磁控溅射制备Ti-Si-N纳米薄膜的摩擦磨损性能

采用磁控溅射方法在1Cr18Ni9Ti不锈钢基体上沉积Ti-Si-N纳米薄膜。结果发现：随着Si含量增加，薄膜的晶粒尺寸逐渐变小，晶粒尺寸范围在3nm～20nm之间。薄膜的显微硬度相对于TiN有明显增加，最大硬度可达43．5GPa。Si元素的加入亦改善了膜基结合强度。同时发现，Ti-Si-N纳米薄膜的摩擦系数和比磨损率随着Si含量的增加先减小后增加，其高温摩擦系数明显低干常温，但比磨损率却有显著提高。     

Ti-Si-N纳米复合薄膜的结构与性能

用工业型脉冲直流等离子体增强化学气相沉积技术,在高速钢(W18Cr4V)表面沉积了Ti-Si-N复合薄膜,研究了Ti-Si-N复合薄膜的微观组织和力学性能.结果显示,薄膜相结构为纳米晶TiN和纳米晶或非晶TiSi2以及非晶相Si3N4;在Si含量为5.0 at%～28.0 at%范围内,薄膜的晶粒尺寸逐渐变大;Ti-Si-N薄膜的显微硬度相对于TiN有明显增加,最高硬度可达40 GPa;高温退火后,Ti-Si-N纳米复合薄膜的显微硬度与晶粒尺寸在800℃高温下仍然保持稳定.     

低能量离子束辐照磁控溅射沉积超硬质nc-TiN/nc-Cu纳米复合膜

利用诱导型等离子体辅助双靶磁控溅射法在Si（100）基板表面沉积Cu含量（原子分数）为0～10．0％的Ti—Cu—N膜,研究了Cu含量对薄膜结构及硬度的影响．结果表明,添加少量Cu可极大地提高薄膜硬度．Cu含量为2．0％的Ti—Cu—N薄膜具有超硬特性,硬度HV达到42,约为纯TiN薄膜硬度的2倍．超硬质Ti—Cu—N薄膜为nc-TiN／nc—Cu纳米复合薄膜,具有柱状晶结构．薄膜的超硬特性源于薄膜的纳米复合结构．     

PCVD制备新型Ti-Si-C-N纳米复合超硬薄膜及其微观结构表征

用脉冲直流等离子体增强化学气相沉积（PCVD）方法,在高速钢试样表面沉积出一种新型Ti-Si-C-N薄膜材料.研究了不同SiCl4流量对薄膜成分、微观组织形貌以及薄膜晶体结构的影响.X射线衍射（XRD）、X射线光电子能谱（XPS）、透射电子显微镜（TEM）和扫描电子显微镜（SEM）分析结果表明：Ti-Si-C-N薄膜是由Ti（C,N）/a-C/a-Si3N4组成的纳米复合结构,薄膜的晶粒尺寸在2-25 nm范围内;当Ti-Si-C-N薄膜中N含量很少时,Ti（C,N）结构转变为TiC,薄膜的表面形貌由颗粒状转变为粗条状.     

脉冲直流PCVD制备新型Ti-Si-C-N纳米复合超硬薄膜

用工业型脉冲直流等离子体化学气相沉积（PCVD）设备，在高速钢（W18Cr4V）基材表面沉积新型四元Ti-Si-C-N复合超硬薄膜。结果表明：Ti-Si-C-N薄膜是由面心立方结构的TiN和TiC纳米晶、Ti（C，N）固溶体及存在于晶界的非晶Si3N4和α-C组成，形成TiN／TiC／Ti（C，N）／α-C／α-Si3N,复相结构，这种复相结构存在着[111]，[220]和[200]混合择优取向。SiCl4和CH4流量变化是影响薄膜相组成和硬度变化的主要工艺参数。随Si含量的增加，薄膜的显微硬度先升后降，表面形貌由致密的细颗粒状变为粗大的枝条状；C元素的加入能抑制柱状晶的形成，对硬度影响较小。     

Ti-Si-N纳米复合超硬薄膜的高温热稳定性

用脉冲直流等离子体增强化学气相沉积（PCVD）方法在高速钢（HSS）基体上制备了Ti—Si-N薄膜，重点从不同温度退火后薄膜相结构、晶粒尺寸和显微硬度的变化等方面，探讨了不同Si含量的Ti-Si-N薄膜的高温热稳定性。结果表明：Ti-Si-N薄膜在900℃以内退火处理后，晶粒尺寸和显微硬度并无明显突变，尤其是Si含量较低时，在800℃，晶粒尺寸和显微硬度几乎没有变化，表明Ti-Si-N薄膜具有非常良好的高温热稳定性，这可能与薄膜相形成在高温下仍为调幅分解有关。     

脉冲偏压对电弧离子镀Ti/TiN纳米多层薄膜显微硬度的影响

采用脉冲偏压电弧离子镀方法在高速钢基体上沉积Ti／TiN纳米多层薄膜,采用正交实验法设计脉冲偏压电参数,考察脉冲偏压对Ti／TiN纳米多层薄膜显微硬度的影响．结果表明,在所有偏压参数（脉冲偏压幅值、占空比和频率）和几何参数（调制周期和周期比）中,脉冲偏压幅值是影响显微硬度的最主要因素;当沉积工艺中脉冲偏压幅值为900V、占空比为50％及频率为30kHZ时,薄膜硬度可高达34．1GPa,此时多层膜调制周期为84nm,TiN和Ti单元层厚度分别为71和13nm;由于薄膜中的单层厚度较厚,纳米尺寸的强化效应并未充分体现于薄膜硬度的贡献中,硬度的提高主要与脉冲偏压工艺,尤其是脉冲偏压幅值对薄膜组织的改善有关．     

PCVD制备Til-xAlxN硬质薄膜的结构与硬度

用直流等离子体增强化学气相沉积(PCVD)方法获得了Ti1-xA1xN硬质薄膜,考察了A1含量x及高温退火对薄膜微观结构转变过程及其硬度的影。结果表明，制备的Ti1-xA1xN薄膜由3-10nm晶粒组成.随A1含量x增加，薄膜硬度升高，x超过0．83时，硬度开始急剧下降；结构分析证实x小于0．83，Ti1-xA1xN薄膜是固溶强化；x=0．83，薄膜中出现六方氮化铝相(h-AIN),热稳定性实验表明，Ti1-xA1xN薄膜的纳米结构和硬度在N2环境下可以维持到900℃。     

纳米晶NiSi2/Ti5Si3复合涂层耐磨耐蚀性能研究

采用双阴极等离子溅射技术在TC4合金表面制备了纳米晶NiSi2/Ti5Si3复合涂层。利用XRD、SEM和TEM研究了复合涂层的微观组织特征,利用纳米压入和声发射划痕仪考察了复合涂层的硬度、弹性模量以及涂层与基体的结合力。结果表明：纳米晶NiSi2/Ti5Si3复合涂层由外层厚度为7 μm的NiSi2沉积层和其下3 μm厚的Ti5Si3扩散层组成,沉积层的平均晶粒尺寸约为40 nm,而扩散层的平均晶粒尺寸约为70 nm,且存在大量的栅栏状孪晶。纳米晶NiSi2/Ti5Si3复合涂层硬度呈梯度分布,与基体具有较高的结合强度,其结合力为49 N。纳米晶NiSi2/Ti5Si3复合涂层的比磨损率较TC4合金降低一个数量级以上,且对载荷和温度不具敏感性。与TC4合金相比,纳米晶NiSi2/Ti5Si3复合涂层的腐蚀电流密度降低了两个数量级,且具有更大的容抗弧值     

PCVD制备Ti1-xAlxN硬质薄膜的结构与硬度

用直流等离子体增强化学气相沉积(PCVD)方法获得了Ti1-xAlxN硬质薄膜;考察了Al含量x及高温退火对薄膜微观结构转变过程及其硬度的影响.结果表明,制备的Ti1-xAlxN薄膜由3-10 nm晶粒组成.随Al含量x增加,薄膜硬度升高,x超过0.83时,硬度开始急剧下降;结构分析证实x小于0.83,Ti1-xAlxN薄膜是固溶强化;x=0.83,薄膜中出现六方氮化铝相(h-AlN).热稳定性实验表明,Ti1-xAlxN薄膜的纳米结构和硬度在N2环境下可以维持到900℃.     

The effect of microstructure and composition on mechanical properties in thick-layered nanocomposite Ti-Si-C-N coatings

Recently great emphases have been placed on material characteristics, such as hardness and toughness in development of protective hard coatings. This work aims to investigate the microstructures and mechanical properties of rather thick Ti-Si-C-N coatings, deposited by a plasma enhanced magnetron sputtering (PEMS). It has been evidently proved that Ti-Si-C-N coatings can effectively enhance hardness due to nanocomposite structure. The composition of the Ti-Si-C-N coatings was quantitatively measured with an electron probe microanalyzer (EPMA). Detailed microstructure of the Ti-Si-C-N coatings was performed by a transmission electron microscopy (TEM). The X-ray diffractometry (XRD) was also used to further identify microstructures. The results indicated that the hardness and microstructures of thick Ti-Si-C-N coatings were strongly affected by the Si contents. A nanocomposite coating with nano grains embedded in amorphous matrix was revealed.     

Dependence of Microstructure and Hardness of Nanocomposite Coatings of nc-(Ti_(1-x)Al_xN)/a-Si_3N_4 on Aluminum Contents

HARD COATINGS are finding a widely applicationin machining industries as tools and moulds since1980s[1].Hard coatings consisting of a variety of thetransition metal nitrides,for instance,TiN,TiC,TiCN,TiBN,TiAlN,CrN etc,usually service as a protectioncoatings that requires some better properties ofwear-resistance,corrosion-resistance and also highfatigue-strength especially at elevated temperature(formore details see Ref.2-6).The generic concept for the design of novelsuper-hard(>40G…     

Advantages of nanocomposite coatings deposited by high power pulse magnetron sputtering technology

Recent advantages in PVD coatings for cutting tools enable high speed and dry machining with superior cutting parameters in commercial manufacturing sectors. For this reason hard coatings with high oxidation resistance and thermal stability are used for economically justifiable machining. In this regard nc-(Ti,Al)N/a-Si₃N₄ films were sputtered on tungsten carbide cutting tools and WC/Co samples by using the high power pulse magnetron sputtering (HPPMS) technology. Coating composition, microstructure and applied properties were investigated by using X-ray diffraction, scanning electron microscope and nanoindentation. The hardness value was about 29 GPa for a Si content of 3.3 at.%. The grain size was about 6 nm. As this study focuses on the thickness uniformity of the coatings, SEM pictures of the cross-section have been taken around the cutting edge to determine the deposition rate and the film growth. The coatings morphology has been compared to middle frequency and direct current sputtered nanocomposite (Ti,Al,Si)N films. The results demonstrate the enhanced HPPMS coatings properties, including a denser structure, a smoother surface and a favourable thickness uniformity.     

Synthesis and characterization of super hard,self-lubricating Ti–Si–C–N nanocomposite coatings

Quaternary super hard Ti–Si–C–N coatings with different carbon contents were deposited on high-speed steel substrates by pulsed direct current plasma-enhanced chemical vapor deposition (PECVD) technology, using a gaseous mixture of TiCl₄/SiCl₄/N₂/H₂/CH₄/Ar. A variety of technologies have been employed to characterize the coatings, including X-ray diffraction, scanning and transmission electron microcopies, X-ray photoelectron spectroscopy, energy dispersive X-ray analysis, automated load–depth sensing and pin-on-disc. The super hard Ti–Si–C–N coatings were found to have unique nanocomposite structures composed of nanocrystallite and amorphous nc-Ti(C,N)/a-Si₃N₄/a-C and/or nc-Ti(C,N)/nc-TiSi₂/nc-Si/a-Si₃N₄/a-C, depending on the carbon contents in the coatings. The friction coefficient of the Ti–Si–C–N coatings with a higher carbon content (nc-Ti(C,N)/a-Si₃N₄/a-C nanocomposites) were found to be much lower than those of the Ti–Si–N coatings both at room and elevated temperatures, suggesting the formation of a graphite-like lubricious phase of amorphous carbon. However, they are still super hard (32–48 GPa) in spite of the carbon incorporation. This is due to a strong, thermodynamically driven and diffusion-rate-controlled (spinodal) phase segregation that leads to the formation of a stable nanostructure by self-organization. The energy difference between the grain boundary and the crystallite/amorphous phase interface hinders grain boundary mobility, leading to a gradual decrease in the grain size of the nanocrystallites. As a result, nanocomposite Ti–Si–C–N coatings with high hardness and a low friction coefficient can be produced. The coatings are foreseen to have high potential in dry and high-speed cutting tool applications, thus providing for cleaner, healthier and more pleasant machining conditions.     

Microstructure evolution and mechanical properties of Ti-B-N coatings deposited by plasma-enhanced chemical vapor deposition

Ternary Ti-B-N coatings were synthesized on AISI 304 and Si wafer by plasma-enhanced chemical vapor deposition (PECVD) technique using a gaseous mixture of TiCl4,BCl3,H2,N2,and Ar.By virtue of X-ray diffraction analysis,X-ray photoelectron spectroscopy,scanning electron microscope,and high-resolution transmission electron microscope,the influences of B content on the microstructure and properties of Ti B N coatings were investigated systematically.The results indicated that the microstructure and mechanical properties of Ti-B-N coatings largely depend on the transformation from FCC-TiN phase to HCP-TiB2 phase.With increasing B content and decreasing N content in the coatings,the coating microstructure evolves gradually from FCC-TiN/a-BN to HCP-TiB2 /a-BN via FCC-TiN+HCP-TiB2/a-BN.The highest microhardness of about 34 GPa is achieved,which corresponds to the nanocomposite Ti-63%B-N (mole fraction) coating consisting of the HCP-TiB2 nano-crystallites and amorphous BN phase.The lowest friction-coefficient was observed for the nanocomposite Ti-41%B-N (mole fraction) coating consisting of the FCC-TiN nanocrystallites and amorphous BN phase     

电弧离子镀制备 TiSiN 纳米复合涂层

目的在SiH4气氛下制备Si掺杂的TiSiN纳米复合涂层,为SiH4用于工业化TiSiN涂层生产提供依据。方法采用电弧离子镀技术,在SiH4气氛下,于单晶硅和硬质合金衬底上制备Si掺杂的TiSiN纳米复合涂层,研究SiH4流量对TiSiN涂层化学组分、微观结构、硬度和耐磨性能的影响。结果 SiH4流量对TiSiN纳米复合涂层的微观结构、硬度及摩擦系数的影响明显。随着SiH4流量的增加,TiSiN涂层由柱状晶生长的晶体结构逐渐转变为纳米晶镶嵌于非晶基体的复合结构。Si在涂层中以Si3N4非晶相存在,随着涂层中Si含量逐渐增加,TiN晶粒尺寸逐渐减小,Si3N4起到细化晶粒的作用。在42 m L/min的SiH4流量下,涂层硬度高达4100HV0.025。在对磨材料为硬质合金的条件下,TiSiN涂层摩擦系数小于0.6。结论 SiH4气氛下可以制备出Ti N纳米晶镶嵌于Si3N4非晶相结构的TiSiN纳米复合涂层,涂层的显微硬度较高。SiH4可以作为Si源用于TiSiN纳米复合涂层的工业化生产。     

Comparative investigation of Al- and Cr-doped TiSiCN coatings

The aim of this work was a comparative investigation of the structure and properties of Al- and Cr-doped TiSiCN coatings deposited by magnetron sputtering of composite TiAlSiCN and TiCrSiCN targets produced by self-propagating high-temperature synthesis method. Based on X-ray diffraction, scanning and transmission electron microscopy, X-ray photoelectron spectroscopy, and Raman spectroscopy data, the Al- and Cr-doped TiSiCN coatings possessed nanocomposite structures (Ti,Al)(C,N)/a-(Si,C) and (Ti,Cr)(C,N)/a-SiC_xN_y/a-C with cubic crystallites embedded in an amorphous matrix. To evaluate the thermal stability and oxidation resistance, the coatings were annealed either in vacuum at 1000, 1100, 1200, and 1300 °C or in air at 1000 °C for 1 h. The results obtained show that the hardness of the Al-doped TiSiCN coatings increased from 41 to 46 GPa, reaching maximum at 1000 °C, and then slightly decreased to 38 GPa at 1300 °C. The Cr-doped TiSiCN coatings demonstrated high thermal stability up to 1100 °C with hardness above 34 GPa. Although both Al- and Cr-doped TiSiCN coatings possessed improved oxidation resistance up to 1000 °C, the TiAlSiCN coatings were more oxidation resistant than their TiCrSiCN counterparts. The TiCrSiCN coatings showed better tribological characteristics both at 25 and 700 °C and superior cutting performance compared with the TiAlSiCN coatings.     

Self-lubricant nanocomposite hard coatings in Ti-Al-N-C system

An ambitious objective in the development of self-lubricating wear-resistant coatings is to make use of lubricious phases such as graphite, amorphous carbon or MoS2 incorporated into coatings. A series of (Ti,Al)(N,C)coatings with different carbon contents (0 -28 %, mole fraction) were deposited by reactive magnetron sputtering of TiAl in a mixture of Ar, N2 and CH4 gases. The microstructure and constitution of these coatings were investigated using EPMA, AFM, XPS, (HR)TEM, Raman spectroscopy and X-ray diffraction. Starting from a pure TiAlN coating significant changes in the microstructure of the coatings were observed dependent on the carbon concentration. Under optimum conditions nanocomposite coatings with a structure of a coexisting metastable hard, nanocrystalline fcc (Ti,Al)(N,C) phase and an amorphous carbon phase were deposited. The localization of an amorphous carbon phase was shown by HRTEM.     

Nitrogen Contents on Tribological Properties of Magnetron Sputtered SICN Coatings

SiCN COATINGS have stimulated wide interestbecause they exhibit many good properties for potentialindustrial applications,such as high opticaltransparency in Infrared(IR)region,wide bandgap,chemical inertness and high refractive index,goodinsulating property,good mechanical and tribologicalproperties(high hardness,elastic modulus,low friction,etc.)[1-4].Amorphous and/or hydrogenated SiCNcoatings can be prepared by various depositionmethods,such as laser ablation[5],plasma-assistedchemica…