Thermal stability of ultrathin amorphous carbon films synthesized by plasma-enhanced chemical vapor deposition and filtered cathodic vacuum arc

Abstract

Ultrathin hydrogenated amorphous carbon (a-C:H) films deposited by plasma-enhanced chemical vapor deposition (PECVD) and hydrogen-free amorphous carbon (a-C) films of similar thickness deposited by filtered cathodic vacuum arc (FCVA) were subjected to rapid thermal annealing (RTA). Cross-sectional transmission electron microscopy (TEM) and electron energy loss spectroscopy (EELS) were used to study the structural stability of the films. While RTA increased the thickness of the intermixing layer and decreased the sp³ content of the a-C:H films, it did not affect the thickness or the sp³ content of the a-C films. The superior structural stability of the FCVA a-C films compared with PECVD a-C:H films, demonstrated by the TEM and EELS results of this study, illustrates the high potential of these films as protective overcoats in applications where rapid heating is critical to the device functionality and performance, such as heat-assisted magnetic recording.     

Deposition of thick and adherent Teflon-like coating on industrial scale stainless steel shell using pulsed dc and RF PECVD

A unique combination of pulsed dc and radio frequency (RF) discharge deposition was used to deposit thick (∼5 μm) and adherent (2-4 MPa) Teflon-like coatings on a stainless steel (SS) shell of 2 m diameter size, through plasma enhanced chemical vapor deposition (PECVD). The details of deposition on such a big industrial scale component are reported for the first time. In this method, highly adherent thin interface layers were grown on SS shell that was electrically grounded, using pulsed dc discharge, followed by RF discharge deposition to build up the required coating thickness. The fluorocarbon precursor molecules, required for the deposition of Teflon-like coating, are generated indigenously by pyrolyzing the Teflon powder. The deposited coating was studied for its chemical bond state, surface roughness (Ra), morphology, thickness, and adhesive strength. These studies were carried out by using XPS, AFM, SEM, etc. The adhesive strength of the coating was measured by pin-pull test as per ASTM D4541 standard test. The coatings deposited with pulsed dc discharge were observed to have higher adhesive strength when compared with those deposited with RF discharge.     

Radio frequency plasma enhanced chemical vapor based ZnO thin film deposition on glass substrate: A novel approach towards antibacterial agent

In the present study, the structural, optical and antibacterial properties of ZnO thin films are reported. ZnO thin films are deposited on borosilicate glass substrates by radio frequency plasma enhanced chemical vapor deposition (PECVD) using oxygen as process gas. The crystallinity of the deposited films is improved upon annealing at 450 °C in air for 1.5 h and the polycrystalline nature of the films is further confirmed by selected area electron diffraction. The particle size of the annealed film (thickness 476 nm) is found to be ∼34 nm from the transmission electron microscopic observation. Energy dispersive X-ray spectrum indicates the stoichiometric deposition of ZnO films. The films are highly transparent (transmittance >85%) in the visible region of electromagnetic spectrum. The films exhibit excellent antibacterial effect towards the growth of Escherichia coli and Pseudomonas aeruginosa.     

GaSb基PECVD法制备SiO2薄膜的应力研究

为了实现在GaSb衬底上获得低应力的SiO₂薄膜,研究了等离子体增强化学气相沉积法（PECVD）在晶格失配较大的GaSb衬底上沉积SiO₂薄膜的应力情况。通过改变薄膜沉积时的工艺条件,如反应温度、射频功率、反应压强、气体流量比,并基于曲率法模型,对镀膜前后的曲率半径进行了实验测量,利用Stoney公式计算相关应力值并绘制应力变化曲线。详细讨论了PECVD工艺条件的改变对SiO₂薄膜应力所产生的影响。同时通过在Si衬底上沉积SiO₂薄膜,对比分析了导致薄膜应力产生的因素及变化过程。实验结果表明,在沉积温度为300℃、射频功率为20 W、腔体压强为90 Pa、气体流量比SiH₄/N₂O为125/70 cm³·min^-1的工艺参数下,PECVD法在GaSb衬底上沉积的SiO₂薄膜应力相对较小。     

多腔耦合微波表面波PECVD法沉积 DLC薄膜研究

报道了利用多腔耦合微波表面波等离子体增强化学气相沉积(PECVD)的方法制备类金刚石(DLC)薄膜。通过发射光谱(OES)测量,对Ar等离子体中的各种放电参数以及全部四个腔室内放电的均匀性作出评估。采用表面轮廓仪测量了薄膜的厚度;薄膜的表面形貌、组成结构通过原子力显微镜(AFM)、激光拉曼光谱和X射线衍射光谱(XPS)进行了表征。在12.5μm厚度的有机薄膜聚酯(PET)表面沉积一定厚度DLC后,通过测量水蒸气透过率(WVTR)对DLC薄膜的阻隔性能进行了研究。结果表明,这种多腔耦合微波表面波等离子体装置,不仅能够实现四个腔室同时相对均匀的放电,也能够实现单个腔室的轴向均匀放电。制备的DLC薄膜结构致密、成分均匀,可以使PET薄膜阻隔性能提高约20倍。     

21.0%‐efficient co‐diffused screen printed n‐type silicon solar cell with rear‐side boron emitter

Plasma enhanced chemical vapor deposition (PECVD) is applied to deposit boron silicate glasses (BSG) acting as boron diffusion source during the fabrication of n‐type silicon solar cells. We characterize the resulting boron‐diffused emitter after boron drive‐in from PECVD BSG by measuring the sheet resistances R_sheet,B and saturation current densities J_0,B. For process optimization, we vary the PECVD deposition parameters such as the gas flows of the precursor gases silane and diborane and the PECVD BSG layer thickness. We find an optimum gas flow ratio of SiH₄/B₂H₆= 8% and layer thickness of 40 nm. After boron drive in from these PECVD BSG diffusion sources, a low J_0,B values of 21 fA/cm² is reached for R_sheet,B = 70 Ω/□. The optimized PECVD BSG layers together with a co‐diffusion process are implemented into the fabrication process of passivated emitter and rear totally diffused (PERT) back junction (BJ) cells on n‐type silicon. An independently confirmed energy conversion efficiency of 21.0% is achieved on 15.6 × 15.6 cm² cell area with a simplified process flow. This is the highest efficiency reported for a co‐diffused n‐type PERT BJ cell using PECVD BSG as diffusion source. A loss analysis shows a small contribution of 0.13 mW/cm² of the boron diffusion to the recombination loss proving the high quality of this diffusion source. (© 2016 WILEY‐VCH Verlag GmbH &Co. KGaA, Weinheim)     

Surface passivation of crystalline silicon by sputter deposited hydrogenated amorphous silicon

This letter shows that intrinsic hydrogenated amorphous silicon (a‐Si:H) films deposited by RF magnetron sputtering can provide outstanding passivation of crystalline silicon surfaces, similar to that achieved by plasma enhanced chemical vapour deposition (PECVD). By using a 2% hydrogen and 98% argon gas mixture as the plasma source, 1.5 Ω cm n‐type FZ silicon wafers coated with sputtered a‐Si:H films achieved an effective lifetime of 3.5 ms, comparable to the 3 ms achieved by PECVD (RF and microwave dual‐mode). This is despite the fact that Fourier transform infrared spectroscopy measurements show that sputtering and PECVD deposited films have very different chemical bonding configurations. We have found that film thickness and deposition temperature have a significant impact on the passivation results. Self‐annealing and hydrogen plasma treatment during deposition are likely driving forces for the observed changes in surface passivation. These experimental results open the way for the application of sputtered a‐Si:H to silicon heterojunction solar cells. (© 2014 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Thin zirconium nitride films prepared by plasma-enhanced CVD

Thin films of zirconium nitride have been deposited at temperatures as low as 573 K by PECVD using tetrakis(diethylamido)zirconium, Zr[N(C₂H₅)₂]₄ as precursor. The influence of the various experimental parameters on film properties and deposition rates has been studied. Under most experimental conditions hard coatings of good adherence and low carbon contamination resulted.     

Investigation of surface cleaning procedure of InP:S (1 0 0) substrates by high resolution XPS

The angle resolved X-ray photoelectron spectroscopy measurements were used to monitor a level of contamination of the InP:S (1 0 0) substrates during the cleaning processes with deionized water and isopropanol. Some contaminations with carbon and oxygen were found for a broken under ultrahigh vacuum InP:S substrate, indicating the contamination of the crystal during the growth process. The substrates after cleaning with deionized water and isopropanol were contaminated with carbon, oxygen, nitrogen and silicon. Concentration of carbon decreases inwards the substrates while concentration of oxygen is enhanced even in the deeper layers for both processes. The nitrogen concentration is higher for the samples rinsed with water. Roughness of the surfaces is higher for the samples rinsed with water what indicated the AFM measurements.     

Analysis of a hollow-cathode reflex discharge in a hydrocarbon flow

Variation of parameters of a reflex discharge with a hollow cathode operating continuously in propane with a flow rate of 1.3–5.6 (m³ mPa)/s and a discharge current of 0.1–0.4 A is analyzed. It is shown that for a hydrocarbon flow rate of 2.4 (m³ mPa)/s and higher, an increase in the discharge voltage takes place after a time interval depending on the discharge current and gas pressure; this is explained by the formation of coating of the dissociation products of hydrocarbon molecules on the electrodes of the discharge chamber. An increase in the thickness of the carbon coating of the cathodes with time and their charging with ions lead to electric breakdown of coatings and the formation of cathode spots. The oscillograms of the discharge current and voltage indicate a short-term transformation of the glow discharge into the arc discharge. The energy spectra of ions emerging from the discharge are measured, and the effect of the discharge current and the gas flow rate on the energy spread of ions is analyzed. The operation time of the discharge in hydrocarbon after which the cleaning of the discharge chamber is required is determined. The possibility of using an ion source based on the reflex discharge with a hollow cathode for technological purposes is established.     

Optical,structural, and photocatalytic properties of the nanosized titanium dioxide films deposited in magnetron discharge plasma

The conditions of the optimum and controlled deposition of titanium dioxide nanolayers in the cylindrical gas discharge plasma of a magnetron having a unique design are found and described. The examination of the grown films by Raman spectroscopy is used to determine the conditions of deposition of the amorphous and polycrystalline phases of titanium dioxide. The films deposited on a cold substrate are amorphous, and the films deposited on a heated substrate consist of polycrystalline anatase. The evolution of the spectral lines of argon, oxygen, and titanium and the discharge voltage drop are studied as a function of the magnitude and the direction of changing the discharge current. The results obtained are shown to be applied for contactless optical monitoring. The refractive index of the films n is shown to have a nonlinear dependence on the layer thickness, and the layers that have a high photocatalytic activity and can be used to remove inorganic pollutants from the environment are shown to be grown.     

A point source analytical model of inverse pulsed laser deposition

A simple analytical model for inverse pulsed laser deposition is proposed. In the model the motion of the evaporated material is assumed to emerge as from a point source located above the surface of evaporation at some distance. The obtained thickness profiles of inverse deposited films agree well with those calculated by the test particle Monte Carlo method. The proposed approach has been applied for analysis of experimental data on inverse pulsed laser deposition of graphite in nitrogen atmosphere with nanosecond pulses of laser fluences between 1 and 7 J/cm². The model describes well the thickness profiles and pressure dependence of film growth rate for inverse deposition.     

Deposition of plasma-polymerized acetylene by an intense pulsed RFplasma source

An inductively coupled, intense, pulsed RF plasma source deposited plasma-polymerized acetylene at a rate of 127 Å per discharge. The potassium bromide substrate was located 18-cm downstream from the RF coil. A puff valve admitted parent acetylene gas just before the transient RF current was applied. Fourier transform infrared (FTIR) spectra showed that carbon-to-carbon double bonds were formed. Scanning-electron-microscope images showed that the film thickness after 79 discharges was 1 μm. A photodiode showed substantial light emission for about 30 μs during each discharge     

椭偏透射法测量氢化非晶硅薄膜厚度和光学参数

针对多角度椭偏测量透明基片上薄膜厚度和光学参数时基片背面非相干反射光的影响问题,报道了利用椭偏透射谱测量等离子增强化学气相沉积法(PECVD)制备的a-Si:H薄膜厚度和光学参数的方法,分析了基片温度T_s和辉光放电前气体温度T_g的影响.研究表明,用椭偏透射法测量的a-Si:H薄膜厚度值与扫描电镜(SEM)测得的值相当,推导得到的光学参数与其他研究者得到的结果一致.该方法可用于生长在透明基片上的其他非晶或多晶薄膜. 关键词： 椭偏测量 透射法 光学参数 氢化非晶硅薄膜     

用锌有机源和CO2/H2混合气源PECVD沉积ZnO薄膜

在等离子体作用下,以CO2/H2混合气为氧源,Zn(C2H5)2锌为锌源,在单晶硅上生长出高度择优取向的氧化锌薄膜。X射线衍射分析表明,薄膜为六方结构,c轴高度择优;原子力显微镜观察到晶粒是有规律地按六方排布,薄膜的表面粗糙度较小;从光致发光谱还发现在380 nm处有非常强的紫外峰。     

应用于ICF实验的软X射线平面镜反射率

在北京同步辐射装置上,通过对应用于惯性约束聚变（ICF）实验的平面镜反射率的进一步研究,提高了辐射温度的测量精度。进行了对软X射线平面镜反射率的测量、反射镜的清洗、反射率的模拟计算,证明影响反射率变化的主要因素是平面镜的安装角度和沾污。实验结果表明:平面镜的沾污主要来源于ICF实验中的油沾污,采用射频辉光放电清洗非常有效。     

气相合成SnO2超微粒薄膜研究

用直流气体放电活化反应蒸发法在玻璃基片上沉积的SnO2超微粒薄膜,研究其过程中各工艺参数对薄膜结构的影响及作用机理,结果表明,SnO2超微粒薄膜粒径随氧分压增加而增大;蒸镀时间的延长有助于SnO2的生成,也使薄膜发生晶化;而增加放电电压,则薄膜出现外延单晶生长趋势。     

On the macroparticle flux from vacuum arc cathode spots

The macroparticle contamination of vacuum-arc-deposited thin films generated by a plasma source with an optional axial magnetic field is studied. Emphasis is placed on the macroparticle flux near the discharge axis. The arc current, metal species, deposition system geometry and axial magnetic field strength are varied. Distribution functions for macroparticles of Pb, Ag, Cu, Pt, W, and Ni are determined, normalized to the film thickness deposited or the charge transferred. The application of the axial magnetic field leads to a considerable reduction of the normalized macroparticle flux since the plasma is effectively focused by the field, whereas the macroparticle production is not influenced. The macroparticle content normalized to the deposited film thickness is reduced to about 20-35% of that without an additional magnetic field     

Mass transport characteristics in a pulsed plasma enhanced chemicalvapor deposition reactor for thin polymer film deposition

A pulsed plasma enhanced chemical vapor deposition (PECVD) reactor is used for the preparation of thin polyacetylene films. A theoretical model based on the mass transport characteristics of the reactor is developed in order to correlate with experimentally obtained spatial deposition profiles for the acetylene plasma polymer film deposited within the cylindrical reactor. Utilizing a free radical mechanism with gas phase initiation of the polymerization reaction as the rate controlling step, a system parametric study is performed to predict the Peclet number range of operation for the pulsed PECVD reactor. This parametric study indicates radical decay by diffusion to the reactor walls to be the significant physical phenomenon in the system. It is concluded that a quasi-steady-state model is a good tool for predicting the important mass transfer phenomena occurring in the pulsed plasma reactor     

Study of the composition and properties of protective layers formed by the ion-beam-assisted deposition of cadmium,zinc, and aluminum onto steel surfaces

Layers formed by the ion-beam-assisted deposition of cadmium, zinc, and aluminum onto the surface of carbon and stainless steels to protect aluminum and its alloys from corrosion in the case of their contact with steel parts are investigated. The protective layers are created via ion-beam-assisted deposition, in which metal deposition and mixing of the deposited layer with the substrate surface (this process is implemented by accelerated (U = 5 kV) ions of the same metal) occurs, respectively, from a neutral vapor fraction and the vacuum arc plasma of a pulsed electric-arc ion source. The morphology and composition of the generated surface layers are studied by means of scanning electron microscopy, electron-probe microanalysis, and Rutherford backscattering spectrometry. The layer composition is revealed to include atoms of the deposited metal, the substrate material, oxygen, and carbon. The layer thickness varies from ~50 to 80 nm, and the deposited metal content of the layers is ~(1.0–3.5) × 10¹⁷ atom/cm². Corrosion tests of the aluminum and its alloy in contact with the materials under study confirm the efficiency of the ion-beam modification of steel surfaces.