Microtrenching geometry of 6H-SiC plasma etching

Single-crystal 6H-SiC films were etched in a SF₆/O₂ inductively coupled plasma. Microtrenching which occurred in most experiments at the feet of the profile sidewall was characterized in terms of maximum depth and width. Each characteristic was examined as a function of the process parameters, including ICP coil power, bias voltage, and the O₂ percentage. Experimental results showed that microtrench is caused by the addition of O₂. Apart from the etch mechanisms, relationships between microtrenching and profile angle were also identified. In most cases, the depth and width variations were strongly dependent on the profile angle variation. The statistical experimental design of the process parameters showed that the percentage of O₂ was identified as the most important parameter. The addition of O₂ has influence on the effect of microtrench due to the formation of a SiF_xO_y layer, which have a greater tendency to charge than SiC.     

On the use of a neural network to characterize the plasma etching of SiON thin films

Using a generalized regression neural network (GRNN), plasma etching of oxynitride thin films was modeled. The etch process was characterized by means of a statistical experiment. A genetic algorithm was employed to improve prediction performance by optimizing multiparameterized training factors. Compared to a conventional GRNN model, the constructed etch rate model demonstrated an improvement of about 60% in the prediction performance. 3-D plots were generated to qualitatively interpret etch mechanisms while validating the predictions with experimental data. In separating physical and chemical effects, both dc bias and profile angle variations were effectively utilized. The source power affected significantly the etch rate irrespective of changes in the bias power or C₂F₆ flow rate. For pressure variations, the etch rate was estimated to be dominated by chemical etching. The complex effect of C₂F₆ flow rate could be explained by dominant chemical etching or polymer deposition.     

Surface reaction processes in C4F8 and C5F8 plasmas for selective etching of SiO2 over photo-resist

Surface reactions induced by fluorocarbon plasmas were studied on Si substrates with SiO₂ and photo-resist overlayers using an inductively coupled plasma source. As source gases, C₄F₈ and C₅F₈ were employed to investigate their differences in the etching performance and the selectivity between SiO₂ and photo-resist. Deposition of fluorocarbon polymer was noticed in both gases by Fourier-transform infrared ellipsometric measurements when substrate bias was not applied. With the bias application, etching started on both substrate from certain threshold values of the bias voltage and the rate increased with increase of the voltage. However, in C₅F₈ plasma the increasing tendency on photo-resist was much less than on SiO₂, while in C₄F₈ plasma the difference is small. This difference is attributed to a larger deposition ability of C₅F₈ plasma with higher content of fluorine atoms in the polymer than that of C₄F₈ plasma as confirmed by X-ray photoelectron spectroscopy.     

Etch characteristics of indium zinc oxide thin films in a C2F6/Ar plasma

Dry etching of indium zinc oxide (IZO) thin films was performed using inductively coupled plasma reactive ion etching in a C₂F₆/Ar gas. The etch characteristics of IZO films were investigated as a function of gas concentration, coil rf power, dc-bias voltage to substrate, and gas pressure. As the C₂F₆ concentration was increased, the etch rate of the IZO films decreased and the degree of anisotropy in the etch profile also decreased. The etch profile was improved with increasing coil rf power and dc-bias voltage, and decreasing gas pressure. An X-ray photoelectron spectroscopy analysis confirmed the formation of InF₃ and ZnF₂ compounds on the etched surface due to the chemical reaction of IZO films with fluorine radicals. In addition, the film surfaces etched at different conditions were examined by atomic force microscopy. These results demonstrated that the etch mechanism of IZO thin films followed sputter etching with the assistance of chemical reaction.     

Wavelet uniformity of plasma-processed surface roughness

A technique to characterize the nonuniformity of surface roughness (NSR) is presented. A discrete wavelet transformation (DWT) was used to quantitatively differentiate surface patterns. The technique was evaluated with the data collected from the etching of silicon oxynitride films in a C₂F₆ inductively coupled plasma. 3-D surface images were obtained by using atomic force microscopy. Vertical and lateral NSRs were investigated as a function of process parameters, including radio frequency source power, bias power, and pressure. The NSR data were correlated to experimental measurements of the surface roughness. It is noticeable that for any parameter variations there exist nearly identical NSRs. For each parameter variation, there was at least one specific NSR consistent with the surface roughness measurement. Selected NSRs can be utilized to monitor a variation in NSR and surface roughness simultaneously. Also, NSR may be more stringently optimized by controlling NSRs in a directional fashion.     

Plasma polymerization of fluorocarbon thin films on high temperature substrate and its application to low-k films

Amorphous fluorinated carbon films have been prepared by plasma enhanced chemical vapor deposition method using C₆F₆ at substrate temperature of 400 °C. Thermal stability up to 400 °C is automatically achieved. Dielectric constant of the films is 2. Infrared absorption spectra of the films have indicated that the films contain benzene rings, and F/C ratio is unity as seen in monomer molecules. No film deposition has been observed if C₅F₈ is used as a source monomer at this substrate temperature. In situ Fourier transform infrared spectroscopy of C₆F₆ plasma has indicated production of C₆F₅ because C₁₂F₁₀ has been observed. This result and inclusion of benzene rings in the films suggest that a possible deposition precursor is C₆F₅.     

Surface modification of materials by dielectric barrier discharge deposition of fluorocarbon films

Dielectric barrier discharges have been used to deposit fluorocarbon (FC) films on various materials, such as paper, glass, and silicon substrates. The primary monomers used for plasma polymerization were difluoromethane (CH₂F₂), octafluoropropane (C₃F₈), and octafluorocyclobutane (C₄F₈). FC films were characterized using Fourier transform infrared spectroscopy, atomic force microscopy, static contact angle measurements, and scanning electron microscopy. Surface and structural properties of deposited films are strongly dependent on the plasma compositions and plasma parameters. FC films deposited on paper are to enhance its barrier properties and to achieve hydrophobic surfaces. Contact angle studies reveal that a minimum FC film thickness of about 200 nm on paper is required to completely cover surface and near-surface fibers, thereby providing the paper with long term hydrophobic character. In the C₃F₈ and C₄F₈ systems, the contact angles of the deposited films do not change appreciably with plasma parameters and are strongly dependent on the substrate roughness. Hydrogenated FC films deposited with CH₂F₂ plasmas show the relatively low contact angles due to the existence of CH_X (x = 1-3) groups.     

Deposition of hydrophobic nano-coatings with low-pressure radio frequency CH2F2/Ar plasma processing

In an attempt to perform hydrophobic nano-coating, this investigation examined various operational parameters including in RF plasma power, system gas pressure, and CH₂F₂:Ar ratio of low-pressure plasma processing. The low-pressure plasma, generated with radio frequency power at 13.56 MHz, was fed difluoromethane (CH₂F₂)/Ar gas mixture. The surface characteristics of the plasma polymerized films were studied by static contact angle measurement (CA) and atomic force microscopy (AFM). As a result, increasing deposition of CH₂F₂ plasma polymerized films was achieved in enhanced RF plasma power input. The CH₂F₂ plasma polymerized films also were conducted in a varying system gas pressure with enhanced hydrophobic surface property. The effects of CH₂F₂/Ar plasma on the surface characteristics of the plasma polymerized films were investigated as a function of the Ar content. The super hydrophobic coating under optimized operational parameters prepared in this study obtained water contact angles greater than 150°. It was found that the maximum water contact angles (161°) was obtained at 1.5:1 (CH₂F₂: Ar) ratio. In addition, AFM analysis shows that possible ion bombardment from CH₂F₂/Ar plasma can increase surface roughness, and effectively form a hydrophobic coating on the surface of heat sensitive materials.     

Surface energy modification of SiOxCyHz film using PECVD by controlling the plasma processes for OMCTS (Si4O4C8H24) precursor

SiO_x films produced from octamethylycyclodisiloxane (Si₄O₄C₈H₂₄, OMCTS) with oxygen carrier gas have a low contact angle. The surface energy of the SiO_x films can be changed by controlling the plasma process. SiO_xC_yH_z films were deposited on polycarbonate substrates by plasma enhanced chemical vapor deposition using OMCTS without oxygen carrier gas. The input power in the radio frequency plasma was changed to optimize the surface energy of the resulting SiO_xC_yH_z film. The plasma diagnostics, surface energy and surface morphology were characterized by optical emission spectrometry, contact angle measurements and atomic force microscopy, respectively. The chemical properties of the coatings were examined by Fourier transform infrared spectroscopy. The surface energy of the SiO_xC_yH_z films produced using a room temperature plasma process could be controlled by employing the appropriate intensity of excited neutrals, ionized atoms, molecules and energy (input rf power and bias), as well as the suitable dissociation of OMCTS.     

Scratch-resistant hydrophobic and oleophobic coatings prepared by simple PECVD method

A simple and conventional PECVD method was adopted to synthesize scratch-resistant hydrophobic and oleophobic films, by varying the process condition. The film was designed to be 3 layered. The first SiOx layer was coated on the substrate using OMCTS and O₂, followed by O₂ plasma treatment; hydrocarbon-based hydrophobic film was synthesized using HMDS as a second layer; and finally, CFx-based film was coated using C₂F₆. The first and second layers were synthesized using RF power of 13.56 MHz, while MF power of 40 kHz was used for the CFx layer for ion-assisted deposition. The water contact angle was measured to be 110°–115°, and the oil contact angle was 84° for the best obtained sample. The pencil hardness was measured to be 7H for anti-scratch property. XPS was adopted to analyze the chemical structure and showed that highly cross-linked dense structured film was synthesized.     

Comparison of fluorocarbon film deposition by pulsed/continuous wave and downstream radio frequency plasmas

Fluorocarbon (FC) films have been deposited using pulsed and continuous wave (cw) radio frequency (rf) plasmas fed with hexafluoroethane (C₂F₆), octafluoropropane (C₃F₈), or octafluorocyclobutane (C₄F₈). The effects of feed gases used, discharge pressure, rf power, substrate positions and discharge modes (pulsed or cw) on the deposited films are examined. Film properties are determined using X-ray photoelectron spectroscopy, atomic force microscopy, and static contact angle measurements. The contact angles of FC films are well related to their compositions and structures. Feed gases used, discharge pressure, rf power, substrate positions and discharge modes strongly affect the morphology of the resulting film, as revealed by atomic force microscopy. Optical emission spectrometry measurements were performed to in-situ characterize the gas-phase compositions of the plasmas and radicals’ emission intensities during film deposition. Correlations between film properties, gas-phase plasma diagnostic data, and film growth processes were discussed. The film growth in pulsed or downstream plasmas was controlled by the surface migration of radicals, such as CF₂ towards nucleation centers, which result in the deposition of FC films with less cross-linked nature and rougher surfaces. These results demonstrate that it is possible to control film compositions and surface structure by changing deposition parameters.     

Study of inductively coupled Cl2/BCl3 plasma process for high etch rate selective etching of via-holes in GaAs

We have investigated the selective etching of 50 μm diameter via-holes for etch depth >200 μm using 30 μm thick photo resist mask in Inductively Coupled Plasma system with Cl₂/BCl₃ chemistry. Resultant etch rate/etch profiles are studied as a function of ICP process parameters and photo resist mask sidewall profile. Etch yield and aspect ratio variation with process pressure and substrate bias is also investigated at constant ICP power. The etch yield of ICP process increased with pressure due to reactant limited etch mechanism and reached a maximum of ∼19 for 200 μm depth at 50 mTorr pressure, 950 W coil power, 80 W substrate bias with an etch rate ∼4.9 μm/min. Final aspect ratio of etched holes is increased with pressure from 1.02 at 20 mTorr to 1.38 at 40 mTorr respectively for fixed etch time and then decreased to 1.24 at 50 mTorr pressure. The resultant final etch profile and undercut is found to have a strong dependence on the initial slope of photo resist mask sidewall angle and its selectivity in the pressure range of 20-50mTorr.     

基于ICP工艺的垂直微小硅镜的加工

利用自感应耦合等离子(ICP)蚀刻机进行硅深层反应离子刻蚀,得到了几微米宽的狭槽,其轮廓通常为正锥形,即蚀刻槽的宽度随着蚀刻深度的增大而减小.然而,对一个宽槽来说,由于等离子区内边界层的变形,其蚀刻宽度会随着蚀刻深度的增加而增加.在许多应用中,硅蚀刻轮廓侧面的垂直状况是一个关键性问题.叙述了分离式垂直镜的加工过程;研究了影响蚀刻轮廓的各种重要参数.经过引入多步制法与优化激励源、基底偏压源及加工压力,减小了等离子区边界层内的变形,改善了轮廓的蚀刻状况.得到的结果为:120μm高垂直微镜垂直度为89.7°,200μm高垂直微镜垂直度为89.3°.     

Chemical and biological characteristics of low-temperature plasma treated ultra-high molecular weight polyethylene for biomedical applications

Several low-temperature radio-frequency (RF) plasma surface treatments were performed on ultra-high molecular weight polyethylene (UHMWPE) used in biomedical applications. Process gases included Ar, C₃F₆, CH₄, hexamethyldisiloxane (HMDSO), and NH₄. These treatments were carried out at pressures in the range of 64–400 mTorr, RF powers of 240–1200 W, and temperatures well below the melting point of UHMWPE. X-ray photoelectron spectroscopy (XPS) was used to obtain information about the surface characteristics of UHMWPE treated with the HMDSO, C₃F₆, and CH₄ gases as a function of treatment conditions. XPS spectra of UHMWPE treated with C₃F₆ and CH₄ and exposed to a laboratory environment for different time periods were examined in order to assess the stability of these treatments. It was found that for the C₃F₆ process gas the amount of fluorine at the surface decreased over time, whereas the oxygen content of the CH₄ treated samples increased as a function of time. In vitro cytotoxicity of Ar, C₃F₆, CH₄, and NH₄ plasma treated samples was studied in light of 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl tetrazolium bromide (MTT) test results. The hemolytic nature of the various plasma treatments was evaluated using standard hemolysis tests. All of the samples tested in this study exhibited no cytotoxic and negligible hemolytic effects. The process parameters for several low-temperature plasma treatments demonstrating chemical and structural stability and good biocompatibility are discussed in conjunction with the broad applicability to other biomedical polymers. © 2001 Kluwer Academic Publishers     

Surface roughness of silicon carbide etching in a NF3 inductively coupled plasma

Silicon carbide was etched in a NF₃/CH₄ inductively coupled plasma. Surface roughness measured by atomic force microscopy was investigated as a function of process parameters. Both etch rate and dc bias were correlated to the surface roughness. To optimize the surface roughness, a 2⁴ full factorial experiment was conducted for 700-900 W source power, 50-150 W bias power, 0.80-1.60 Pa, and 20-100% NF₃ percentage. Main effect analysis revealed that the surface roughness is the most strongly affected by the bias power. For variations in the bias power or NF₃ percentage, decrease in the surface roughness was observed only as positive variations in the etch rate and dc bias are considerably large. The surface roughness with the pressure was chemically dominated as illustrated by its inverse relationship with the dc bias. For the variations in the NF₃ percentage, the radical variation was estimated to play a more dominant role. The smoothest surface roughness of 0.312 nm was obtained at 700 W source power, 150 W bias power, 1.60 Pa pressure, and 100% NF₃ percentage.     

Electrical properties of ITO/benzylated cyclodextrins (-CDs (Bz))/Al diode structures

Investigations of the electrical characteristics of benzylated cyclodextrins (β-CDs (Bz)) diodes are reported. We present current–voltage characteristics and impedance spectroscopy measurements performed on partially benzylated cyclodextrins β-CDs (Bz) thin films in sandwich structures ITO/β-CDs (Bz)/Al. The static electrical characterizations show a space charge limited conduction (SCLC) and a conductivity with power low frequency behavior characteristic of a hopping transport in disordered materials. The impedance spectra can be discussed in terms of an equivalent circuit model designed as a parallel resistor R_P and capacitor C_P network in series with resistor R_S. We extract numerical values of these parameters by fitting experimental data. Their evolution with bias voltages has shown that the SCLC mechanism is characterized by an exponential trap distribution. We estimated from the capacitance voltage characteristic an acceptor concentration of about due to trap states.     

Atomic force microscopy indentation of fluorocarbon thin films fabricated by plasma enhanced chemical deposition at low radio frequency power

Atomic force microscopy (AFM) indentation technique is used for characterization of mechanical properties of fluorocarbon (CF_x) thin films obtained from C₄F₈ gas by plasma enhanced chemical vapour deposition at low r.f. power (5-30 W) and d.c. bias potential (10-80 V). This particular deposition method renders films with good hydrophobic property and high plastic compliance. Commercially available AFM probes with stiff cantilevers (10-20 N/m) and silicon sharpened tips (tip radius < 10 nm) are used for indentations and imaging of the resulted indentation imprints. Force depth curves and imprint characteristics are used for determination of film hardness, elasticity modulus and plasticity index. The measurements show that the decrease of the discharge power results in deposition of films with decreased hardness and stiffness and increased plasticity index. Nanolithography based on AFM indentation is demonstrated on thin films (thickness of 40 nm) with good plastic compliance.     

High-rate deposition and mechanical properties of SiOx film at low temperature by plasma enhanced chemical vapor deposition with the dual frequencies ultra high frequency and high frequency

A high efficiency, high-rate deposition process was developed for silicon oxide films using plasma enhanced chemical vapor deposition (PECVD) with an additional ultra high frequency (UHF) power with high frequency (HF) bias. The effect of the UHF input power with HF bias on the anti-scratch properties of the silicon oxide films was examined. The hybrid plasma process was also examined by advanced plasma source. Dissociation of the octamethylycyclodisiloxane (OMCTS) precursor was controlled by the plasma processing parameters. SiO_x films were deposited on polycarbonate substrates by PECVD using OMCTS and oxygen carrier gas. The rate of SiO_x film deposition increased with increasing input energy. The plasma was analyzed by optical emission spectroscopy. The deposition rate was characterized using an alpha-step. The mechanical properties of the coatings were examined using a nano-indenter and pencil hardness measurements. The chemical properties of the coatings were examined by Fourier transform infrared spectroscopy. The deposition rate of the SiO_x films was controlled by the dissociation of OMCTS using the appropriate intensity of excited neutrals, ionized atoms and input UHF input power with HF bias at room temperature.