magnetron sputtering at room temperature and post-annealed in rapid thermal annealing (RTA) system. The effect of post-annealing temperature on the structural, optical, and electrical properties was investigated. As the post-annealing temperature increased, electrical conductivity is deteriorated due to a decrease in the mobility or carrier concentration, gradually. According to X-ray photoelectron spectroscopy (XPS) analysis, the behavior of mobility and carrier concentration is attributed to increase the O₂ absorption on film surface, which act as rising the barrier potential at the low post-annealing temperature (200 °C) and reducing the density of donor-like defects at the high post-annealing temperature (400 °C). In case of post-annealing, the minimization of O₂ absorption is a very important factor to obtain better electrical properties.     

Al/CdSe/GaSe/C resonant tunneling thin film transistors

An Al/CdSe/GaSe/C thin film transistor device was prepared by the physical vapor deposition technique at a vacuum pressure of 10⁻⁵ mbar. The x-ray diffraction measurements demonstrated the polycrystalline nature of the surface of the device. The dc current-voltage characteristics recorded for the Al/CdSe/C and Al/CdSe/GaSe/C channels displayed a resonant tunneling diode features during the forward and reverse voltage biasing, respectively. In addition, the switching current ratio of the Al/CdSe/C increased from 18.6 to 9.62×10³ as a result of the GaSe deposition on the CdSe surface. Moreover, the alternating electrical signal analyses in the frequency range of 1.0 MHz to 1.8 GHz, showed some remarkable properties of negative resistance and negative capacitance spectra of the Al/CdSe/GaSe/C thin film transistors. Two distinct resonance-antiresonance phenomena in the resistance spectra and one in the capacitance spectra were observed at 0.53, 1.04 and 1.40 GHz for the Al/CdSe/C channel, respectively. The respective resonating peak positions of the resistance spectra shift to 0.38 and 0.95 GHz when GaSe is interfaced with CdSe. These features of the thin film transistors are promising for use in high quality microwave filtering circuits and also for use as ultrafast switches.     

A wet chemical preparation of transparent conducting thin films of Al-doped ZnO nanoparticles

A wet chemical deposition method for preparing transparent conductive thin films on the base of Al-doped ZnO (AZO) nanoparticles has been demonstrated. AZO nanoparticles with a size of 7 nm have been synthesised by a simple precipitation method in refluxed conditions in ethanol using zinc acetate and Al-isopropylate. The presence of Al in ZnO was revealed by the EDX elemental analysis (1.8 at.%) and UV–Vis spectroscopy (a blue shift due to Burstein–Moss effect). The obtained colloid solution with the AZO nanoparticles was used for preparing by spin-coating thin films on glass substrates. The film demonstrated excellent homogeneity and transparency (T > 90%) in the visible spectrum after heating at 400 °C. Its resistivity turned to be excessively high (ρ = 2.6 Ω cm) that we ascribe to a poor charge percolation due to a high film porosity revealed by SEM observations. To improve the percolation via reducing the porosity, a sol–gel solution was deposited “layer-by-layer” in alternation with layers derived from the AZO colloid followed by heating. As it was shown by optical spectroscopy measurements, the density of thus prepared film was increased more than twice leading to a significant decrease in resistivity to 1.3 × 10⁻² Ω cm.     

Microstructural and surface property variations due to the amorphous region formed by thermal annealing in Al-doped ZnO thin films grown on n-Si (1 0 0) substrates

X-ray diffraction (XRD) patterns revealed that the as-grown and annealed Al-doped ZnO (AZO) films grown on the n-Si (1 0 0) substrates were polycrystalline. Transmission electron microscopy (TEM) images showed that bright-contrast regions existed in the grain boundary, and high-resolution TEM (HRTEM) images showed that the bright-contrast regions with an amorphous phase were embedded in the ZnO grains. While the surface roughness of the AZO film annealed at 800 °C became smoother, those of the AZO films annealed at 900 and 1000 °C became rougher. XRD patterns, TEM images, selected-area electron diffraction patterns, HRTEM images, and atomic force microscopy (AFM) images showed that the crystallinity in the AZO thin films grown on the n-Si (1 0 0) substrates was enhanced resulting from the release in the strain energy for the AZO thin films due to thermal annealing at 800 °C. XRD patterns and AFM images show that the crystallinity of the AZO thin films annealed at 1000 °C deteriorated due to the formation of the amorphous phase in the ZnO thin films.     

Ultrathin amorphous Ti–Al film used as a diffusion barrier for copper metallization

The viability of ultrathin amorphous Ti–Al film (～4 nm) as a diffusion barrier layer between Cu and Si for the application in Si-based ultra-large scale integration (ULSI) has been investigated. The Cu/Ti–Al/Si heterostructures are annealed in a high vacuum at various temperatures. There is no impurity peaks in the X-ray diffraction patterns for the samples up to annealing temperature of 800 ^°C, although the island-like grains were observed on the surface of the 800 ^°C annealed sample due to dewetting and agglomeration of the Cu film. No inter-reactions can be found from the images of transmission electron microscopy and Ti–Al is still amorphous after high-temperature annealing. These results indicate that Ti–Al film can effectively separate Cu from Si at high temperatures, and that the amorphous ultrathin Ti–Al film can be a very good barrier layer for Cu metallization.     

Growth, coalescence, and electrical resistivity of thin Pt films grown by dc magnetron sputtering on SiO2

Ultra thin platinum films were grown by dc magnetron sputtering on thermally oxidized Si (1 0 0) substrates. The electrical resistance of the films was monitored in situ during growth. The coalescence thickness was determined for various growth temperatures and found to increase from 1.1 nm for films grown at room temperature to 3.3 nm for films grown at 400 °C. A continuous film was formed at a thickness of 2.9 nm at room temperature and 7.5 nm at 400 °C. The room temperature electrical resistivity decreases with increased growth temperature, while the in-plain grain size and the surface roughness, measured with a scanning tunneling microscope (STM), increase. Furthermore, the temperature dependence of the film electrical resistance was explored at various stages during growth.     

Ultra‐thin (002)‐oriented Al‐doped zinc oxide transparent electrode grown on oxygen‐controlled homo‐seed layer

Highly (002)‐oriented Al‐doped zinc oxide (AZO) thin films with the thickness of less than 200 nm have been deposited on an oxygen‐controlled homo‐seed layer at 200 °C by DC magnetron sputtering. With the homo‐seed layer being employed, the full‐width at half maximum (FWHM) of the (002) diffraction peak for the AZO ultra‐thin films decreased from 0.33° to 0.22°, and, the corresponding average grain size increased from 26.8 nm to 43.0 nm. The XRD rocking curves revealed that the AZO ultra‐thin film grown on the seed layer deposited in atmosphere of O₂/Ar of 0.09 exhibited the most excellent structural order. The AZO ultra‐thin film with homo‐seed layer reached a resistivity of 4.2 × 10^–4 Ω cm, carrier concentration of 5.2 × 10²⁰ cm^–3 and mobility of 28.8 cm² V^–1 s^–1. The average transmittance of the AZO ultra‐thin film with homo‐seed layer reached 85.4% in the range of 380–780 nm including the substrate. (© 2014 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Low-temperature direct wafer bonding of GaAs/InP

An approach for low-temperature direct wafer bonding of GaAs/InP was presented. The bonding procedure was carried out at temperatures from 350 to 500 ^°C, and the bonded n-GaAs/n-InP specimens were obtained even at a temperature as low as 350 ^°C. The compositional profile on the GaAs/InP heterointerface was studied by X-ray photoelectron spectroscopy. The bonded interfacial properties were also characterized by current–voltage (I–V$I\text{–}V$) and bonding strength measurement. The experimental results revealed an InGaAsP (or/and InGaAs) interlayer formed at the bonded interface, which influences the electrical property as well as the bonding strength. For the specimen bonded at 350 ^°C, the transport of major carriers could be explained by a tunneling effect. But the carrier transport was described by the thermionic emission theory for the specimen bonded at 450 ^°C. Finally, the mechanism of GaAs/InP bonding was discussed.     

Stable superhydrophobic surface with hierarchical mesh-porous structure fabricated by a femtosecond laser

Inspired by the lotus leaf, a new superhydrophobic surface with hierarchical mesh-porous structure is fabricated by femtosecond laser irradiation on silicon. The fabricated surface shows a superhydrophobic character with water contact angle being found to reach up to 158^°±1^° and sliding angle of 4^°±0.5^°. The superhydrophobicity is stable even if the PH of solution changes from 1 to 14. And the surface also exhibits excellent self-cleaning effect and bouncing behavior, implying that the adhesion of the surface is extremely low. This work will enhance further understanding of the wettability of a solid surface with special surface morphology.