Laser etching of transparent materials at a backside surface adsorbed layer

The laser etching using a surface adsorbed layer (LESAL) is a new method for precise etching of transparent materials with pulsed UV-laser beams. The influence of the processing parameters to the etch rate and the surface roughness for etching of fused silica, quartz, sapphire, and magnesium fluoride (MgF₂) is investigated. Low etch rates of 1 nm/pulse and low roughness of about 1 nm rms were found for fused silica and quartz. This is an indication that different structural modifications of the material do not affect the etching significantly as long as the physical properties are not changed. MgF₂ and sapphire feature a principal different etch behavior with a higher etch rate and a higher roughness. Both incubation effects as well as the temperature dependence of the etch rate can be interpreted by the formation of a modified near surface region due to the laser irradiation. At repetition rates up to 100 Hz, no changes of the etch rate have been observed at moderate laser fluences.     

The effect of hydrogen as an additive in reactive ion etching of GaAs for obtaining polished surface

The effect of hydrogen on the reactive ion etching (RIE) of GaAs in the CF₂Cl₂ plasma is discussed. The addition of hydrogen into the reaction mixture improves the sharpness of etch borders; the etched surface is smooth for etching depth > 1 μm, etching rate is time-constant.     

Dependence of surface distribution of self-assembled InSb nanodots on surface morphology and spacer layer thickness

Self-assembled InSb nanodots (NDs) were grown on a GaSb (1 0 0) substrate using metal-organic vapour phase epitaxy (MOVPE). The effects of etching depth of the substrate and thickness of the GaSb buffer layer on the density and size distribution of single and double layer dots were studied for detector applications. The etch depth of the substrate was varied up to 30 μm. In this particular study, the dots were grown at 450 °C and the GaSb spacer thickness was varied between 50 nm and 200 nm. The optimum substrate etch depth was found to be 30 μm while the best spacer thickness was found to be 200 nm.     

Quasi-two-dimensional conductivity and magnetoconductivity of graphite-like nanosize crystallites

The temperature dependence of electrical conductivity and magnetoconductivity of new type of carbon films composed of nanosize thin graphite-like crystallites were investigated at temperature interval of 4.2-300 K and in the magnetic field range of 0-12 kG at 4.2 K, respectively. The crystallites consist of several (5-50) graphene layers which have predominant orientation perpendicularly to a film surface. At temperature ≤30 K the logarithmic conductivity decreases linearly with temperature. The positive magnetoconductivity of the films was observed in a magnetic field directed perpendicularly to the film surface in all intervals of field values. In magnetic field B≥4 kG the logarithmic asymptotic of conductivity from magnetic field was observed. That is characteristic of the systems with two-dimensional quantum corrections to magnetoconductivity. In a magnetic field directed along a film surface, the crossover from negative to positive magnetoresistivity is observed at B≥8 kG.     

Dry etching of ITO by magnetic pole enhanced inductively coupled plasma for display and biosensing devices

The dry etching of indium tin oxide (ITO) layers deposited on glass substrates was investigated in a high density inductively coupled plasma (ICP) source. This innovative low pressure plasma source uses a magnetic core in order to concentrate the electromagnetic energy on the plasma and thus provides for higher plasma density and better uniformity. Different gas mixtures were tested containing mainly hydrogen, argon and methane. In Ar/H₂ mixtures and at constant bias voltage (−100 V), the etch rate shows a linear dependence with input power varying the same way as the ion density, which confirms the hypothesis that the etching process is mainly physical. In CH₄/H₂ mixtures, the etch rate goes through a maximum for 10% CH₄ indicating a participation of the radicals to the etching process. However, the etch rate remains quite low with this type of gas mixture (around 10 nm/min) because the etching mechanism appears to be competing with a deposition process. With CH₄/Ar mixtures, a similar feature appeared but the etch rate was much higher, reaching 130 nm/min at 10% of CH₄ in Ar. The increase in etch rate with the addition of a small quantity of methane indicates that the physical etching process is enhanced by a chemical mechanism. The etching process was monitored by optical emission spectroscopy that appeared to be a valuable tool for endpoint detection.     

Catalysis, by amorphous carbon, of H2 attack on oxidized U-0.1 wt% Cr surfaces

Amorphous carbon, evaporated on a thin oxide layer covered U-0.1 wt% Cr sample, was proven to significantly catalyze H₂ reaction with the metal. A hydride was formed preferentially on the carbon-covered surface, for vacuum pretreatment temperatures of 150 and 190 °C and hydrogen reactions of 150 and 90 °C, respectively. Dependence of the reaction rate on the thickness of the layer was observed.     

In situ HCl etching of Si for the elaboration of locally misorientated surfaces

We have studied the in situ HCl etching of Si active areas on patterned wafers. After some in situ HCl etching at 20 Torr of Si(1 0 0), we have locally obtained 2 μm long areas with misorientation angles around 4.5° towards 〈1 1 0〉. Furthermore, we have evidenced a recess shape transition from convex (T ≤ 865 °C) to concave (T ≥ 895 °C) as the etch temperature increases, with a nearly flat surface with no facets at T = 880 °C. The morphology of the etched structures at a given time, temperature and PHCl/PH₂ ratio will be a function of the slope lengths and the pattern dimensions. Different kinds of surfaces (rounded areas, facets) were obtained in 3.5 μm × 3.5 μm Si windows after HCl etching at 850 °C during 300 s, depending on the stress within. Thermal oxidations can indeed be used to increase by 65 MPa up to 110 MPa the compressive stress in those Si windows which are bordered by SiO₂ shallow trench isolation. An increase of the misorientation angle from 4.5° up to 6° occurred after the above-mentioned HCl etch when switching from conventional to highly strained Si windows. For the shortest etching times studied here (150 s), a selective etching of 3.5 μm × 3.5 μm Si windows edges is responsible for the misorientation. The etch is then more uniform. Stress gradients might consequently be one of the main misorientation causes. We have also probed the influence of the shallow trench isolation (STI) thickness on the misorientation. A morphological difference before HCl etching has been shown to be responsible for the transition from sloped to rounded areas. A local loading effect may prevail in this case.     

Properties of AlN grown by plasma enhanced atomic layer deposition

The influence of growth parameters on the properties of AlN films fabricated by plasma-enhanced atomic layer deposition using trimethylaluminum and ammonia precursors was investigated. The atomic concentrations, refractive index, mass density, crystallinity and surface roughness were studied from the films grown in the temperature range of 100-300 °C with plasma discharge times between 2.5 and 30 s. The AlN films were shown to be hydrogen rich having H concentrations in the range of 13-27 at.% with inverse dependence on the growth temperature. The carbon and oxygen concentrations in the films were less than 2.6% and 0.2%, respectively. The refractive index and mass density of the films correlated with the hydrogen concentration so that higher concentrations (lower growth temperatures) resulted in smaller refractive index and mass density. The film grown at 300 °C was found to be crystalline whereas lower growth temperature produced amorphous films.     

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.     

Dry etching of CuCrO2 thin films

Highly conducting films of p-type CuCrO₂ are attractive as hole-injectors in oxide-based light emitters. In this paper, we report on the development of dry etch patterning of CuCrO₂ thin films. The only plasma chemistry that provided some chemical enhancement was Cl₂/Ar under inductively coupled plasma conditions. Etch rates of ∼500 Å min⁻¹ were obtained at chuck voltages around −300 V and moderate source powers. In all cases, the etched surface morphologies were improved relative to un-etched control samples due to the smoothing effect of the physical component of the etching. The threshold ion energy for the onset of etching was determined to be 34 eV. Very low concentrations (≤1 at.%) of residual chlorine were detected on the etched surfaces but could be removed by simple water rinsing.     

Current-temperature measurements of a SBD evaporated onto inductively coupled plasma cleaned germanium

Inductively coupled plasma (ICP) etching has been used primarily on compound semiconductors. There are however compelling reasons to study the effects of ICP etching on Ge. Pd Schottky barrier diodes (SBDs) were resistively evaporated onto Ge (1 1 1) that was ICP etched at a rate of 60 Å per minute for three or ten minute intervals. Although plasma cleaning is known to introduce defects that were observed with DLTS, the diodes exhibited excellent current-voltage characteristics when cooled down to 80 K. Current-temperature (IT) scans that were recorded from 20 K up to 300 K after cooling under reverse bias showed no effect of recombination/generation (RG). On the other hand, IT scans that were recorded after cooling under zero or forward bias clearly exhibited RG effects in the 100-240 K temperature range. This effect was found to be completely reversible. In addition, ICP etching leads to superior devices when compared to devices manufactured by RF sputter deposition.     

Microstructuring of fused silica by laser-induced backside wet etching using picosecond laser pulses

The laser-induced backside wet etching (LIBWE) is an advanced laser processing method used for structuring transparent materials. LIBWE with nanosecond laser pulses has been successfully demonstrated for various materials, e.g. oxides (fused silica, sapphire) or fluorides (CaF₂, MgF₂), and applied for the fabrication of microstructures. In the present study, LIBWE of fused silica with mode-locked picosecond (t_p = 10 ps) lasers at UV wavelengths (λ₁ = 355 nm and λ₂ = 266 nm) using a (pyrene) toluene solution was demonstrated for the first time. The influence of the experimental parameters, such as laser fluence, pulse number, and absorbing liquid, on the etch rate and the resulting surface morphology were investigated. The etch rate grew linearly with the laser fluence in the low and in the high fluence range with different slopes. Incubation at low pulse numbers as well as a nearly constant etch rate after a specific pulse number for example were observed. Additionally, the etch rate depended on the absorbing liquid used; whereas the higher absorption of the admixture of pyrene in the used toluene enhances the etch rate and decreases the threshold fluence. With a λ₁ = 266 nm laser set-up, an exceptionally smooth surface in the etch pits was achieved. For both wavelengths (λ₁ = 266 nm and λ₂ = 355 nm), LIPSS (laser-induced periodic surface structures) formation was observed, especially at laser fluences near the thresholds of 170 and 120 mJ/cm², respectively.     

Analysis of mechanism of carbon removal from GaAs(1 0 0) surface by atomic hydrogen

Etching of carbon contaminations from the GaAs(1 0 0) surface by irradiating with atomic hydrogen, which is one of the key reactions to promote high-quality thin films growth by molecular beam epitaxy (MBE), has been investigated by mass spectrometry (MS), Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS). It is shown that during the cleaning process at room temperature a total reduction of the Auger carbon signal, accompanied by desorption of methane as major reaction product, can be observed. The reaction pathways as well as the processes responsible for the observed carbon removal are discussed in detail to give a support for etching and growth quality enhancement not only in thin films epitaxy but in all atomic hydrogen promoted gas-phase III-V semiconductor processes.     

Molecular dynamics simulation of deposition and etching of Si bombarding by energetic SiF

In this study, SiF interaction with amorphous Si surface at normal incidence was investigated using molecular dynamics simulation at 300 and 600 K. The incident energies of 50, 100 and 200 eV were used. The results show that the deposition rate is not sensitive to the incident energy, while with increasing the surface temperature, the deposition rate decreases. The etch yield is sensitive to the incident energy and the surface temperature. The etch yield increases with increasing incident energy and temperature. After bombarding, a Si_xF_y interfacial layer is formed. The interfacial layer thickness increases with increasing incident energy mainly through enhanced penetration of the silicon lattice. In the interfacial layer, for SiF_x (x = 1-3) species, SiF is dominant and only little SiF₃ is present. At the outmost and innermost of the interfacial layer, SiF species is dominant. Most of SiF₃ species is concentrated above the initial surface.     

Electron transport in high quality undoped ZnO film grown by plasma-assisted molecular beam epitaxy

High quality ZnO films were grown on c-plane sapphire substrate using low temperature ZnO buffer layer by plasma-assisted molecular beam epitaxy. The film deposited at 720 °C showed the lowest value of full-width at half maximum for the symmetric (0002) diffraction peak of about 86 arcsec. The highest electron mobility in the films was about 103-105 cm²/V s. From temperature-dependent Hall effect measurements, the mobility strongly depends on the dislocation density at low temperature region and the polar optical phonon scattering at high temperature, respectively. Moreover, by obtaining the activation energy of the shallow donors, it was supposed that hydrogen was source of n-type conductivity in as-grown ZnO films.     

Improving p-type contact characteristics by Ni-assisted annealing and effects on surface morphologic evolution of InGaN LED films grown on Si (1 1 1)

Ni thin layer was deposited to assist to activate p-GaN and then was removed. The process was named Ni-assisted annealing (NA). We investigate the surface morphology and p-type contact behaviors of InGaN LED films grown on Si (1 1 1) substrates. Compared with conventional thermal annealing (TA), NA can improve the p-type contact characteristic at lower anneal temperature and a smaller specific contact resistivity (ρ_c = 6.1 × 10⁻⁵ Ω cm²) employing nonalloy Pt electrode was obtained. A wet etching method using acid-hydrogen peroxide was adopted to boil films surface after activation. We found that some nano-pits appeared on surfaces while original surface step structure was still clearly visible, which shows a defect-selective etching characteristic. Otherwise, we demonstrated that the surface morphology could be affected by NA while independent to TA. Some mechanisms for experimental phenomena were also discussed in the letter.     

Backside etching of fused silica with Nd:YAG laser

The laser-induced backside etching of fused silica with gallium as highly absorbing backside absorber using pulsed infrared Nd:YAG laser radiation is demonstrated for the first time. The influence of the laser fluence, the pulse number, and the pulse length on the etch rate and the etched surface topography was studied. The comparable high threshold fluences of about 3 and 7 J/cm² for 18 and 73 ns pulses, respectively, are caused by the high reflectivity of the fused silica-gallium interface and the high thermal conductivity of gallium. For the 18 and 73 ns long pulses the etch rate rises almost linearly with the laser fluence and reaches a value of 350 and 300 nm/pulse at a laser fluence of about 12 and 28 J/cm², respectively. Incubation processes are almost absent because etching is already observed with the first laser pulse at all etch conditions and the etch rate is constant up to 30 pulses.The etched grooves are Gaussian-curved and show well-defined edges and a smooth bottom. The roughness measured by interference microscopy was 1.5 nm rms at an etch depth of 0.6 μm. The laser-induced backside etching with gallium is a promising approach for the industrial application of the backside etching technique with IR Nd:YAG laser.     

Structural changes of diamond-like carbon films due to atomic hydrogen exposure during annealing

We have deposited diamond-like carbon (DLC) films by radio-frequency magnetron sputtering, and have annealed the films under various conditions to investigate the effects of annealing on the structural properties by visible Raman spectroscopy, X-ray photoelectron spectroscopy and atomic force microscopy. The structural ordering of hydrogenated DLC films occurs during annealing below 400 °C in a vacuum and a hydrogen gas atmosphere, while unhydrogenated DLC films are not ordered during annealing even at 700 °C. On the other hand, the ordering and the decrease of the sp³ content are observed for both the films after annealing under an atomic hydrogen exposure. The ordering progresses as the annealing temperature and time are increased. The reduction of the film thickness after annealing is suppressed with increasing annealing temperature. The results suggest that both the preferential etching by atomic hydrogen and the hydrogen evolution encourage the structural changes under an atomic hydrogen exposure.     

Reactive ion etching of FePt using inductively coupled plasma

We propose a reactive ion etching (RIE) process of an L1₀-FePt film which is expected as one of the promising materials for the perpendicular magnetic recording media. The etching was carried out using an inductively coupled plasma (ICP) RIE system and an etching gas combination of CH₄/O₂/NH₃ was employed. The L1₀-FePt films were deposited on (1 0 0)-oriented MgO substrates using a magnetron sputtering system. The etching masks of Ti were patterned on the FePt films lithographically. The etch rates of ∼16 and ∼0 nm/min were obtained for the FePt film and the Ti mask, respectively. The atomic force microscopy (AFM) analyses provided the average roughness (R_a) value of 0.95 nm for the etched FePt surface, that is, a very flat etched surface was obtained. Those results show that the highly selective RIE process of L1₀-FePt was successfully realized in the present study.     

Control over the wettability of amorphous carbon films in a large range from hydrophilicity to super-hydrophobicity

Control of wettability is of significance in industry as well as our daily live. Amorphous carbon (a-C) films with nanostructured surface were deposited on silicon and glass substrates at different substrate temperatures through a magnetron sputtering technique. The microstructures of the a-C films were studied by SEM and XPS, which indicate that the surface of the a-C films deposited at room temperature are smooth due to their much dense sp³-bonded carbon, while they turn to be more porous graphite-like structure with elevated deposition temperature. The water contact angle (CA) measurements show that these pure carbon films exhibit different wettability, ranging from hydrophilicity with CA less than 40° to super-hydrophobicity with CA of 152°, which reveal that the surface wettability of a-C films can be controlled well by using nanostructures with various geometrical and carbon state features. The graphite-like carbon film deposited at 400 °C without any modification exhibits super-hydrophobic properties, due to the combining microstructures of spheres with nanostructures of protuberances and interstitials. It may have great significance on the study of wettability and relevant applications.