多元等离子体浸没离子注入与沉积和磁控溅射技术制备TiAlSiN/WS_2多层薄膜的力学性能和腐蚀行为(英文)

为了降低超硬TiAlSiN复合涂层的摩擦因数,采用多元等离子体浸没离子注入与沉积和射频(RF)磁控溅射技术制备TiAlSiN/WS2多层薄膜,利用XRD、SEM、Raman光谱、纳米探针、摩擦和电化学试验对薄膜的微结构、力学性能和腐蚀行为进行测试与分析。SEM结果表明:TiAlSiN/WS2多层薄膜具有清晰的调制周期。纳米硬度结果表明,TiAlSiN/WS2多层薄膜硬度介于TiAlSiN和WS2涂层硬度之间。摩擦实验结果证实TiAlSiN/WS2多层薄膜的摩擦因数低于TiAlSiN涂层的,且摩擦过程平稳。此外,TiAlSiN/WS2多层薄膜表现出良好的抗腐蚀能力,在相对较小的调制周期内,其腐蚀电流密度显著降低。     

等离子体浸没离子注入与沉积合成TiN薄膜的滚动接触疲劳寿命和机械性能

采用等离子体浸没离子注入与沉积（PIII＆D）技术在AISI 52100轴承钢表面合成了高硬耐磨的TiN薄膜.膜层元素分布、化学组成和表面形貌分别用XRD,XPS表征.合成薄膜前后试样的滚动接触疲劳寿命和摩擦磨损性能分别由球棒疲劳磨损试验机和球-盘磨损试验机测定;疲劳破坏后的微观形貌通过SEM观察;薄膜力学性能经纳米压痕和纳米划痕实验评价.结果表明,TiN膜中还含有少量的TiO2和Ti,N,O的化合物.在优化条件下,TiN膜层致密均匀,与基体结合良好,纳米硬度和弹性模量分别达到25和350 GPa;最低摩擦系数由基体的0.92下降到0.2.被处理薄膜试件在90%置信区间下的最大L10,L50,La和-↑L寿命较基体分别提高了约4.5,1.8,1.3和1.2倍,疲劳寿命的分散性得到了显著改善.     

低能Si离子注入对TiN硬质薄膜性能的影响

采用低能MEVVA离子源技术对由磁过滤阴极真空弧沉积的TiN硬质膜进行了Si离子注入.采用场发射扫描电子显微镜、纳米硬度测试等方法,研究了基体离子注入剂量对薄膜性能的影响.结果表明,Si离子注入能在薄膜表面形成均匀细小的纳米颗粒.使基体及薄膜硬度从33 GPa提高到56 GPa,弹性模量从360 GPa提高到750 GPa.对薄膜进行多(4)次注入,硬度和弹性模量的提高并不显著,但对基体离子注入充分,薄膜的整体硬度和吸收塑性变形能的能力均有显著提高.     

TiAlSiN纳米复合涂层的改性研究现状及发展

随着切削技术向高速、高效、高精、绿色、智能方向发展,切削加工对刀具及涂层性能提出了更高的要求,以TiAlSiN涂层为代表的四元硬质涂层发展迅速。综述了单层TiAlSiN纳米复合涂层的制备工艺、结构与性能特点,根据TiAlSiN单层涂层存在低韧性和低结合强度的问题,提出了对TiAlSiN涂层改性研究的必要性。综述了结构改性、成分改性以及二者相结合改性TiAlSiN涂层的制备工艺、结构与性能特点,指出了纳米多层结构的TiAlSiN涂层中存在的横向层间界面对原子的扩散具有良好的阻碍作用,涂层的抗氧化性由此被提高,涂层硬度等力学性能受多层结构的调制层成分、调制周期等因素影响而被提高或降低。介绍了C、Cu、Cr、V等合金化元素在TiAlSiN涂层中的作用效果,C元素在涂层中具有减摩作用,Cu元素的主要作用是增强涂层与基体的结合,Cu、Cr、V元素在涂层中均使涂层硬度不同程度降低,提出了最大限度发挥添加元素与层间界面结构的协同作用来获取最佳性能的纳米多层结构TiAlSiN基多元涂层是今后研究的重要方向之一。此外,还提出了通过基体前处理和涂层后处理增强TiAlSiN涂层韧性和层基结合强度的发展方向。     

高功率调制脉冲磁控溅射沉积TiAlSiN纳米复合涂层对钛合金基体抗氧化性能的影响研究

目的研究Ti6Al4V基TiAlSiN涂层在800℃下的抗循环氧化性能。方法采用高功率调制脉冲磁控溅射技术,通过调节N2/Ar的流量比fN2,在Ti6Al4V合金和Si(100)上沉积了一系列不同Si含量的TiAlSiN涂层。通过X射线衍射仪、扫描电子显微镜、电子探针、透射电镜和纳米压痕仪,表征了TiAlSiN涂层的成分、相组成、微结构和硬度,并通过X射线衍射仪和扫描电子显微镜,进一步对Ti AlSiN涂层在800℃下循环氧化后的微观结构和形貌进行分析。结果脉冲平均功率为2k W时,fN2由10%增至30%,TiAlSiN涂层的Si含量(以原子数分数计)由6.1%增加至16.4%,涂层中Ti和Al含量则相应地降低。当fN2为10%时,TiAlSiN涂层呈现典型的X射线非晶结构特征,涂层中N含量(以原子数分数计)约为47%;当fN2为30%时,TiAlSiN涂层呈现Ti Al N和非晶相的混合结构。TEM结果表明,涂层中TiAlN晶粒尺寸约为5nm并均匀镶嵌在非晶相上。所有沉积于Si基底上的TiAlSiN涂层均具有相近的纳米硬度、弹性模量及残余应力,分别为17 GPa、225 GPa和–...     

Si添加对TiN涂层微结构、力学及抗氧化性能的影响

借助EDX、XRD、SEM及纳米压痕研究了采用磁控溅射技术制备的TiN和Ti-Si-N涂层的微观组织结构和力学性能。研究表明:TiN和Ti-Si-N涂层均呈面心立方结构,Si元素的加入使TiN涂层的组织形貌由柱状晶结构转变为Si3N4界面相包裹纳米晶TiN的纳米晶复合结构;由于界面强化效应,Si的加入使涂层的硬度显著增加;涂层的应力也随着Si元素的加入而增加;Si的加入使TiN涂层的抗氧性得到明显改善。     

等离子体浸没离子注入与沉积技术的发展及前沿问题

表面热功能结构是指在固体表面加工出具有不同形貌、不同尺度、不同维数,并具有散热或传热功能的结构。复杂表面热功能结构在高集成度芯片热控制方面有着广阔的应用前景。如何根据热功能需求主动设计表面结构并提出适合高效率低成本的制造方法是解决高热流密度问题的核心所在。在对当前表面热功能结构的发展现状分析基础上,较详细论述了表面热功能结构制造领域的关键技术,指出未来表面热功能结构研究的重点应集中在结构的微细化和复杂化、表面热功能结构的高效低成本制造方法等方面。     

工作气压对TiBN/TiAlSiN纳米多层涂层的结构和性能影响

为应对高速干式切削、工磨具行业对新型防护涂层的需求,制造高硬度、耐摩擦磨损的纳米复合涂层具有巨大的市场前景。 采用阴极多弧离子镀技术,在不同的工作气压下用 TiB2 和 TiAlSi 合金靶作为阴极蒸发靶材,在硬质合金衬底上分别沉积了 TiBN,TiAlSiN 涂层和 TiBN/ TiAlSiN 多层涂层。 借助于 XRD、 XPS、 SEM、 AFM 和 HRTEM 对涂层的成分、形貌及微观结构进行表征分析。 并用纳米压痕硬度计和球盘式摩擦测试仪分别研究了涂层的硬度和摩擦磨损性能。 研究结果表明:TiBN/ TiAlSiN 涂层呈现一种非晶相包裹纳米多晶相的微观结构形态,工作气压越高,涂层表面越趋于光滑;涂层在 1. 0 Pa 工作气压下涂层显微硬度值达到 38 GPa;在 2. 0 Pa 的工作气压下,涂层显微硬度值约 34 GPa,摩擦因数低于 0. 29。 与 TiBN 和 TiAlSiN 涂层相比,TiBN/ TiAlSiN 纳米多层涂层的机械、摩擦学性能更加优越,这为应用在干式切削、磨削工具领域的硬质润滑多层涂层的制备与研究指明了一条方向。     

等离子体基离子注入氮对铝合金耐磨性的影响

利用等离子体基离子注入技术对硬铝ＬＹ１２和锻铝ＬＤ１０两种材料通过改变注入脉宽、频率、时间和电压等参数进行氮离子注入,注入剂量范围为２×１０１７～１×１０１８Ｎ＋／ｃｍ２。利用低角Ｘ射线衍射法（ＧＩＸＲＤ）分析氮离子注入层的相结构。在此基础上进行了显微硬度和摩擦磨损试验。由于氮离子注入铝合金能形成硬质的ＡｌＮ析出相,合金表面硬度及耐磨性都得到改善,随着注入脉宽、频率、时间和电压的增加,铝合金表层硬度及耐磨性也相应提高。     

热震对TiAlSiN涂层结构与性能的影响

目的探究TiAlSiN涂层经过不同热震次数后,其组织结构及性能的变化规律及机制。方法采取电弧离子镀技术在单晶硅和M2高速钢(W6Mo5Cr4V2)表面沉积TiAlSiN涂层,采用加热-水淬循环的方法进行热震试验。采用3D表面轮廓仪、扫描电子显微镜(SEM)表征涂层显微形貌,用金相显微镜测定膜/基结合力,用能谱仪(EDS)分析涂层元素含量变化,用X射线衍射仪(XRD)表征物相结构,用划痕仪和硬度计测量涂层力学性能,用摩擦磨损试验仪、光学显微镜探究涂层摩擦学性能及摩擦磨损机制。结果随着热震次数的增加,涂层表面产生的TiO颗粒尺寸增大,含量增多,粗糙度增加。XRD衍射峰向小角度发生偏移,但仍保持立方结构。涂层的力学性能变差,硬度值由2066HV_(0.025)下降至1447HV_(0.025),结合力由常温的71.8 N下降至33.9 N,结合力等级由常温的HF1降至HF4。此外,30、40、50次热震后,涂层展现出比常温下更优异的耐磨性能,摩擦系数由常温的0.571分别降低至0.427、0.389、0.273,磨损率由常温时的1.4×10~(-14) m~3/(N·m)分别降至1.01×10~(-14)、0.93×10~(-14)、0.71×10~(-14)m~3/(N·m),磨损类型主要为粘着磨损与氧化磨损。结论 TiAlSiN涂层在600℃下具备优异的抗热震性能,多次冷-热循环后仍为立方结构。随着热震次数的增加,TiAlSiN涂层表面质量及力学性能下降,但摩擦磨损试验中,由于涂层表面多次热震形成的氧化物起到润滑效果,有效减缓了涂层与摩擦球的剧烈接触,使TiAlSiN涂层的耐磨减摩性能提高。     

全方位离子注入与沉积类金刚石碳膜的结构与性能

用等离子体浸没离子注入与沉积(PIIID)复合强化新技术在AISI440C不锈钢表面制备了类金刚石(DLC)碳膜。膜层表面的原子力显微镜(AFM)形貌显示出DLC膜结构致密均匀。Raman光谱分析结果表明,制备的DLC主要是由金刚石键(sp3)和石墨键(sp2)组成的混合无定形碳膜,且sp3键含量大于10%。以纯石墨棒做阴极,C2H2为工作气体条件下合成的DLC薄膜中,sp3键含量总体上较单纯用石墨作阴极而无工作气体条件下合成的DLC薄膜中sp3键含量高。与基体相比,薄膜试样的显微硬度和摩擦磨损性能均得到了较大改善,最大硬度提高88.7%,磨损寿命延长超过4倍。     

Diamond-like carbon films synthesized on bearing steel surface by plasma immersion ion implantation and deposition

Diamond-like carbon (DLC) films were synthesized by plasma immersion ion implantation and deposition (PIIID) on 9Cr18 bearing steel surface. Influences of working gas pressure and pulse width of the bias voltage on properties of the thin film were investigated. The chemical compositions of the as-deposited films were characterized by Raman spectroscopy. The micro-hardness, friction and wear behavior, corrosion resistance of the samples were evaluated, respectively. Compared with uncoated substrates, micro-hardness results reveal that the maximum is increased by 88.7%. In addition, the friction coefficient decreases to about 0.1, and the corrosion resistance of treated coupons surface are improved significantly.     

Tribological behavior of AISI302 austenitic stainless steel modified by elevated temperature nitrogen plasma immersion ion implantation

AISI302 stainless steel samples were modified by elevated temperature nitrogen plasma immersion ion implantation at temperature ranging from 330 ℃ to 450 ℃. The tribological behaviors of the implanted layers of the samples were investigated. The samples were characterized by Auger electron spectroscopy (AES), glancing angle X-ray diffraction (GXRD), and nanoindentation. The results show that the implantation temperature plays an important rule on the microstructure and surface properties of the implanted layers. The thickness of the modified layer implanted at 390 ℃ is about 9 μm. It is improved about two orders compared with that of the implanted at room temperature. The surface nanohardness and the wear resistance of elevated temperature implanted layers increase significantly, and the friction coefficient decreases obviously in comparison with the unimplanted one. These data suggests that the improvement results from the formation of new phases such as ε-(Fe, Cr, Ni)2 xN, or noncrystal phase.     

Structure and properties of silver-containing a-C(H) films deposited by plasma immersion ion implantation

In this study, we have grown silver-containing hydrogenated (a-C:H) and non-hydrogenated (a-C) amorphous carbon coatings by two plasma immersion ion implantation methods: I) chemical vapor deposition of methane combined with pulsed filtered cathodic arc deposition of silver, and II) by alternating arc pulses from graphite and silver in a dual cathodic arc plasma source. This unique “bias selective” feature of the deposition system allowed the deposition of silver with the substrates at ground and avoided the sputtering of the grown a-C film. Chemical composition of the samples was analyzed by acquiring their compositional depth-profiles using radio-frequency Glow Discharge Optical Emission Spectroscopy (rf-GDOES), while the microstructural properties were analyzed by X-ray absorption near edge spectroscopy (XANES) and Raman spectroscopy. In this contribution, we compare mechanical and biomedical properties by means of nanoindentation and cell viability tests, respectively, of a-C(H) films obtained by two different plasma immersion ion implantation techniques.     

TiN/ZrO2 multilayers synthesized on GCr15 bearing steel using plasma immersion ion implantation and deposition

TiN/ZrO₂ multilayers with different modulation periods were synthesized on GCr15 bearing steel using plasma immersion ion implantation and deposition (PIIID). The total thickness of the TiN/ZrO₂ multilayers was approximately 2 μm and the modulation period was varied from 8 to 400 nm. The as-deposited films were characterized by scanning electron microscopy (SEM), micro-hardness, friction, scratch and corrosion tests. The SEM result indicates that the structure of the TiN/ZrO₂ multilayers has a good periodicity. Micro-hardness testing results show that the hardness enhancement effect takes place at the specific period of 15 nm, 100 nm and 200 nm. In addition, the friction coefficient declined from 0.8 to 0.1-0.3 and the cut-through number was increased greatly. The critical load in the scratch test exceeds 100 N, which shows a high adhesion strength. Moreover, the corrosion resistance of the TiN/ZrO₂ multilayers was improved significantly at the modulation period of 100 nm and 200 nm.     

Plasma immersion ion implantation induced improvements of mechanical properties, wear resistance, and adhesion of diamond-like carbon films deposited on tool steel

Nitrogen-rich layers are formed on the surface of JIS-SKH51 tool steel substrates using the plasma immersion ion implantation (PIII) technique. An unbalanced magnetron sputtering (UBMS) system is then used to coat the steel substrates with diamond-like carbon (DLC) films of various thicknesses. The adhesive strength and wear resistance of the DLC films are then examined by performing nanoscratch and nanowear tests. Finally, the microstructures of the DLC films are analyzed using TEM and Raman spectroscopy. The nanoindentation test results show that the PIII treatment yields an effective improvement in both the hardness and the Young's modulus of the SKH51 substrates. Moreover, cross-sectional observations show that the implantation depth and microstructure of the nitrogen-rich surface layer are dependent on the nitrogen/hydrogen flow ratio used in the PIII process. The nanoscratch test results show that the PIII treatment improves the adhesion of the DLC film to the steel substrate. Furthermore, the Raman spectroscopy results indicate that the use of hydrogen in the PIII process limits the increase in the I(D)/I(G) ratio by increasing the DLC film thickness. Finally, the nanowear test results show that the deposition of a DLC coating with a sufficient thickness yields a significant improvement in the wear resistance of the steel substrate.     

钛中间层对改性层结构及性能的影响

用XPS和GXRD研究了铝合金等离子体基离子注入氮后再注入钛最后复合注入氮和钛改性层的成分深度分布及相结构 ,用XTEM观察了改性层截面的组织结构 ,用AFM观察了改性层的表面形貌 ,在此基础上测量了改性层的纳米硬度 ,进行了球盘摩擦磨损试验。结果表明 ,钛中间层使复合改性层的厚度有效增加 ,主要由α Ti,TiN及TiO2 组成 ,且TiN及TiO2 弥散分布在α Ti基材中 ,使表面形貌有所改善 ,使表面硬度及耐磨性明显提高。     

Fluorine and carbon ion implantation and deposition on metals by plasma source ion implantation

Deposition of fluorine containing diamond-like carbon films is an effective solution for the improvement of machine parts in an aggressive aqueous environment when the combination of a hydrophobic surface with good corrosion protection and low friction coefficients is required. Stainless steel and silicon were treated by plasma source ion implantation using the gases CF₄, C₆F₆ and C₆H₅F, in the latter case with previous methane implantation. Depending on the plasma gas there are differences in the fluorine content, depth distribution, film thickness, water contact angle and friction coefficient.     

Electrochemical studies of stainless steel implanted with nitrogen and oxygen by plasma immersion ion implantation

Plasma Immersion Ion Implantation (PIII) of stainless steel with nitrogen at temperatures lower than 400 °C has been reported to increase the hardness of the material by several times. However, expectations that the corrosion resistance will remain unaffected after implantation were not found to be so. In the present study the influence of post-oxygen implantation on the corrosion resistance of nitrogen implanted stainless steel is presented. Stainless steel samples were subjected to oxygen, nitrogen and post-oxygen ion implantation at different temperatures. GIXRD and microRaman studies of the implanted samples showed that oxygen implantation leads to the formation of an oxide layer consisting of corundum and spinel structures. The corrosion properties of the implanted samples were studied by potentiodynamic polarization and electrochemical impedance techniques in 3.5% NaCl solution. After nitrogen implantation the corrosion current increased and the corrosion potential shifted to the less noble side to − 0.486 V as compared to − 0.284 V for the substrate. Oxygen implantation at 400 °C shifted the corrosion potential to the nobler side to − 0.2 V with decrease of corrosion current. For post-oxygen ion implantation at temperatures lower than 400 °C, the corrosion current was higher than the substrate and the corrosion potential was also on the less noble side. However, post-oxygen ion implantation at 400 °C after nitrogen ion implantation resulted in improved corrosion resistance as the corrosion potential shifted to nobler side and the corrosion current was lower than that of substrate.