Plasma Diagnosis for Microwave ECR Plasma Enhanced Sputtering Deposition of DLC Films

Application of the Langmuir probe in plasma circumstance for deposition of diamond-like carbon(DLC) thin films usually faces the problem of rapid failure of the probe due to surface insulative coating.In this paper,we circumvent the problem by using the floating harmonic probe technique.In the real circumstance of DLC film deposition,the floating harmonic probe worked reliably over 3 hours,correctly indicating the ion density and electron temperature.The technique was practically used to measure the ion density and electron temperature in DLC film deposition processes using the microwave ECR plasma enhanced sputtering.Combined with the Raman spectroscopic characterization of the films,the conditions for deposition of DLC films were investigated.     

A Study of Diamond-Like Carbon Thin Films Prepared by Microwave Plasma Chemical Vapour Deposition

In order to deposit good films, we need to study the uniformity of plasma density and the plasma density under different gas pressures and powers. The plasma density was diagnosed by a Langmuir probe. The optical emission spectroscopy （OES） of CH4 and H2 discharge was obtained with raster spectroscopy, with characteristic peaks of H and CH achieved. Diamond-like carbon films were achieved based on the study of plasma density and OES and characterized by atomic force microscope （AFM）, X-ray diffraction instrument （XRD）, Raman spectroscope and profiler.     

磁控溅射沉积U薄膜性能研究

采用X射线光电子能谱仪(XPS)和扫描透射电镜(STEM)分析了在Al薄膜基材上磁控溅射沉积U薄膜的表面形貌、组织和结构;分别采用排代法、霍美尔(T20S)粗糙度测量仪测量了薄膜的密度和表面粗糙度.结果表明溅射沉积的U薄膜由金属U和少量UO2组成,薄膜结构属微晶和无定形态,密度是块材密度的(75±5)%,表面粗糙度小于0.3 μm.     

Structure and Tribology Property of Carbon Nitride Films Deposited by MW-ECR Plasma Enhanced Unbalanced Magnetron Sputtering

Carbon nitride films were deposited by a twinned microwave electron cyclotron resonance （ECR） plasma source enhanced unbalanced magnetron sputtering system. The results indicate that the structure of the films is sensitive to the nitrogen content. The increase in the nitrogen flow ratio leads to an increase in the sp3 content and an improvement of the tribological properties.     

Microstructure,Hardness and Corrosion Resistance of ZrN Films Prepared by Inductively Coupled Plasma Enhanced RF Magnetron Sputtering

ZrN fihns were deposited on Si（111） and M2 steel by inductively coupled plasma （ICP）-enhanced RF magnetron sputtering. The effect of ICP power on the microstructure, mechanical properties and corrosion resistance of ZrN films was investigated. When the ICP power is below 300 W, the ZrN films show a columnar structure. With the increase of ICP power, the texture coefficient （To） of the （111） plane, the nanohardness and elastic modulus of the films increase and reach the maximum at a power of 300 W. As the ICP Power exceeds 300 W, the films exhibit a ZrN and ZrNx mixed crystal structure without columnar grain while the nanohardness and elastic modulus of the films decrease. All the ZrN coated samples show a higher corrosion resistance than that of the bare M2 steel substrate in 3.5% NaCl electrolyte. The nanohardness and elastic modulus mostly depend on the crystalline structure and Tc of ZrN（111）.     

Effect of Power and Nitrogen Content on the Deposition of CrN Films by Using Pulsed DC Magnetron Sputtering Plasma

CrN thin films are deposited on stainless steel (AISI-304) substrate using pulsed DC magnetron sputtering in a mixture of nitrogen and argon plasma. Two set of samples are prepared. The first set of sample is treated at different powers (100 W to 200 W) in a mixture of argon (95%) and nitrogen (5%). The second set of samples is treated at different nitrogen concentrations (5% to 20%) in argon (95% to 80%) for a constant power (150 W). X-ray diffraction (XRD) analysis exhibits the development of new phases related to different compounds. The crystallinity of CrN varies by varying the applied power and nitrogen content. Crystallite size and residual stresses of the CrN (111) plane show similar variation for the applied power and nitrogen contents. Scanning electron microscopy (SEM) analysis shows the formation of a granular surface morphology that varies with the change of powers and nitrogen content. The thickness of the film is measured using SEM cross sectional images and using atomic force microscopy (AFM) scratch analysis. The maximum film thickness (about 755 nm) is obtained for the film deposited at 5% nitrogen in 95% argon at 150 W power. For these conditions, maximum hardness is also observed.     

Study on the Hydrogenated Diamond-Like Carbon Films Synthesized by RF-PECVD from n-decane

Using a mixture of n-decane and hydrogen, diamond-like carbon thin films (DLCTFs) with high growth rate of 35?nm/min are deposited by radio frequency plasma enhanced chemical vapor deposition. We show that n-decane can be considered as a promising carbon source in DLCTF deposition. The properties of the deposited films such as structure, hydrogen content, deposition rate and refractive index are studied for 20, 50 and 100?sccm hydrogen flow rates (HFRs). It is shown that the deposition rate has a maximum of 35?nm/min for HFR?=?20?sccm and by increasing hydrogen concentration, deposition rate drops to 19?nm/min for HFR?=?100?sccm. The Raman spectra reveal that the films represent hydrogenated diamond-like carbon features. The photoluminescence background of the Raman spectra is used as a measure for hydrogen content of the films. The hydrogen content varies from 29 to 46% which yields a various amount of sp³ fraction. The results of the spectroscopic ellipsometry indicate that by increasing HFR, refractive index decreases from 2.1 to 1.9 at 632?nm. The aforementioned trends are attributed to the increase of hydrogen content in DLCTFs which is in very good agreement with enhancing of the photoluminescence background of the Raman spectra.     

Microstructure and Mechanical Properties of CrN Films Deposited by Inductively Coupled Plasma Enhanced Radio Frequency Magnetron Sputtering

CrN films have been synthesized on Si（100） wafer by inductively coupled plasma （ICP）-enhanced radio frequency （RF） magnetron sputtering. The effects of ICP power on microstructure, crystal orientation, nanohardness and stress of the CrN films have been investigated. With the increase of ICP power, the current density at substrate increases and the films exhibit denser structure, while the DC self-bias of target and the deposition rate of films decrease. The films change from crystal structure to amorphous structure with the increase of ICP power. The measured nanohardness and the compressive stress of films reach the topmost at ICP power of 150 W and 200 W, respectively. The mechanical properties of films show strong dependence on the crystalline structure and the density influenced by the ICP power.     

溅射功率对磁控溅射制备Bi薄膜结构和性能的影响

采用直流磁控溅射方法在不同功率下制备了铋(Bi)薄膜,对薄膜的沉积速率、表面形貌、生长模式、晶体结构进行了研究,并对其晶粒尺寸和应力的变化规律进行了分析。扫描电镜(SEM)图像显示：薄膜均为柱状生长,平均晶粒尺寸随溅射功率先增大后减小,薄膜的致密度随着功率的增加而降低,在60W时又变得较致密。X射线衍射(XRD)结果表明：Bi薄膜均为多晶斜六方结构,薄膜内应力随功率的增加由张应力变为压应力。     

Physical Properties of Titanium Oxide Thin Films Prepared by DC Magnetron Sputtering: Influence Substrate Temperature and O2/Ar in the Gas Mixture

Titanium oxide thin film compounds were grown on p-type Si (100) and BK7 glass as substrate using reactive DC magnetron sputtering. The effect of temperature growth on structural, optical and morphological properties was investigated. By means of X-ray diffraction (XRD) the phase composition was characterized. UV–Vis-NIR spectroscopy was used for reflection and transmission measurements of deposited thin film layers. Atomic force microscopy was used to evaluate and compute the surface roughness changes for different temperatures growth. The XRD results show that the temperature growth effects on the phase formation and structure. Increasing the substrate growth temperature would result in change of film thickness due to different phase and structure formation. The calculated band gap from optical measurements of the thin films shows a decrease at higher substrate temperature growth.     

Synthesis of Diamond-Like Carbon Films Using Hot Filament-Aided Microwave Plasma Chemical Vapor Deposition

1. IntroductionDiamond-like carbon (DLC) films have receivedconsiderable attention recently because their inher-ent properties such aJs hardness, thermal conductiv-ity and electrical resistance are excellent and closeto those of a diamond. The DLC films have beenprepared by a variety of methods, for instance, radiofrequency (RF) plasma deposition [l], ion beam de-position [2] and electron cyclotron resonance (ECR)chemical vapor deposition [3]. As sllrface wave dis-charges [4] have advanta…     

Influence of Nitrogen on Hydrogenated Amorphous Carbon Thin Films Deposited by Plasma Focus Device

To carry out our research, a plasma focus device is used to deposit thin films of nitrogen doped hydrogenated amorphous carbon (a-C:H:N) onto the stainless steel-AISI-304 substrates at room temperature. Thin films are deposited with the same numbers of focus shots, at the same distance from the anode tip and with different partial pressures of nitrogen in the mixtures of acetylene/nitrogen as working gas. The nitrogen contents of deposited films are studied using nuclear reaction analysis (NRA) techniques. The results prove that nitrogen contents of the samples do not increase significantly by increasing partial pressure of nitrogen of the working gas for both sets of the samples. Moreover, NRA results exhibit the limitation of nitrogen incorporated into the samples, when this experimental setup is used. G-peak position and peak intensity ratio of the D-band to G-band (I_D/I_G) are used to investigate the diamond characters. Also, they show that sp² clustering is highly dependent on the nitrogen atomic contents and angular position of the samples. Scanning electron microscopy (SEM) shows the granular surface morphology of the films. Furthermore, it shows that angular position of the samples with respect to the anode axis plays an important role in the grain size of the surface of the samples. The thickness of the films decreases significantly by increasing angular position of the samples, while it decreases slightly by increasing partial pressure of nitrogen of the working gas. The Vickers surface hardness of the thin films exhibits significant dependency on the sp² clustering.     

Effect of N2-Gas Partial Pressure on the Structure and Properties of Copper Nitride Films by DC Reactive Magnetron Sputtering

Copper nitride thin films were deposited on glass substrates by reactive direct current （DC） magnetron sputtering at various N2-gas partial pressures and room temperature. Xray diffraction measurements showed that the films were composed of Cu3N crystallites and exhibited a preferential orientation of the [111] direction at a low nitrogen gas （N2） partial pressure. The film growth preferred the [111] and the [100] direction at a high N2 partial pressure. Such preferential film growth is interpreted as being due to the variation in the Copper （Cu） nitrification rate with the N2 pressure. The N2 partial pressure affects not only the crystal structure of the film but also the deposition rate and the resistivity of the Cu3N film. In our experiment, the deposition rate of Cu3N films was 18 nm/min to 30 nm/min and increased with the N2 partial pressure. The resistivity of the Cu3N films increased sharply with the increasing N2 partial pressure. At a low N2 partial pressure, the Cu3N films showed a metallic conduction mechanism through the Cu path, and at a high N2 partial pressure, the conductivity of the Cu3N films showed a semiconductor conduction mechanism.     

Effect of Gas Sources on the Deposition of Nano-Crystalline Diamond Films Prepared by Microwave Plasma Enhanced Chemical Vapor Deposition

Nano-crystalline diamond (NCD) films were deposited on silicon substrates by a microwave plasma enhanced chemical vapor deposition (MPCVD) reactor in C2H5OH/H2 and CH4/H2/O2 systems, respectively, with a constant ratio of carbon/hydrogen/oxygen. By means of atomic force microscopy (AFM) and X-ray diffraction (XRD), it was shown that the NCD films deposited in the C2H5OH/H2 system possesses more uniform surface than that deposited in the CH4/H2/O2 system. Results from micro-Raman spectroscopy revealed that the quality of the NCD films was different even though the plasmas in the two systems contain exactly the same proportion of elements. In order to explain this phenomenon, the bond energy of forming OH groups, energy distraction in plasma and the deposition process of NCD films were studied. The experimental results and discussion indicate that for a same ratio of carbon/hydrogen/oxygen, the C2H5OH/H2 plasma was beneficial to deposit high quality NCD films with smaller average grain size and lower surface roughness.     

In vitro Cyto and Blood Compatibility of Titanium Containing Diamond-Like Carbon Prepared by Hybrid Sputtering Method

In recent years,diamond-like carbon films (DLC) have been given more attention in research in the biomedical industry due to their potential application as surface coating on biomedical materials such as metals and polymer substrates.There are many ways to prepare metal containing DLC films deposited on polymeric film substrates,such as coatings from car-bonaceous precursors and some means that incorporate other elements.In this study,we in-vestigated both the surface and biocompatible properties of titanium containing DLC (Ti-DLC) films.The Ti-DLC films were prepared on the surface of poly (ethylene terephthalate) (PET) film as a function of the deposition power level using reactive sputtering technique.The films’ hydrophilicity was studied by contact angle and surface energy tests.Their surface morphology was studied by scanning electron microscopy (SEM) and atomic force microscopy (AFM).Their elemental chemical composition was analyzed using energy dispersive X-spectra (EDX) and X-ray photoelectron spectroscopy (XPS).Their blood and cell compatibility was studied by in vitro tests,including tests on platelet adhesion,thrombus formation,whole blood clotting time and osteoblast cell compatibility.Significant changes in the morphological and chemical composition of the Ti-DLC films were observed and found to be a function of the deposition level.These morphological and chemical changes reduced the interfacial tension between Ti-DLC and blood proteins as well as resisted the adhesion and activation of platelets on the surface of the Ti-DLC films.The cell compatibility results exhibited significant growth of osteoblast cells on the surface of Ti incorporated DLC film compared with that of DLC film surface.     

合金化对溅射Ti膜材结构和力学性能的影响

研究了直流磁控溅射Ti、TiMo、TiMoY及TiMoYAl薄膜的形貌、结构和力学性能,探讨了合金化对Ti膜的影响。结果表明,合金化使Ti膜由α相结构转变为α+β双相结构,改变了薄膜的择优取向,降低了薄膜表面粗糙度,并改善了薄膜的力学性能。     

磁控溅射制备金属铀膜

研究了通过磁控溅射方法制备高纯金属铀膜的可行性。采用X射线衍射（XRD）、俄歇电子能谱（AES）、扫描电镜（SEM）、表面轮廓仪分析了沉积在单晶硅或金基材上铀薄膜的微观结构、成分、界面结构及厚度、表面形貌和表面粗糙度。分析结果表明：磁控溅射制备的铀薄膜为纯金属态,氧含量和其它杂质含量均低于俄歇电子能谱仪的探测下限;溅射沉积的铀镀层与铝镀层之间存在界面作用,两者相互扩散并形成合金相,扩散层厚度约为10nm。铀薄膜厚度可达微米级,表面光洁,均方根（RMS）粗糙度优于15nm。     

Physical Properties of Silver Oxide Thin Film Prepared by DC Magnetron Sputtering: Effect of Oxygen Partial Pressure During Growth

In this paper the physical properties of silver oxide thin film have been prepared on BK7 substrate at room temperature by reactive DC magnetron sputtering technique using pure silver metal target by varying oxygen partial pressure during growth at reported. The reactive sputter gas was a mixture of Ar (99.999%) and N₂ (99.999%) with the different ratio Ar and N₂ by volume at the constant pressure of the growth chamber. The X-ray diffraction measurements showed that by increasing O₂ volume during the Growth, change in crystalline structure will occur. The Atomic Force Microscope images shown by increasing O₂ volume, the RMS roughness decreasing consistently. The thickness of the thin films decreases (from 353 to 230 nm) with increasing oxygen partial pressure in chamber. The reflectivity of thin films was investigated with a spectrophotometer system, and the surface reflectivity measurements indicate that by increasing O₂ volume growth, the optical properties of the films changes.     

Optical Characterization of Amorphous Hydrogenated Carbon(a-C:H)Thin Films Prepared by Single RF Plasma Method

Methane(CH4) plasma was used to produce amorphous hydrogenated carbon(aC:H) films by a single capacitively coupled radio frequency(RF) powered plasma system.The system consists of two parallel electrodes:the upper electrode is connected to 13.56 MHz RF power and the lower one is connected to the ground.Thin films were deposited on glass slides with different sizes and on silicon wafers.The influence of the plasma species on film characteristics was studied by changing the plasma parameters.The changes of plasma species during the deposition were investigated by optical emission spectroscopy(OES).The structural and optical properties were analyzed via Fourier transform infrared(FTIR) spectroscopy,X-ray diffraction(XRD) and UV-visible spectroscopy,and the thicknesses of the samples were measured by a profilometer.The sp~3/sp~2 ratio and the existing H atoms play a significant role in the determination of the chemical properties of thin films in the plasma.The film quality and deposition rate were both increased by raising the power and the flow rate.