Diamond-Like Carbon Depositing on the Surface of Polylactide Membrane for Prevention of Adhesion Formation During Tendon Repair

Post-traumatic peritendinous adhesion presents a significant challenge in clinical medicine.This study proposes the use of diamond-like carbon(DLC)deposited on polylactic acid(PLA)membranes as a biophysical mechanism for anti-adhesion barrier to encase ruptured tendons in tendon-injured rats.The results indicate that PLA/DLC composite membrane exhibits more efficient anti-adhesion effect than PLA membrane,with histological score decreasing from 3.12±0.27 to 2.20±0.22 and anti-adhesion effectiveness increasing from 21.61%to 44.72%.Mechanistically,the abundant C=O bond functional groups on the surface of DLC can reduce reactive oxygen species level effectively;thus,the phosphorylation of NF-κB and M1 polarization of macrophages are inhibited.Consequently,excessive inflammatory response augmented by M1 macrophage-originated cytokines including interleukin-6(IL-6),interleukin-1β(IL-1β),and tumor necrosis factor-α(TNF-α)is largely reduced.For biocompatibility evaluation,PLA/DLC membrane is slowly absorbed within tissue and displays prolonged barrier effects compared to traditional PLA membranes.Further studies show the DLC depositing decelerates the release of degradation product lactic acid and its induction of macrophage M2 polarization by interfering esterase and PLA ester bonds,which further delays the fibrosis process.It was found that the PLA/DLC membrane possess an efficient biophysical mechanism for treatment of peritendinous adhesion.

Studies of diamond-like carbon (DLC) films deposited on stainless steel substrate with Si/SiC intermediate layers

In this work, diamond-like carbon （DLC） films were deposited on stainless steel substrates with Si/SiC intermediate layers by combining plasma enhanced sputtering physical vapour deposition （PEUMS-PVD） and microwave electron cyclotron resonance plasma enhanced chemical vapour deposition （MW-ECRPECVD） techniques. The influence of substrate negative self-bias voltage and Si target power on the structure and nano-mechanical behaviour of the DLC films were investigated by Raman spectroscopy, nano-indentation, and the film structural morphology by atomic force microscopy （AFM）. With the increase of deposition bias voltage, the G band shifted to higher wave-number and the integrated intensity ratio ID/IG increased. We considered these as evidences for the development of graphitization in the films. As the substrate negative self-bias voltage increased, particle bombardment function was enhanced and the sp^3-bond carbon density reducing, resulted in the peak values of hardness （H） and elastic modulus （E）. Silicon addition promoted the formation of sp^3 bonding and reduced the hardness. The incorporated Si atoms substituted sp^2- bond carbon atoms in ring structures, which promoted the formation of sp^3-bond. The structural transition from C-C to C-Si bonds resulted in relaxation of the residual stress which led to the decrease of internal stress and hardness. The results of AFM indicated that the films was dense and homogeneous, the roughness of the films was decreased due to the increase of substrate negative self-bias voltage and the Si target power.

Nanomechanical and Electrochemical Properties of Diamond-Like Carbon (DLC) Films Deposited by Plasma Enhanced Chemical Vapor Deposition (PECVD) Technique

Diamond-like carbon （DLC） films was deposited successfully on stainless steel sub- strates with Si/SiC intermediate layers by combining plasma enhanced unbalanced magnetron sputtering physical vapor deposition （PEUMS-PVD） and microwave electron cyclotron resonance plasma enhanced chemical vapor deposition （MW-ECR PECVD） techniques. The effect of sil- icon dopant on the structure, morphology, nanomechanical properties and electrochemical be- havior of DLC films were investigated by Raman spectroscopy, nano-indentation, atomic force microscopy （AFM） and potentiodynamic method and electrochemical impedance spectroscopy （EIS）. It showed that the incorporated silicon atoms substituted sp2-bonded carbon atoms in the ring structures, promoting the formation of sp3-bonds. The structural transition from C-C to C-Si bonds resulted in the relaxation of the residual stress, leading to the decrease in films hardness. The DLC films with Si/SiC intermediate layers led to significant improvement in the corrosion resistance of the stainless steel substrate due to effective isolation and good chemical inertness of the DLC films.

Electron Injection Enhancement by Diamond-Like Carbon Film in Polymer Electroluminescence Devices

A diamond-like carbon （DLC） film is deposited as an electron injection layer between the polymer light-emitting layer（MEH-PPV） and aluminum （Al） cathode electrode in polymer electroluminescence devices （PLEDs） using a radio frequency plasma deposition system. The source material of the DLC is n-butylamine. The devices consist of indium tin oxide （ITO）/MEH-PPV/DLC/Al. Electron injection properties are investigated through I-V characteristics,and the mechanism of electron injection enhancement due to a thin DLC layer has been studied. It is found that： （1） a DLC layer thinner than 1.0nm leads to a higher turn-on voltage and decreased electroluminescent （EL） efficiency; （2） a 5.0nm DLC layer significantly enhances the electron injection and results in the lowest turn-on voltage and the highest EL efficiency; （3） DLC layer that exceeds 5.0nm results in poor device performance;and（4） EL emission can hardly be detected when the layer exceeds 10.0nm. The properties of ITO/MEH-PPV/DLC/Al and ITO/MEH-PPV/LiF/Al are investigated comparatively.

退火温度对DLC和Si-DLC涂层微观结构和摩擦学性能的影响

类金刚石(DLC)涂层因具有优异的减磨耐摩性能被广泛应用,而涂层内部存在较高的内应力这一缺点限制其在摩擦学领域的进一步应用。退火处理可以通过改变涂层微观结构来降低涂层内应力,从而提高涂层的摩擦学性能。为研究退火温度对DLC和硅掺杂类金刚石(Si-DLC)涂层微观结构和摩擦学性能的影响,采用等离子体增强化学气相沉积(PECVD)和电弧离子镀的复合沉积技术制备DLC和Si-DLC涂层,将涂层在大气环境中进行不同温度的退火处理。运用扫描电子显微镜、高分辨率透射电子显微镜、拉曼光谱以及XPS光谱仪对涂层摩擦试验前后的形貌和结构进行表征,采用纳米压痕仪和摩擦磨损试验机测试涂层的力学性能和摩擦学性能。结果表明:沉积的DLC和Si-DLC涂层为非晶结构。退火温度对涂层的微观结构和摩擦学性能有重要影响。随着退火温度从RT上升到500℃,由于C-H键断裂,C网发生集束化,DLC涂层的sp^(3)含量呈现先上升后降低的趋势,涂层的sp^(3)含量在300℃热处理后获得最大值,涂层硬度达到最大的20.66 GPa;而Si-DLC涂层由于Si元素的掺杂提高了涂层的热稳定性,其在400℃热处理时sp^(3)含量最大,硬度最大值为24.28 GPa。涂层与氧化锆对磨球的磨损机理为磨粒磨损,涂层的磨损率呈现先降低后升高的趋势,热处理温度为300和400℃为最优。研究证明涂层的微观结构和摩擦学性能可以通过热处理温度调控,优选热处理温度的涂层具有优异的综合性能。研究结果可为退火处理对DLC和Si-DLC涂层的性能影响提供理论支持。

Ti-DLC薄膜压阻性能及载流子输运行为研究

围绕压阻传感器领域对高性能类金刚石(Diamond Like Carbon,DLC)薄膜压阻敏感材料的需求,针对金属掺杂DLC存在的载流子输运行为和实际多工况(如温度、湿度等)下压阻性能不明的问题,本工作以Ti-石墨复合拼接靶为靶材,采用高功率脉冲磁控溅射技术,高通量制备出4种Ti含量(原子分数为0.43%~4.11%)的Ti掺杂类金刚石(Ti-DLC)薄膜,研究了Ti含量对薄膜组分结构、电学性能、变湿度环境下压阻性能的影响规律。结果表明:Ti含量(原子分数)在0.43%~4.11%范围内,掺杂Ti原子均以固溶形式均匀镶嵌于非晶碳网络中,Ti-DLC薄膜电学行为表现为典型半导体特性,在200~350 K温度范围内,薄膜电阻率均随温度升高而降低。载流子传导机制在200~270 K内为Mott型三维变程跳跃传导,在270~350 K范围内则为热激活传导。Ti-DLC薄膜压阻系数(Gauge Factor,GF)最大值为95.1,在20%~80%相对湿度范围内,所有样品GF均随湿度增加而增大,这可能是引入的固溶Ti原子缩短了导电相之间的平均距离,同时吸附表面水分子导致电阻变化。

硅氧共掺DLC薄膜的制备及阻隔性能研究

目的研究硅(Si)、氧(O)元素掺杂对类金刚石(Diamond like Carbon,DLC)薄膜沉积、结构、表面形貌以及阻隔性能的影响,为高效制备高阻隔硅氧共掺类金刚石(Si and O Incorporated DLC,Si/O-DLC)薄膜提供新的思路参考。方法利用微波等离子体化学气相沉积(Plasma Enhanced Chemical Vapor Deposition,PECVD)技术在聚对苯二甲酸乙二醇酯(Polyethylene terephthalate,PET)基底表面沉积Si/O-DLC薄膜,具体研究反应单体中六甲基二硅氧烷(Hexaethyldisiloxane,HMDSO)含量对薄膜沉积和阻隔性能的影响。通过台阶仪、傅里叶红外光谱(FTIR)、X射线光电子能谱(XPS)、原子力显微镜(AFM)表征薄膜厚度、结构和微观形貌,并通过测试氧气透过率表征复合薄膜的阻隔性能。结果随着混合气体中HMDSO含量增加,薄膜的沉积速率提高,不同高度位置上沉积速率波动变弱,平均沉积速率最高达到310 nm·min^(–1),同时,薄膜中Si、O元素含量增加,相关的键合结构含量增加,薄膜表面致密性变差,氧气阻隔性能变弱;当HMDSO流量控制在1 mL·min^(–1)时,PET薄膜的氧气透过率可从未涂覆时的132mL·m^(2)·d^(–1)降低至2mL·m^(2)·d^(-1),阻隔性能明显改善。结论在一定工艺条件下,通过微波PECVD技术在PET薄膜表面涂覆Si/O-DLC薄膜,可明显改善其阻隔性能。

Synthesis and Characteristics of Diamond-like Carbon Films Deposited on Quartz Substrate

Diamond-like carbon (DLC) films are deposited on quartz substrate using pure CH4 in the surface wave plasma equipment. A direct current negative bias up to -90 V is applied to the substrate to investigate the bias effect on the film characteristics. Deposited films are characterized by Raman spectroscopy, infrared (IR) and ultraviolet-visible absorption techniques. There are two broad Raman peaks around 1340 cm-1 and 1600 cm-1 and the first one has a greater sp3 component with an increased bias. Infrared spectroscopy has three sp3 C-H modes at 2852 cm-1, 2926 cm-1 and 2962 cm-1, respectively and also shows an intensity increase with the negative bias. Optical band gap is calculated from the ultraviolet-visible absorption spectroscopy and the increased values with negative bias and deposition time are obtained. After a thermal anneal at about 500℃ for an hour to the film deposited under the bias of-90 V, we get an almost unchanged Raman spectrum and a peak intensity-reduced IR signal, which indicates a reduced H-content in the film. Meanwhile the optical band gap changed from 0.85 eV to 1.5 eV.

Micro/Nanomechanical and Tribological Properties of Thin Diamond-Like Carbon Coatings

The diamond-like carbon (DLC) films with different thicknesses on 9Crl8bearing steels were prepared using vacuum magnetic-filtering arc plasma deposition. Vickersindentation, nanoin-dentation and nanoscratch tests were used to characterize the DLC films with awide range of applied loads. Mechanical and tribological behaviors of these submicron films wereinvestigated and interpreted. The hardnesses of 9Cr18 and DLC. determined by nanoindentation, areapproximately 8GPa and 60GPa respectively; their elastic moduli are approximately 250GPa and 600GParespectively. The friction coefficients of 9Cr18, DLC, organic coating, determined by nanoscratch,are approximately 0. 35, 0. 20 and 0. 13 respectively. It is demonstrated that nanoindentation andnanoscratch tests can provide more information about the near-surface elastic-plastic deformation,friction and wear properties. The correlation of mechanical properties and scratch resistance of DLCfilms on 9Cr18 steels can provide an assessment for the load-carrying capacity and wear resistance.

Properties of polydimethylsiloxane hydrophobic modified duplex microarc oxidation/diamond-like carbon coatings on AZ31B Mg alloy

A reliable,high-performance coating procedure was developed using PDMS to modify a duplex MAO/DLC coating on an AZ31B Mg alloy.First,the duplex MAO/DLC coating was fabricated via a combined MAO and unbalanced magnetron sputter process.Subsequently,a PDMS solution was used to modify the MAO/DLC coating via a conventional dip-coating method.The surface characteristics,bond strength,hardness,tribological behaviour,and corrosion resistance of the coated samples were evaluated via SEM,CA,Raman spectroscopy,friction and wear behaviour,polarisation curve,and NSS tests.The PDMS modification reduced the HIT of MAO/DLC coating from 15.96 to 8.34GPa;this is ascribed to the penetration of PDMS,which has good rheological properties to form a viscoelastic Si-based organic polymer layer on the MAO/DLC coating.However,the PDMS-modified MAO/DLC coating was denser,hydrophobic,and had higher bond strength compared with MAO-and MAO/DLC-coated samples.Moreover,the PDMS modification reduced the COF and wear rate of the duplex MAO/DLC coating.This indicates that the PDMS improved the tribological behaviour owing to the transferred Si oxide that originated from the Si-O network of the PDMS,as well as the low graphitisation of the DLC layer during sliding.Furthermore,the corrosion current density of the MAO/DLC-coated sample modified by PDMS for 10min decreased by two order of magnitude compared with that of the MAO/DLC-coated sample but by five orders of magnitude compared with that of the bare substrate.The NSS tests proved that the PDMS layer slowed the corrosion of the Mg alloy under long-term service,enhancing the corrosion protection efficiency.The results are attributed to the high bond strength and lubricant MAO/DLC layer,and the dual role of sealing and hydrophobicity of PDMS.Therefore,PDMS modification is promising for the fabrication of protective materials for Mg alloys that require corrosion and wear resistance.

Corrosion performance and tribological behavior of diamond-like carbon based coating applied on Ni−Al−bronze alloy

The effect of diamond-like carbon(DLC)coating(fabricated by cathodic arc deposition)on mechanical properties,tribological behavior and corrosion performance of the Ni−Al−bronze(NAB)alloy was investigated.Nano-hardness and pin-on-plate test showed that DLC coating had a greater hardness compared with NAB alloy.Besides,the decrease in friction coefficient from 0.2 for NAB substrate to 0.13 for the DLC-coated sample was observed.Potentiodynamic polarization and EIS results showed that the corrosion current density decreased from 2.5μA/cm2 for bare NAB alloy to 0.14μA/cm2 for DLC-coated sample in 3.5 wt.%NaCl solution.Moreover,the charge transfer resistance at the substrate−electrolyte interface increased from 3.3 kΩ·cm2 for NAB alloy to 120.8 kΩ·cm2 for DLC-coated alloy,which indicated an increase in corrosion resistance due to the DLC coating.

Preparation of Diamond-like Carbon Films on the Surface of Ti Alloy by Electro-deposition

In this paper, diamond-like carbon (DLC) films were deposited on Ti alloy by electro-deposition. DLC films were brown andcomposed of the compact grains whose diameter was about 400 nm. Examined by XPS, the main composition of the filmswas carbon. In the Raman spectrum, there were a broad peak at 1350 cm^(-1) and a broad peak at 1600 cm^(-1), which indicatedthat the films were DLC films.

Effect of N-ion implantation and diamond-like carbon coating on fretting wear behaviors of Ti6Al7Nb in artificial saliva

The tribology behaviors of Ti6Al7Nb,its alloy with N-ion implantation,and its alloy with diamond-like carbon(DLC)coating were investigated in artificial saliva.Fretting wear tests of untreated,N-ion implanted and DLC coated Ti6Al7Nb alloys plate against a Si3N4ball were carried out on a reciprocating sliding fretting wear test rig.Based on the analysis of X-ray diffraction,Raman spectroscopy,3-D profiler,SEM morphologies and frictional kinetics behavior analysis,the damage behavior of surface modification layer was discussed in detail.The results indicated that the fretting wear behavior of Ti6Al7Nb alloy with N-ion implantation was increased with the dose increase of the implanted nitrogen ions.Moreover,the DLC-coated Ti6Al7Nb alloy with low ion implantation could improve the fretting wear behavior greatly.In addition,the Ti6Al7Nb with DLC coating had better ncorrosion resistance due to the special compact structure.All results suggested that the Ti6Al7Nb with DLC coating had better wear resistance than that with N-ion implantation in artificial saliva.

Deposition of Diamond-Like Carbon on Inner Surface by Hollow Cathode Discharge

A cylindrical hollow cathode discharge （HCD） in CH4/Ar gas mixture at pressure of 20-30 Pa was used to deposit diamond-like carbon （DLC） films on the inner surface of a stainless steel tube. The characteristics of the HCD including the voltage-current curves, the plasma im- ages and the optical emission spectrum （OES） were measured in Ar and CHn/Ar mixtures. The properties of DLC films prepared under different conditions were analyzed by means of Raman spectroscopy and scanning electron microscopy （SEM）. The results show that the electron exci- tation temperature of HCD plasma is about 2400 K. DLC films can be deposited on the inner surface of tubes. The ratio of sp3/sp2 bonds decreases with the applied voltage and the deposition time. The optimizing CH4 content was found to be around CH4/Ar =1/5 for good quality of DLC films in the present system.

Tribological properties of diamond-like carbon films deposited bv pulsed laser arc deposition

A novel method, pulsed laser arc deposition combining the advantages of pulsed laser deposition and cathode vacuum arc techniques, was used to deposit the diamond-like carbon （DLC） nanofilms with different thicknesses. Spectroscopic ellipsometer, Auger electron spectroscopy, x-ray photoelectron spectroscopy, Raman spectroscopy, atomic force microscopy, scanning electron microscopy and multi-functional friction and wear tester were employed to investigate the physical and tribological properties of the deposited films. The results show that the deposited films are amorphous and the sp2, sp3 and C-O bonds at the top surface of the films are identified. The Raman peak intensity and surface roughness increase with increasing film thickness. Friction coefficients are about 0.1, 0.15, 0.18, when the film thicknesses are in the range of 17-21 nm, 30-57 nm, 67-123 nm, respectively. This is attributed to the united effects of substrate and surface roughness. The wear mechanism of DLC films is mainly abrasive wear when film thickness is in the range of 17-41 nm, while it transforms to abrasive and adhesive wear, when the film thickness lies between 72 and 123 nm.

Influence of Microwave Power on the Properties of Hydrogenated Diamond-Like Carbon Films Prepared by ECR Plasma Enhanced DC Magnetron Sputtering

Electron cyclotron resonance （ECR） plasma was applied to enhance the direct current magnetron sputtering to prepare hydrogenated diamond-like carbon （H-DLC） films. For different microwave powers, both argon and hydrogen gas are introduced separately as the ECR working gas to investigate the influence of microwave power on the microstructure and electrical property of the H-DLC films deposited on P-type silicon substrates. A series of characterization methods including the Raman spectrum and atomic force microscopy are used. Results show that, within a certain range, the increase in microwave power affects the properties of the thin films, namely the sp3 ratio, the hardness, the nanoparticle size and the resistivity all increase while the roughness decreases with the increase in microwave power. The maximum of resistivity amounts to 1.1×10^9 Ω.cm. At the same time it is found that the influence of microwave power on the properties of H-DLC films is more pronounced when argon gas is applied as the ECR working gas, compared to hydrogen gas.

Structures of Diamond-Like Carbon Films

The structures of diamond-like carbon （DLC） films, including a-C：H, a-C, ta-C：H and ta-C films have been investigated as a random covalent network with a dense film structure. The results show that sp2 C in a-C：H and a-C films tends to form olefinic and aromatic groups while sp^3 C in ta-C：H and ta-C films tends to form single or multiple sixfold groups. The hydrogen atoms in hydrogenated DLC films contribute to stabilizing the carbon skeletal networks. The film structures are well related to their properties such as optical gaps, density and hardness. The results also indicate that the high density and the extreme hardness of ta-C films are attributed to the forming of large sp^3 C bonded sixfold groups.

Structure and Mechanical Performance of Nitrogen Doped Diamond-like Carbon Films

Nitrogen doped diamond-like carbon （DLC：N） films were prepared by electron cyclotron resonance chemical vapor deposition （ECR-CVD） on polycrystalline Si chips. Film thickness is about 50 nm. Auger electron spectroscopy （AES） was used to evaluate nitrogen content, and increasing N2 flow improved N content from 0 to 7.6%. Raman and X-ray photoelectron spectroscopy （XPS） analysis results reveal CN-sp^3C and N-sp^2C structure. With increasing the N2 flow, sp^3C decreases from 73.74% down to 42.66%, and so does N-sp^3C from 68.04% down to 20.23%. The hardness decreases from 29.18 GPa down to 19.74 GPa, and the Young＇s modulus from 193.03 GPa down to 144.52 GPa.

Fabrication of Diamond-like Carbon Films by Ion Assisted Middle Frequency Unbalanced Magnetron Sputtering

Diamond-like carbon （DLC） films are deposited by the Hall ion source assisted by the mid-frequency unbalanced magnetron sputtering technique. The effects of the substrate voltage bias, the substrate temperature, the Hall discharging current and the argon/nitrogen ratio on the DLC film＇s performance were studied. The experimental results show that the film＇s surface roughness, the hardness and the Young＇s modulus increase firstly and then decrease with the bias voltage incrementally increases. Also when the substrate temperature rises, the surface roughness of the film varies slightly, but its hardness and Young＇s modulus firstly increase followed by a sharp decrease when the temperature surpassing 120 ℃. With the Hall discharging current incrementally rising, the hardness and Young＇s modulus of the film decrease and the surface roughness of the film on 316L stainless steel firstly decreased and then remains constant.

Improvement of Thermal Stability and Tribological Performance of Diamond-Like Carbon Composite Thin Films

Diamond-like carbon (DLC) is a metastable amorphous film that exhibits unique properties. However, many limitations exist regarding the use of DLC, for example, its tribological characteristics at high temperature, as well as its limited thermal stability. In this study, silicon/oxygen and silicon/nitrogen co-incorporated diamond-like carbon (Si-O-DLC and Si-N-DLC) films are studied, taking into account the thermal stability and tribological performance of these films compared with pure DLC. All the films were prepared on Si wafers, WC-Co materials, and aluminum foils using a plasma-based ion implantation (PBII) technique using acetylene (C2H2), tetramethylsilane (TMS, Si(CH3)4), oxygen (O2) and nitrogen (N2) as plasma sources. The structure of the films was characterized using Raman spectroscopy. The thermal stability of the films was measured using thermogravimetric and differential thermal analysis (TG-DTA). The friction coefficient of the films was assessed using ball-on-disk friction testing. The results indicate that Si-N-DLC films present better thermal stability due to the presence of Si-O networks in the films. The Si-N-DLC (23 at.%Si, 8 at.%N) film was affected using thermal annealing in an air atmosphere with increasing temperature until 500°C. The film can also resist thermal shock by cycling 10 times between the various temperatures and air atmosphere until 500°C. Further, Si-O-DLC and Si-N-DLC films exhibit excellent tribological performance, especially the Si-N-DLC (23 at.%Si, 8 at.%N) film, which exhibits excellent tribological performance at 500°C in an air atmosphere. It is concluded that Si-O-DLC and Si-N-DLC films improve upon the thermal stability and tribological performance of DLC.