脉冲偏压磁过滤电弧离子镀TiN薄膜的组织结构及耐磨性研究

利用脉冲偏压磁过滤电弧离子镀在高速钢(M2)基底上沉积了厚约2.5μm的TiN薄膜;分别采用FESEM、GDOES、XRD和划痕试验法观察薄膜表面和断面形貌、测试薄膜成分及相结构,分析膜基结合强度,通过显微硬度计和球盘摩擦磨损试验机对比考察TiN薄膜和M2高速钢基体的硬度和耐磨性。结果表明,TiN薄膜表面光滑致密,呈现致密柱状晶结构和明显的(111)择优取向,膜基结合强度大于60 N,薄膜硬度约为26 GPa;脉冲偏压磁过滤电弧离子镀制备的TiN薄膜表现出很好的减摩和耐磨性能。     

负偏压对电弧离子镀复合TiAlN 薄膜的影响

采用电弧离子镀技术,以W18Cr4V高速钢为基体,调整基体负偏压,制得多个复合TiAlN薄膜试样,研究了基体负偏压对薄膜微观组织形貌、物相组成、晶格位向、硬度、厚度和沉积速率的影响。结果表明,过高或过低的负偏压会使得膜层表面不平整,显微硬度下降。当负偏压为200 V时,膜层的沉积速率最大;负偏压为150 V时,有利于薄膜(111)晶面的择优取向生长,且TiAlN膜的硬度最高。     

负偏压对低温沉积TiN薄膜表面性能的影响

研究了在低温磁控溅射沉积TiN薄膜过程中,负偏压对基体温度、薄膜表面性能、薄膜与基体界面结合强度以及摩擦学性能的影响.研究结果表明,加负偏压条件下,明显提高基体温度,有益于晶粒细化,提高硬度,改善色泽,提高TiN/基体的界面结合强度,但会引起表面轻微的粗糙化;摩擦学试验表明,负偏压对低温磁控溅射TiN薄膜及其摩擦副的摩擦磨损性能的影响较明显.     

硬质合金表面多弧离子镀(Ti,Al,Zr,Cr)N多元氮化物膜

采用Ti-Al-Zr合金靶和Cr靶,用多弧离子镀技术在WC-8%Co硬质合金基体上沉积(Ti,Al,Zr,Cr)N多元氮化物膜。分析了薄膜的成分、形貌、粗糙度和结构,研究了薄膜的显微硬度、膜/基结合力和抗高温氧化性能。结果表明,获得的多元氮化物膜仍是B1-NaCl型TiN面心立方结构;适当控制偏压条件可以改善薄膜的表面形貌;在不同的偏压条件下,(Al+Zr+Cr)/(Ti+Al+Zr+Cr)的成分比为0.41～0.43,当其比值趋于0.4时,薄膜的显微硬度和膜/基结合力达到最大值3600HV0.01和200N;同时薄膜的抗高温氧化性能提高,最高温度可达700℃左右。     

65Mn钢基体CrTiAlN微纳米复合膜的制备与抗高温磨损性能研究

采用多弧离子镀在活塞环65Mn钢基体表面制备CrTiAlN微纳米复合膜,研究了CrNx过渡缓冲层与工作负偏压对CrTiAlN微纳米复合膜性能的影响规律,采用X射线衍射(XRD)、扫描电子显微镜(SEM)、划痕仪、纳米硬度仪和发动机台架试验装置,系统分析了薄膜相结构、表面形貌、纳米硬度和抗高温摩擦磨损性能。结果表明:当N2含量为45%时,CrNx薄膜中主要以CrN(220)相为主,此时复合膜结合强度相对较高;复合膜厚度随负偏压增大而减小,纳米硬度随负偏压增大而增大,当偏压为–200V时,CrTiAlN微纳米复合膜的晶粒较为细小。采用优化工艺沉积的CrTiAlN复合膜具有优异的抗高温粘着磨损性能,优于CrN膜和电镀Cr,最后对3种活塞环涂层的抗高温磨损机理进行了分析讨论。     

脉冲偏压对电弧离子镀TiCN薄膜组织结构的影响

目的改善TiCN薄膜的组织结构,进一步提高其硬度与结合力。方法采用电弧离子镀技术,通过改变脉冲偏压的幅值,制备一系列的TiCN薄膜。通过扫描电子显微镜(SEM)观察薄膜的表面和截面形貌,采用X射线衍射(XRD)对薄膜进行物相分析,用X射线光电子谱(XPS)表征元素的化学状态,通过能谱仪(EDS)分析薄膜的成分。采用显微维氏硬度计测量薄膜硬度,使用3D轮廓仪测量薄膜厚度,利用多功能材料表面性能试验仪进行划痕测试。结果偏压对薄膜的硬度、结合力、组织结构和沉积速度都有影响。随着脉冲偏压的提高,TiCN薄膜晶粒逐渐细化,沉积速率、结合力有先增大后减小的趋势,TiCN薄膜的硬度保持线性提高。偏压为-200 V时,TiCN薄膜出现C_3N_4新相,此时薄膜的硬度和结合力都大幅度提高,表面形貌发生突变,液滴最多。偏压为-250 V时,TiCN薄膜综合性能最好,并且表面的液滴明显减少,此时硬度值为4017HV,结合力为51 N。结论偏压对组织结构及碳元素在薄膜中的存在形式有一定影响,适当地改变脉冲偏压可以使TiCN薄膜的显微组织更加致密,同时,形成的弥散硬化相使薄膜具备较高的硬度和膜基结合强度。     

多弧离子镀负偏压对氮化钛薄膜的影响

目的确定适当的负偏压,提高多弧离子镀氮化钛薄膜的综合性能。方法采用不同的负偏压,在4Cr13不锈钢表面制备Ti N薄膜,探讨偏压对薄膜表面质量、结构、硬度、结合力和摩擦系数的影响。结果负偏压对薄膜表面质量的影响较大:负偏压为0 V时,Ti N薄膜表面凹凸不平,液滴较多;随着负偏压升高,薄膜表面变得光滑,液滴减少并变小,薄膜致密性也得到提高。在不同负偏压下,Ti N薄膜均呈现出在(111)晶面的择优取向,但随着负偏压的增大,这种择优取向逐渐减弱,当负偏压达到400 V时,薄膜在(220)晶面的峰值逐渐增强。随着负偏压从0增至400 V,薄膜的硬度、结合力和耐磨性均先提高,后降低。当负偏压为300 V时,薄膜的硬度和结合力达到最大,分别为2650HV和58 N;摩擦系数和磨损量最小,分别为0.48和0.1065 mm3。结论施加适当的负偏压可以提高薄膜的硬度、结合力、耐磨性等性能,当负偏压为300 V时,薄膜的各项性能达到最佳。     

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．     

脉冲偏压电弧离子镀Ti/TiN纳米多层薄膜的结构与硬度

采用脉冲偏压电弧离子镀设备在高速钢基体上沉积Ti／TiN纳米多层硬质薄膜,通过仅改变偏压幅值的方法进行对比实验。XRD分析和薄膜断截面SEM形貌显示出薄膜的纳米多层组织结构;硬度测试表明纳米多层薄膜硬度随脉冲偏压升高而升高。在-900V时超过同等条件制备的TiN单层薄膜,硬度高达34．1GPa;分析表明硬度的提高主要与脉冲偏压工艺对薄膜组织的改善有关;用脉冲偏压电弧离子镀可以制备纳米多层硬质薄膜,并且在工艺控制上相对简单。     

多弧离子镀工艺参数对氮化钛薄膜结合力的影响研究

应用多弧离子镀对4Cr13不锈钢基体沉积TiN薄膜,用WS-2005型附着力自动划痕仪测试薄膜的结合力,研究弧电流、沉积温度和偏压对膜基结合强度的影响。结果表明:随着靶电流、沉积温度和偏压的增大,TiN薄膜与基体的结合力先增大后减小。在其它参数不变时,当弧电流为85、95、105、120 A时,薄膜结合力分别为42、50、75、63N;当沉积温度为150、200、250、300℃时,薄膜的结合力分别为45、45、48、40 N;当偏压为0、200、300、400 V时,薄膜的结合力分别为38、42、58、42 N。本试验膜基结合强度最佳工艺参数为:弧电流105A、沉积温度250℃、偏压300V。     

Structural and nano-mechanical properties of nanostructured diamond-like carbon thin films

The effect of self bias on structural and nano-mechanical properties of nanostructured diamond-like carbon (ns-DLC) thin films is explored. These films are grown at different negative self biases ranging from ?100 V to ?200 V using radio frequency (13.56 MHz) plasma enhanced chemical vapor deposition technique. The generation of nanostructured morphology at room temperature in these films is confirmed by scanning electron microscopy, whereas change in microstructure produced by varying the self biases is confirmed by Raman analysis. These ns-DLC films exhibit very high hardness, which varied from 16 GPa to 31 GPa. With the help of load versus displacement curves, various other important nano-mechanical parameters such as elastic modulus, elastic recovery etc are also estimated. The nano-mechanical properties are further correlated with the Raman and SEM analyses. Owing to their versatile nano-mechanical properties, these ns-DLC films may find application as hard and protective coatings.     

脉冲偏压电弧离子低温沉积TiN硬质薄膜的力学性能

利用直流和脉冲偏压电弧离子镀技术沉积TiN硬质薄膜，研究了不同偏压下基体的沉积温度、薄膜的表面形貌及力学性能．结果表明，与直流偏压相比，脉冲偏压可以明显降低基体的沉积温度，大大减少薄膜表面的大颗粒污染，改善表面形貌，而薄膜的综合力学性能仍保持良好，说明利用脉冲偏压技术是实现电弧离子镀低温沉积的有效途径．     

脉冲偏压占空比对TiN/TiAlN多层薄膜微观结构和硬度的影响

目的研究脉冲偏压占空比对TiN/TiAlN多层薄膜微观结构和硬度的影响规律。方法利用脉冲偏压电弧离子镀的方法,改变脉冲偏压占空比,在M2高速钢表面制备5种TiN/TiAlN多层薄膜,对比研究了薄膜的微观结构、元素成分、相结构和硬度的变化规律。结果 TiN/TiAlN多层薄膜表面出现了电弧离子镀制备薄膜的典型生长形貌,随着脉冲偏压占空比的增加,薄膜表面的大颗粒数目明显减少。此外,脉冲偏压占空比的增加还引起多层薄膜中Al/Ti原子比的降低。结论 TiN/TiAlN多层薄膜主要以(111)晶面择优取向生长,此外还含有(311),(222)和(200)晶相结构。5种多层薄膜的纳米硬度均在33GPa以上,当脉冲偏压占空比为20%时,可实现超硬薄膜的制备。     

Mechanical Behaviors of Ti-Si-N Coatings Deposited by Bias Sputtering

Ti-Si-N hard coatings were deposited on steel substrates by reactive unbalanced magnetron sputtering from Ti and Si elemental targets in a mixture of Ar and N2 gases.The influences of negative bias voltage(in the range of-30 to-80 V)on the mechanical properties of the coatings were investigated.In particular,the critical cycle during dynamic impact tests was employed to indicate the bonding strength of the coatings.It was found that the Ti-Si-N coatings prepared at lower constant bias voltages could effectively improve the adhesion and the cyclic impact performance,but their hardness was dropped significantly to 13 GPa at a bias of-30 V.Higher bias voltage values induced greater hardness.A maximum hardness of 47 GPa was obtained at a bias of-60 V.However,the coating adhesion was worse in this case,and the number of impact cycles(～8×10 3)that the coatings could endure was much shorter than that of TiN binary coatings(～2×104).On the other hand,the bias voltage was varied linearly from-40 to-60 V during Ti-Si-N deposition.Under this circumstance,the hardness of the coatings deposited with the bias-graded configuration remained very high(42 GPa),and the adhesion strength was improved substantially.Also,the critical impact cycle could reach as high as 1.8×104.Therefore,bias-graded deposition can provide an effective processing route to prepare Ti-Si-N superhard coatings with high adhesion strength and impact resistance.     

偏压对离子源辅助HiPIMS制备纳米TiN薄膜力学性能和耐蚀性能的影响

为提高磁控溅射制备薄膜的致密度,减少结构缺陷,研究薄膜显微结构对硬度、韧性及耐蚀性能的影响,尝试在改变离子源和基材偏压的条件下,采用离子源辅助HiPMIS技术在304不锈钢和P型（100）晶向硅片上制备TiN纳米薄膜。采用扫描电子显微镜、小角X射线衍射仪对薄膜的形貌和晶体结构进行分析;采用纳米压痕仪和维氏硬度计分别测量计算薄膜的硬度和韧性,并通过电化学工作站对薄膜的耐蚀性能进行检测。结果表明：随着偏压的增加以及离子源的引入,离子的轰击效应增强,薄膜的沉积速率下降,致密度增加。偏压为-200 V时,薄膜的硬度达到最大值16.2 GPa,且对应的晶粒尺寸最小,（111）晶面衍射峰的强度最高。离子源的加入使所制备薄膜的硬度略有下降。此外,随着偏压的增加,薄膜的韧性和耐腐蚀性能也有一定提高。     

Microstructure and physical properties of PVD TiN/（Ti, Al）N multilayer coatings

Magnetron sputtered （Ti, Al） N monolayer and TiN/（Ti, Al） N multilayer coatings grown on cemented carbide substrates were studied by using energy dispersive X-ray spectroscopy （EDX）, scanning electron microscopy （SEM）, nanoindentation, Rockwell A indentation test, strength measurements and cutting tests. The results show that the （Ti, Al）N monolayer and TiN/（Ti, Al）N multilayer coatings perform good affinity to substrate, and the TiN/（Ti, Al）N multilayer coating exhibits higher hardness, higher toughness and better cutting performance compared with the （Ti, Al）N monolayer coating. Moreover, the strength measurement indicates that the physical vapour deposition （PVD） coating has no effect on the substrate strength.     

Characterization of Zinc-Cobalt Electrodeposits

The structure and morphology of electrodeposits depend on many factors including temperature, current density, time of deposition and composition of the bath. The properties of an electrodeposit depend on its micro structure. For example corrosion and wear resistance, hardness, internal stress, strength, brightness, electrical conductivity, magnetic properties and leveling are all affected by structure.

The relationships between electroplating parameters such as current density, temperature, bath agitation and electrolyte composition have been investigated for the zinc-cobalt system. It was found that electrolyte composition and temperature affect both deposit composition and morphology. The cathodic current efficiency decreased with current density and hardness was raised with increasing cobalt content in the deposit.

Three powerful techniques were used to access the microstructure of zinc-cobalt deposits: scanning electron microscopy, transmission electron microscopy and X-ray diffraction. The results show that the alloy is constituted of a single phase of a solid solution of cobalt dissolved in zinc within an hexagonal crystal system. The deposit is porous and changes from dendritic to nodular with increasing cobalt content.     

沉积温度对高性能TiAlN涂层微观结构和力学性能的影响

采用真空电弧离子镀（AIP）技术在不同沉积温度下TiAlN涂层,用于高性能制造,并研究了沉积温度与表面性能的关系。结果表明,由于离子轰击作用,表面大颗粒随沉积温度的升高而减少。随着沉积温度的升高,涂层表面的晶粒尺寸先急剧减小后逐渐增大。此外,沉积温度对合成涂层的相组成和化学成分影响不大。随着沉积温度的升高,硬度和粘结强度先迅速增加,后逐渐降低。当沉积温度在450℃左右时,沉积的TiAlN涂层硬度最高,粘结强度最大。上述现象的发生机理与沉积过程中表面与界面之间的微观组织和残余应力的变化有关。合成的涂层在高达900℃的空气中具有良好的热稳定性。