高能氮离子轰击对四面体非晶碳膜的表面改性和摩擦系数影响的研究

利用过滤阴极真空电弧技术制备了sp³键含量不小于80%的四面体非晶碳(ta-C)膜.利用冷阴极潘宁离子源产生不同能量的氮离子对制备的ta-C薄膜进行轰击,通过X射线光电子能谱和原子力显微镜对薄膜表面结构与形貌进行分析研究.研究表明,随着氮离子的轰击能量的增大,薄膜中的CN键结构略有增大,形成了轻N掺杂;同时,在薄膜表层发生了sp³键结构向sp²键结构的转化;薄膜的表面粗糙度在经过氮离子轰击后从0.2 nm减小至0.18 nm,然后随着轰击能 关键词： 四面体非晶碳 X射线光电子能谱 摩擦系数     

氮离子轰击能量对ta-C:N薄膜结构的影响

利用磁过滤真空阴极电弧技术制备了sp³键含量不小于80%的四面体非晶碳薄膜(ta-C), 然后通过氮离子束改性技术制备了氮掺杂的四面体非晶碳(ta-C:N)薄膜. 利用Raman光谱和X射线光电子能谱对薄膜结构的分析,研究了氮离子轰击能量对ta-C:N薄膜结构的影响. 氮离子对ta-C薄膜的轰击,形成了氮掺杂的ta-C:N薄膜. 氮离子轰击诱导了薄膜中sp³键向sp²键转化, 以及CN键的形成.在ta-C:N薄膜中,氮掺杂的深度和浓度随着氮离子能量的增大而增大. ta-C:N薄膜中sp²键的含量和sp²键团簇的尺寸随着氮离子轰击能量的增大而增加; 在ta-C:N薄膜中, CN键主要由C-N键和C＝N键构成, C-N 键的含量随着氮离子轰击能量的增大而减小,但是C＝N 键含量随着氮离子轰击能量的增大而增大.在ta-C:N薄膜中不含有C≡N键结构.     

磁过滤器电流对非晶碳薄膜摩擦学特性影响的研究

研究了过滤阴极真空电弧技术中,不同的磁过滤器电流下(5—13 A),制备的四面体非晶碳(ta-C)薄膜对摩擦学特性的影响.通过对薄膜厚度,薄膜结构以及薄膜表面粗糙度随磁过滤电流的变化结果进行了测试,结果表明,随着磁过滤器电流的增大,薄膜的sp³键含量逐渐减少,表面粗糙度从0.13增大到0.38.磁过滤器电流在5 A时,薄膜的摩擦系数最小约为0.08,当电流增大到7 A时,摩擦系数显著增大,磁过滤器电流从7 A增大到13 A时,薄膜的摩擦系数再次减小约为0.1. 关键词： 四面体非晶碳 过滤阴极真空电弧 磁过滤器电流 摩擦系数     

氮对类金刚石薄膜的微观结构内应力与附着力的影响

采用原子力显微镜(AFM)、俄歇电子能谱(AES)和显微压痕分析等手段对射频等离子体增强化学气相沉积法制备的掺氮类金刚石(DLC：N)薄膜的微观结构和力学性能进行了研究.结果表明,随着含氮量的增加,DLC薄膜的AFM表面形貌中出现了几十纳米的颗粒,原子侧向力显微镜和AES分析表明这种纳米颗粒是x大于0.126的非晶氮化碳CN_x结构.这种非晶DLC/CN_x的纳米复合结构,减小了薄膜的内应力,从而提高了薄膜与衬底的附着力. 关键词： 类金刚石碳膜 微观结构 附着特性     

基底表面纳米织构对非晶四面体碳膜结构和摩擦特性的影响研究

本文利用离子束表面改性技术对基底表面进行不同时间的轰击, 形成不同规则的纳米织构, 对不同织构的变化规律进行了研究, 同时, 利用磁过滤真空阴极电弧技术, 在具有不同纳米织构的各基底上沉积相同时间的四面体非晶碳薄膜. 采用原子力显微镜对各基底的织构进行形貌分析, 结果表明, 高能粒子束的轰击对基底表面形貌有较大的影响, 根据离子束轰击时间的不同, 可以在基底表面形成各种不同规则的纳米织构, 轰击15 min后发现基底表面形成点阵纳米织构, 之后随着时间的增加, 基本维持点阵结构. 通过X射线光电子能谱仪和摩擦磨损试验仪对沉积在具有不同织构的基底上的ta-C薄膜进行测试, 研究表明, 基底表面纳米织构的非晶层结构引起薄膜内部sp³键的含量降低, 释放了薄膜的内应力, 同时发现基底表面纳米织构将ta-C薄膜磨损时间从不足10 min提高到约70 min, 有效提高了薄膜的耐磨性.     

椭偏法表征四面体非晶碳薄膜的化学键结构

采用自主研制的双弯曲磁过滤阴极真空电弧(FCVA)技术,在不同衬底负偏压下制备了四面体非晶碳(ta-C)薄膜。通过分光光度计和椭偏(SE)联用技术精确测量了薄膜厚度,重点采用椭偏法对不同偏压下制备的ta-C薄膜sp3 C键和sp2 C键结构进行了拟合表征,并与X射线光电子能谱(XPS)和拉曼光谱的实验结果相对比,分析了非晶碳结构的椭偏拟合新方法可靠性。结果表明,在-100V偏压时薄膜厚度最小,为33.9nm;随着偏压的增加,薄膜中的sp2 C含量增加,sp3 C含量减小,光学带隙下降。对比结果发现,椭偏法作为一种无损、简易、快速的表征方法,可用于ta-C薄膜中sp2 C键和sp3 C键含量的准确测定,且在采用玻璃碳代表纯sp2 C的光学常数及拟合波长选取250～1700nm时的椭偏拟合条件下,拟合数值最佳。     

氩离子轰击对四面体非晶碳膜内应力和摩擦系数影响的研究

利用磁过滤真空阴极电弧技术制备了sp³键大于80%的四面体非晶碳(ta-C)薄膜, 通过冷阴极离子源产生keV能量的氩离子轰击ta-C薄膜,研究了氩离子轰击能量对ta-C薄膜结构, 内应力以及耐磨性的影响.通过X射线光电子能谱和原子力显微镜研究了氩离子轰击对薄膜结构 与表面形貌的改性,研究表明,氩离子轰击诱导了ta-C薄膜中sp³键向sp²键的转化, 并且随着氩离子轰击能量的增大,薄膜中sp²键的含量逐渐增多, 薄膜内应力随着氩离子轰击能量的增大逐渐减小.氩离子轰击对薄膜的表面形貌有较大影响, 在薄膜表面形成刻蚀坑,并且改变了薄膜的表面粗糙度,随着氩离子轰击能量的增大, 薄膜的表面粗糙度也会逐渐增大.通过摩擦磨损仪的测试结果,氩离子轰击对薄膜的初始摩擦系数影响较大, 但是对薄膜的稳定摩擦系数影响较小,经过氩离子轰击前后的ta-C薄膜的摩擦系数为0.1左右, 并且具有优异的耐磨性.     

硼掺杂对四面体非晶碳膜电导性能的影响

以单质硼和高纯石墨的混合粉末压制成型的靶材作为靶源,采用过滤阴极真空电弧技术制备不同硼含量的掺硼四面体非晶碳膜.分别采用四探针法、阻抗分析仪和电化学界面对薄膜的变温电导率、I-V特性和C-V特性进行了测试和研究.实验结果表明,当B含量由0增加至6.04 at%时,薄膜的室温电导率先逐渐增大而后逐渐减小,相应薄膜的电导激活能先逐渐减小而后逐渐增大,并在2.13 at%时分别出现最大和最小值1.42×10^-7S/cm和0.1eV.此外,掺硼四面体非晶碳/n型硅异质结的I-V曲线表现出典型的整流特性,表明p-n结二极管已经形成,且结两端的掺杂能级在空间上连续统一. 关键词： 四面体非晶碳 电导率 I-V曲线')" href="#">I-V曲线 C-V曲线')" href="#">C-V曲线     

不同能级加速过滤电弧沉积四面体非晶碳膜的结构和性能

采用过滤阴极真空电弧技术，通过施加0—2000 V衬底负偏压使沉积离子获得不同能级的入射能量，在单晶硅上制备了四面体非晶碳薄膜.拉曼光谱分析表明，薄膜的结构为非晶sp³骨架中镶嵌着平面关联长度小于1 nm的sp²团簇.原子力显微镜研究表明：在低能级、富sp³能量窗口和次高能级，薄膜中sp³的含量越多，其表面就越光滑，应用sp³浅注入生长机制能够圆满地解释薄膜表面形态与离子入射能量之间的关系；但在高 关键词： 四面体非晶碳 过滤阴极真空电弧 能级     

退火对AlTiN多层薄膜结构及力学性能影响

使用TiAl合金靶,利用中频反应磁控溅射系统,通过交替改变氮气流量的方法,在高速钢(W18Cr4V)基体上沉积了一组氮含量周期性改变的AlTiN多层薄膜,并分别在600,700和800 ℃下真空退火热处理. 利用X射线衍射仪、场发射扫描电镜和高分辨透射电镜等方法研究了沉积态和退火态AlTiN多层薄膜组织和微观结构;AlTiN多层薄膜的力学和膜基结合性能用纳米压痕硬度仪、摩擦磨损仪以及划痕试验仪得到. 研究表明,采用沉积过程中周期改变氮气流量的方法,可以制备出稳定的、力学性能良好的AlTiN多层薄膜. 80 关键词： AlTiN多层薄膜 退火 微观结构 力学性能     

Effect of ECR-assisted microwave plasma nitriding treatment on the microstructure characteristics of FCVA deposited ultra-thin ta-C films for high-density magnetic storage applications

There are higher technical requirements for protecting layer of magnetic heads and disks used in future high-density storage fields. In this paper, ultra-thin (2 nm thickness) tetrahedral amorphous carbon (ta-C) films were firstly prepared by filtered cathodic vacuum arc (FCVA) method, then a series of nitriding treatments were performed with nitrogen plasma generated using electron cyclotron resonance (ECR) microwave source. Here it highlighted the influence of nitrogen flow and applied substrate bias voltage on the structural characteristics of ta-C films during the plasma nitriding process. The chemical compositions, element depth distribution profiles, physical structures and bonding configurations of plasma-nitrided ta-C films were investigated by X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES) and UV-vis Raman spectroscopy. The experimental results show that the carbon nitride compounds (CN_x) are formed in nitrogenated ta-C films in which the N content and its depth distribution depends on bias voltage to large extent rather than N₂ flow. The N content of nitrogenated ta-C films can reach 16 at.% for a substrate bias of −300 V and a N₂ flow of 90 sccm. With increasing nitrogen content, there is less G peak dispersion and more ordering of structure. Furthermore, appropriate nitriding treatment (substrate bias: −100 V, N₂ flow: 150 sccm) can greatly increase the fraction of sp³ and sp³C-N bonds, but the values begin to fall when the N content is above 9.8 at.%. All these indicate that suitable ECR-assisted microwave plasma nitriding is a potential modification method to obtain ultra-thin ta-C films with higher sp³ and sp³C-N fractions for high-density magnetic storage applications.     

Effect of cathodic arc PVD parameters on roughness of TiN coating on steel substrate

Titanium nitride which is widely used as a hard coating material was coated on tool steel, by physical vapor deposition method. Surface roughness was investigated as a function of deposition rate, substrate bias and temperature, nitrogen flow rate and metal ion etching. The study showed that increase in surface roughness mainly depends on the condition of sample preparation, surface treatment, macro-droplets, pitting defects, rise in compressive stress at higher coating thickness, growth defects and to a lesser extent selection of surface under testing. It was observed that chromium ion etching significantly reduced the surface roughness compared to titanium ion etching.     

The preparation and evaluation of graded multilayer ta-C films deposited by FCVA method

In this study, a series of graded multilayer ta-C films were investigated by varying their sublayer thickness ratios, in which each film sublayer was prepared at different substrate bias by filtered cathode vacuum arc (FCVA) method. The experimental results show that the graded multilayer film structure can effectively decrease the internal stress level of deposited ta-C film, and meanwhile the graded multilayer ta-C films still have high sp³ fractions. The applied substrate bias voltage and sublayer thickness ratio can apparently influence the microstructure characteristics and internal stress of the graded multilayer ta-C films. The graded multilayer ta-C film has larger sp³ fraction when applying a larger negative substrate bias voltage and having a thicker outer sublayer during the film deposition process. However, the internal stress in the as-deposited film also increases with larger thickness of the outer sublayer, and the optimal ratio of sublayer thicknesses is 1:1:1:1 for graded ta-C film with four sublayers.     

The influence of compressive stress applied by hard coatings on the power loss of grain oriented electrical steel sheet

To reduce the core loss of electrical steel the vacuum arc ion plating technique has been used to deposit titanium nitride (TiN) layers on highly grain oriented electrical steel sheets. The layer thickness, the stresses of layers and coated sheets and the achieved reduction in core losses have been measured as functions of coating duration and applied bias voltage. Well adhered layers with high compressive stress up to 6.8 GPa have been produced. With increasing bias voltage the layer thickness decreases and the intrinsic stress of the layers increase. A further increase of bias voltage leads to a drop in stress due to thermal relaxation. In general, the tensile stress of the coated sheets rises with increasing layer thickness while the core loss of the coated material decreases with increasing tensile stress of the steel sheet and increasing bias voltage. The highest reduction of core loss has been found to be 28% (from P_1.7=0.86 W/kg for commercially coated HGO electrical steel sheet with glass film to 0.62 W/kg for TiN coated material) and is due to the reduction of excess loss only.     

Fabrication and characteristics of ta-C biomaterial coatings on Ti–6Al–4V using metal plasma immersion ion implantation and deposition

We have formed amorphous diamond (ta-C) coatings on Ti–6Al–4V substrates using a metal plasma immersion ion implantation and deposition (MEPIIID) technique, and characterized the mechanical properties and biological compatibility of the coating material. The hemocompatibility of the coating compared favorably with that of low temperature isotropic (LTI) carbon, with kinetic clotting time and hemolysis rate approximately the same as for LTI carbon, and platelet consumption about twice that of the latter. The mechanical properties were good, with a microhardness greater than that of the uncoated metal substrates, and high adhesion of >0.75 GPa (interface shear stress) as estimated from a thermal quench method. Glancing-angle X-ray diffraction measurements indicated the presence of a TiC transition layer, suggesting the formation of a Ti/TiC/ta-C multilayer structure, leading in turn to good film–substrate adhesion. We conclude that this kind of amorphous diamond coating could provide benefit as a biocompatible hard coating for Ti–6Al–4V substrate material.     

非晶金刚石薄膜的X射线反射研究

利用过滤阴极真空电弧系统制备了不同衬底偏压下非晶金刚石薄膜,分别采用X射线反射法测定了相应的非晶金刚石膜密度,分析了薄膜密度与沉积能量之间的变化规律．建立了薄膜密度随衬底偏压的变化曲线。研究发现在-80V时非晶金刚石膜密度存在最大值3．26g／cm^2,随着偏压的增大和减小,薄膜的密度都相应的下降;当衬底偏压加到-2000V时,密度减小到2．63g／cm^2,相对于密度的最大值变化较小。通过薄膜sp^3能态杂化含量与密度的简单比例关系,近似推算出非晶金刚石膜中sp^3能态的含量最高可达80％以上。     

Tribological characterization of chromium nitride coating deposited by filtered cathodic vacuum arc

CrN coatings were prepared by filtered cathodic vacuum arc (FCVA) technique. The influence of the deposition parameters (nitrogen partial pressure PN₂, substrate bias voltage V_s and preheating of the substrate) on the structural, mechanical and tribological properties of the FCVA CrN coatings was investigated. Further, the FCVA CrN coating was compared in dry reciprocating sliding with commercial multi-arc ion plating (MAIP) CrN coating as to friction and wear properties. Profilometer, scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDX) were used to evaluate the wear scars and the wear mechanisms were discussed. The results showed that the structural, mechanical and tribological properties of the FCVA CrN coatings were significantly dependent on the deposition parameters. The FCVA CrN coating deposited with PN₂ of 0.1 Pa, V_s of −100 V and without preheating exhibited the optimal mechanical and tribological properties. The FCVA CrN coating exhibited much better anti-abrasive and anti-spalling properties than the MAIP CrN coating, which was resulted from significant reduction of macroparticles and pitting defects by the FCVA technique. The MAIP CrN coating suffered severe concentrated wear by a combination wear mechanisms of delamination, abrasive and oxidative wear when high normal load was applied, while for the FCVA CrN coating the wear mechanisms were ultra-mild abrasive and oxidative wear.     

Stress, microstructure and mechanical properties of graded multilayer tetrahedral amorphous carbon films

Tetrahedral amorphous carbon (ta-C) films deposited using a filtered cathodic vacuum arc (FCVA) system, have high intrinsic stress which limits their application as protective coatings. To reduce the film stress and to improve the adhesion, a multilayer structure is deposited at a gradient substrate negative bias from 1500 V to 80 V. This paper investigates the stress, microstructure and nano-mechanical properties of graded multilayer ta-C film on Si substrates. Compared with that of single-layer films deposited at optimised bias, the graded multilayer film has low stress without a decline in hardness and Young’s modulus. Microstructural evaluation of the multilayer film using visible Raman spectra shows that the average content of the sp³ bonds of the multilayer film remain at a high level. Nanoscratch testing illustrates favorable scratch resistance and good adhesion of the multilayer film. Scanning electron microscope (SEM) observation confirms the collapse of the film surface along the scratching trace. Finally, deposition on single crystal germanium substrates of a durable coating ∼ 1100 nm thick, and composed of three graded multilayer films is demonstrated. PACS 81.05.Uw; 81.15.Jj; 68.65.Ac; 68.55.Nq; 68.60.Bs     

Structural and mechanical properties of compositionally gradient CrNx coatings prepared by arc ion plating

Compositionally gradient CrN_x coatings were fabricated using arc ion plating by gradually increasing N₂ flow rate during the deposition process. The effect of substrate bias, ranging from 0 to −250 V, on film microstructure and mechanical properties were systematically investigated with XRD, SEM, HRTEM, nanoindentation, adhesion and wear tests. The results show that substrate bias has an important influence on film microstructure and mechanical properties of gradient CrN_x coatings. The coatings mainly crystallized in the mixture of hexagonal Cr₂N, bcc Cr and fcc rock-salt CrN phases. N₂ flow rate change during deposition results in phase changes in order of Cr, Cr + Cr₂N, Cr₂N, Cr₂N + CrN, and CrN, respectively, along thickness direction. Phase fraction and preferred orientation in CrN_x coatings vary with substrate bias, exerting an effective influence on film hardness. With the increasing of bias, film microstructure evolves from an apparent columnar structure to a highly dense one. The maximum hardness of 39.1 GPa was obtained for the coatings deposited at a bias of −50 V with a friction coefficient of 0.55. It was also found that adhesion property and wear resistance of gradient CrN_x coatings were better than that of homogeneous CrN coatings.     

Coating of Cr-V ledeburitic steel with CrN containing a small addition of Ag

Samples made from Vanadis 6 PM ledeburitic tool steel were surface machined, ground, and mirror polished. They were heat treated and coated with CrN with and without Ag addition by reactive magnetron sputtering. The CrN film grew in a typically columnar manner. A small addition of 3% Ag did not lead to alterations in the growth mechanism. The hardness of the CrN coating was 16.79 ± 1.49 GPa compared to 15.97 ± 1.44 GPa for the coating with Ag addition. The Ag addition in the CrN improved adhesion of the coating, which can be attributed to the capability of CrAgN coating to accommodate higher deformation energy before failure. The CrAgN coating exhibited superior tribological properties at intermediate temperatures. Compared to pure CrN the friction coefficient is lowered to 70-75% when measured at 400 and 500 °C, respectively. This is reflected in a reduction in the volume wear, which was found to be three times lower for the coating containing Ag. Flexural strength decreased slightly for the CrN- or CrAgN-coated material compared to uncoated steel. However, as the decrease in flexural strength is very weak there is practically no risk of significant embrittlement of the investigated material due to the CrN coating with or without Ag addition.