Iron nitride mask and reactive ion etching of GaN films

One of the major GaN processing challenges is useful pattern transfer. Serious photoresist mask erosion and hardening are often observed in reactive ion etching of GaN. Fine pattern transfer to GaN films using photoresist masks and complete removal of remaining photoresist after etching are very difficult. By replacing the etch mask from conventional photoresist to a sputtered iron nitride (Fe-8% N) film, which is easily patterned by wet chemical etching and is very resistive to Cl based plasmas, GaN films can be finely patterned with vertical etched sidewalls. Successful pattern transfer is realized by reactive ion etching using Cl (H) containing plasmas. CHF₃/Ar, C₂ClF₅/Ar, C₂ClF₅/Ar/O₂, SiCl₄, and CHCl₃ plasmas were used to etch GaN. The GaN etch rate is dependent on the crystalline quality of GaN. Higher crystalline quality GaN films exhibit slower etch rates than GaN films with higher dislocation and stacking fault density.     

Calcination‐ and Etching‐Free Photolithography of Inorganic Phosphor Films Consisting of Rare Earth Ion Doped Nanoparticles on Plastic Sheets

It is demonstrated that patterned inorganic phosphor films consisting of rare earth ion doped nanoparticles (RE‐NPs) can be fabricated on plastic sheets using calcination‐ and etching‐free photolithography. Green up‐conversion luminescence and near‐infrared (NIR) fluorescence appears from the RE‐NPs that are prepared from Y₂O₃ doped with 1 mol% Er³⁺ and 0.85 mol% Yb³⁺. The diameter of the RE‐NPs is estimated to be about 300 nm using dynamic light scattering. Visible transmittance of the RE‐NP film fabricated by dip‐coating is more than 90%. Patterned RE‐NP films are obtained by dip‐coating the RE‐NPs on patterned photoresist films fabricated by UV exposure through a photomask, followed by selective removal of the photoresist. Optical, fluorescence, scanning electron, atomic force, and Kelvin probe force microscopies are used for the characterization of the patterned RE‐NP films. The present methodology enables fabrication of patterned RE‐NP films, not only on inorganic substrates but also on plastic sheets, with low cost and material consumption.     

Ion beam-assisted planarization of chemically vapor deposited diamond thin films using electron cyclotron resonance plasma

The high inherent surface roughness of as-deposited polycrystalline diamond films has made effective planarization processing of these films essential for most industrial applications. We have investigated the efficacy of ion beam sources for planarization in an electron cyclotron resonance plasma system using both direct substrate biasing and an accelerating grid system. Rough polycrystalline diamond films were synthesized using hot filament chemical vapor deposition. Both the etching rates and the resultant surface roughnesses were found to decrease as the angle of incidence (relative to the substrate surface normal) of the ion beam was increased. In the case of direct biasing of the sample, acicular features were observed following processing at higher incident angles. The use of double ion-extraction grids in conjunction with concomitant sample rotation was found to produce more uniform planarization of the diamond films. The rate of surface roughness reduction was found to be nonlinear and decreased with time. For both ion extraction methods investigated, the average film roughness (R_a) was significantly reduced from 0.2 to 0.05–0.06 μm.     

Investigations on the damage caused by ion etching of SiO2 layers at low energy and high dose

The radiation damage caused by argon ion bombardment during ion etching of thermally grown SiO₂ films at an energy below 1 keV and a dose of about 10¹⁸ cm^?2 has been studied by evaluating MOS C-V curves, FET characteristics, as well as Rutherford ion backscattering spectra. The bombarded samples revealed that ion beam etching in this energy range causes a damaged layer of 5–10 nm thickness at the single crystal silicon surface. Moreover, traces of metal atoms are found in the damaged layer together with argon atoms (≈ 10²¹cm^?3).     

Patterning and etching of amorphous teflon films

Amorphous Teflon®, deposited by spin-coating and thermal evaporation, has been studied as a low dielectric constant insulator for high performance interconnects. Since it is difficult to deposit a film on amorphous Teflon because of its inert chemical bonds, plasma etching and Zonyl FSN® fluorosurfactant are used to improve the adhesion of photoresist to amorphous Teflon. Plasma etching is shown to increase surface roughness and change chemical bonds of the amorphous Teflon, resulting in improved adhesion of metals and SiO₂ to amorphous Teflon. While amorphous Teflon cannot be etched by wet chemicals, etching the films in Ar, O₂, or CF₄/O₂ plasma is very effective.     

Fabrication of metallic oxide nanowires

Micron length nanowires with varying widths were patterned in half-metallic La_2/3Sr_1/3MnO₃ (LSMO) thin films of different thicknesses, using a thin negative-tone electron beam lithography (EBL) process. Patterns were realized in the high resolution hydrogen silsesquioxane (HSQ) inorganic resist and successfully transferred to the manganite via an energetic argon ion beam etching (IBE). We have obtained wires with widths down to 65 nm and length up to 4 μm that exhibit transport properties comparable with those of unpatterned thin films.     

Structural and optical properties of ZnO films prepared by ion beam sputtering

Based on the ion beam sputtering deposition technology,ZnO thin films are deposited on the glass substrate.The four-factor and three-level L 9(34)orthogonal experiment is used to obtain the best technological parameters of the deposited ZnO thin films,which are the discharge voltage of 3.5 kV,the oxygen current capacity of 8 sccm,the coil current of 8 A and the distance between target and substrate of 140 mm.The purity of the deposited ZnO thin film is 85.77%,and it has good crystallization in orientation.The experimental results show that research and development of the ion beam sputtering source are advanced,and the ion beam sputtering deposition technology can be used to deposit the orientation preferred thin films with good performance.     

Investigations on a Multiple Mask Technique to Depress Processing-Induced Damage of ICP-Etched HgCdTe Trenches

A multiple mask technique, integrating patterned silicon dioxide (SiO₂) film over patterned thick photoresist (PR) film, has been investigated as a method to perform mesa etching for device delineation and electrical isolation of mercury cadmium telluride (HgCdTe) third-generation infrared focal-plane arrays. The multiple mask technique was achieved by standard thick PR photolithography, SiO₂ film deposition to cover the thick PR patterned film, and etching the SiO₂ film at the bottom region after another photolithography process. The dynamic resistance in the zero-bias and low-reverse-bias regions of HgCdTe photodiode arrays isolated by inductively coupled plasma (ICP) etching with the multiple mask of patterned SiO₂ and patterned thick PR film underneath was improved one- to twofold compared with a simple mask of patterned SiO₂. It is suggested that the multiple mask technique is capable of maintaining high etching selectivity while reducing the side-wall processing-induced damage of ICP-etched HgCdTe trenches. The results show that the multiple mask technique is readily available and shows great promise for etching HgCdTe mesa arrays.     

Deposition and surface treatment with intense pulsed ion beams

Intense pulsed ion beams (500 keV, 30 kA, 0.5 μs) are being investigated for materials processing. Demonstrated and potential applications include film deposition, glazing and joining, alloying and mixing, cleaning and polishing, corrosion improvement, polymer surface treatments, and nanophase powder synthesis. Initial experiments at Los Alamos have emphasized thin-film formation by depositing beam ablated target material on substrates. We have deposited films with complex stoichiometry such as YBa₂Cu₃O_7−x and formed diamond-like-carbon films. Instantaneous deposition rates of 1 mm/s have been achieved because of the short ion range (typically 1 μm), excellent target coupling, and the inherently high energy of these beams. Currently the beams are produced in single shot uncomplicated diodes with good electrical efficiency. High-voltage modulator technology and diodes capable of repetitive firing, needed for commercial application, are being developed.     

Formation and characterization of porous silicon films obtained by catalyzed vapor-chemical etching

Porous silicon films obtained by the metal-assisted vapor-chemical etching technique have been characterized. For the film formation, epitaxial (100) N/P⁺, 1–5 Ω cm monocrystalline silicon wafers were used. The vapors of an alcoholic solution of H₂O₂/HF were drawn towards the silicon surface, which was previously covered with a thin layer of gold (~8 nm) for the catalytic etching. For the optical and morphological characterization of porous films, Raman spectroscopy, Ellipsometry, FTIR spectroscopy and SEM images were used. The films thickness kept a linear relationship with etching time. A porosity gradient from the surface towards the interface (65% to 12%) was observed in the films. A large amount of Si–H bonds as related to O–Si–O bonds were observed and the pore size depends on the HF concentration. Irregular morphology was found in films formed with 50% HF.     

Study of high-quality epitaxial YBCO thin films grown directly on Y-Cut LiNbO3

Pulsed laser deposition was used to deposit high-quality YBa₂Cu₃O_7-δ (YBCO) thin films directly on y-cut LiNbO₃ substrates. The as-deposited YBCO films had a high degree of in-plane orientation and showed superconducting transition temperature (T_co) at 91K with a transition width of less than IK. Transport critical current densities were found to be ∼10⁶ A/cm² at 77K and zero field. An ion beam minimum channeling yield of 16% was obtained for YBCO films, indicating high crystallinity. High-resolution transmission electron microscopy studies showed that the interface between the film and the substrate was quite smooth and free from interfacial interdiffusion. The defects in thin films are also identified. The work showed that high-quality high T_c thin films can be deposited directly on LiNbO₃. Novel devices based on the properties of both YBCO and LiNbO₃ could be realized based on these results.     

Investigation of ion-electron emission in the process of reactive ion-beam etching of dielectric thin film heterostructures

This work presents a series of experimental studies to confirm the main theoretical aspects of ionelectron emission and it searches for the possibility of the practical implementation of the operative control method of reactive ion-beam etching processes of different dielectric thin film materials of electronic engineering. The series of experiments was carried out to study the electron emission on the specially formed thinfilm multilayer heterocompositions of Si₃N₄/Si, Ta₂O₅/Al/Si, and Al/TiO₂/Si. The evaluation of the effect of the induced surface potential in the dielectric film on the integral signal of the secondary electrons at reactive ion-beam etching was carried out. The dependence of the emission properties of thin dielectric films on the electric field generated in the dielectric by the surface potential induced by ion beam during reactive ionbeam etching was established. It is noted that the current level of secondary electrons from the surface of dielectric films deposited on the substrates of different materials differ in magnitude; i.e., it is determined by the substrate emission properties. It is shown that the electric field strength arising in the dielectric film under the influence of the induced potential creates the conditions for the emergence of Malter’s emission determined by the properties of its own dielectric and substrate.     

啁啾光纤光栅相位掩模槽形控制新方法研究

在啁啾光纤光栅相位掩模的制作中,针对光刻胶光栅槽形要求比较高的问题,提出离子束刻蚀和反应离子束刻蚀相结合的方法,来实现对相位掩模槽形占宽比的控制.运用高级线段运动算法模拟分析刻蚀中的图形演化,用Ar离子束刻蚀对光刻胶光栅掩模形貌进行修正,然后采用CHF3反应离子束刻蚀,实验和模拟均表明,Ar离子束刻蚀能很好的改善掩模与基片交界处的基片侧壁形貌,使得在CHF3反应离子束刻蚀下能得到较小的占宽比.对槽形控制提供了有意义的实验手段.     

High-quality conformal silicon oxide films prepared by multi-step sputtering PECVD and chemical mechanical polishing

High-quality conformal oxide films were obtained by using multi-step sputtering (MSSP) plasma enhanced chemical vapor deposition (PECVD) process with argon ion sputtering and chemical mechanical polishing (CMP). The repeated deposition by plasma enhanced chemical vapor deposition (PECVD) and anisotropic etching of oxide films by multi-step sputtering PECVD improve the step coverage and gap filling capability significantly. The argon plasma treatment enhances the binding energy of Si-O in the SiO₂ network, and the temperature dependence of stress for MSSP oxide film showed no hysteresis after the heating cycle up to 440 °C. The stress-temperature slope of MSSP oxide film was found to be much less than that of conventional PECVD oxide film. The slope for 1.1 μm thick film is about 5.8×10⁵ dynes/cm²/°C which is smaller than that of thermally grown oxide film. It seems that MSSP oxide film reduces stress-temperature hysteresis and becomes more dense and void-free in the narrow gaps with inter-metal spacing of 0.5 μm. After filling of the narrow gap, we adopted the CMP process for global planarization and obtained good planarization performance. The uniformity of the film thickness was about 4% and the degree of the planarization was over 95% after CMP process.     

Characterization of GaN films etched using reactive ion etching technique by secondary ion mass spectrometry

We investigated GaN films etched by using reactive ion etching (RIE) technique to fabricate the GaN-based devices. The samples were grown on sapphire substrate by metal organic chemical vapor deposition (MOCVD), and Ti/Al contacts were formed on n-GaN surfaces after etching processes. The effects of the kinds of reactive gases were evaluated by secondary ion mass spectrometry (SIMS). The results showed that in the sample etched using BCl₃ gas, the signal from boron contaminations was strongly detected at the interface between the contact metal and n-GaN, and we found that additional etching in Cl₂ plasma after etching with BCl₃ gas was essential to make a good contact.     

Wet Etching Study of La0.67(Sr0.5Ca0.5)0.33MnO3 Films on Silicon Substrates

Wet etching of colossal magnetoresistive (CMR) perovskite La_0.67(Sr_0.5 Ca_0.5)_0.33MnO₃ (LSCMO) films on Bi₄Ti₃O₁₂/CeO₂/yttrium-stabilized zirconia (YSZ)-buffered Si substrates was investigated using potassium hydroxide (KOH) and buffered hydrofluoric acid (BHF) solutions. X-ray diffraction (XRD) and scanning spreading resistance microscopy (SSRM) measurements revealed that the morphological roughness of the LSCMO films increases, while the electrical resistance roughness decreases, with increasing KOH etching time. The LSCMO films are highly chemically resistant to KOH solution; however, in the case of BHF etching, an etch rate of 22 nm/min was obtained with high selectivity over a photoresist mask.     

Fabrication of high-mobility organic single-crystal field-effect transistors with amorphous fluoropolymer gate insulators

High-mobility rubrene single-crystal field-effect transistors are built on highly water- and oil-repellent fluoropolymer gate insulators. Roughness is introduced at the surface once to provide good adhesion to metal films and photoresist polymers for stable electrodes. Before constructing interfaces to crystals, smoothness of the fluoropolymer surface is recovered by annealing at a moderate temperature to maximize carrier mobility. Mobility values estimated in the saturation region reproducibly exceeded 15 cm²/V s for all the 10 devices, reaching 30 cm²/V s for the best two devices. The results demonstrate that the water-repellency and smoothness of the dielectric polymers are favorable for the excellent transistor performance.     

Free-standing SiO2 films containing Si nanocrystals directly suitable for transmission electron microscopy

Free-standing SiO_x films were prepared by molecular beam deposition following back side Silicon (Si) wafer etching in tetramethyl ammonium hydroxide (TMAH) solution. Transmission Electron Microscopy confirms the presence of Si nanocrystals in the as-prepared film. Raman spectroscopy show that deep structural film reorganization appears during high temperature laser treatment. The laser annealing decreases photoluminescence from the films.     

Fabrication and characterization of Ti-Ba-Ca-Cu-O superconducting films on LaAlO3 substrates

A multi-step process is used to fabricate Tl₂Ba₂Ca₁Cu₂O₈ films on (100) LaA10₃ substrates. Submicron thick precursor films of Ba-Ca-Cu-O are rf magnetron sputter deposited from a single target. Film stoichiometry is measured by ion beam backscattering spectroscopy. Deficiencies of the alkaline earths that are found in the precursor films are then compensated for by the addition of appropriate CaF₂ and/or BaF₂ films onto the surface of the precursor film. Post deposition annealing of the films is then done in an atmosphere of thallium oxide and oxygen in order to form the superconducting phases. The annealed films are examined using x-ray diffraction (XRD), an ac inductance technique, and critical current in an external magnetic field. XRD shows the c-axis length of the superconducting phase to increase as the overall film stoichiometry approaches 2212. The transition widths measured by inductive coupling weakly correlate with 77 K critical current measurements. Our best critical current results are 1.5*10⁶ amps/ cm² for a film measured at 4 K in an 8 T magnetic field (parallel to the films' c-axis).     

Fabrication of 128×128 element optical switch array by micromachining technology

Polycrystalline VO₂ thin films were obtained on Si substrates by ion beam sputtering deposition and annealing in flowing Ar gas. SEM images indicate that VO₂ thin films were grown into compact surfaces. Four-probe measurements indicated that the VO₂ thin films own good electrical homogeneity. After the films' production, micromachining technology including lithography, reaction ion etching and metallization connection processes was used to produce the optical switch array. As a result, the 128×128 element optical switch array was achieved.