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。     

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。     

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．     

氮含量对脉冲偏压电弧离子镀CNx薄膜结构与性能的影响

用脉冲偏压电弧离子镀设备在保持脉冲偏压一致和工作气压恒定的条件下,控制不同氮流量在硬质合金基体上制备了不同氰含量的CNx薄膜.用SEM,GIXRD,XPS,激光Raman谱和纳米压入等方法分别研究了薄膜的表面形貌、成分、结构与性能.结果表明,随着氮流量的增加,薄膜中氮含量先是线性增加然后趋于平缓,薄膜呈非晶结构且为类金刚石薄膜,其硬度与弹性模量随着氮含量增加先增加后下降,在x=0.081时出现最大值,分别为32.1 GPa和411.8 GPa.分析表明,通过氮含量的改变而使sp3键含量发生改变是影响薄膜性能变化的重要因素.     

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。     

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．     

脉冲偏压对TiAlCN薄膜结构与力学性能的影响

利用多弧离子镀-磁控溅射复合技术通过改变脉冲偏压在Si片与SS304基体表面制备了TiAlCN薄膜,研究了不同脉冲偏压对薄膜结构和力学性能的影响。薄膜成分、表面形貌、相结构及力学性能分别利用能量弥散X射线谱(EDS)、扫描电镜(SEM)、X射线衍射(XRD)和纳米压痕仪等设备进行表征。结果表明,随着脉冲负偏压的增加,薄膜中Ti元素的含量先减小后增大,而Al元素有相反的变化趋势。适当增大脉冲偏压,薄膜表面颗粒、凹坑等缺陷得到明显改善。物相分析表明TiAlCN薄膜主要由(Ti,Al)(C,N)相,Ti4N3-x相和Ti3Al相组成。薄膜平均硬度与弹性模量随脉冲负偏压的增加先增大后减小,在负偏压-200 V时达到最大值分别为36.8 GPa和410 GPa。     

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。     

脉冲偏压电弧离子镀C-N-Cr薄膜的成分、结构与性能

用脉冲偏压电弧离子镀设备在保持偏压一致和工作气压恒定的条件下,控制不同氮(N)流量,在硬质合金基体上制备了不同成分的C-N-Cr薄膜.用SEM,XPS,GIXRD,激光Raman谱和纳米压入等方法分别研究了薄膜的表面形貌、成分、结构与性能.结果表明,随着N流量增加,薄膜中N含量先是线性增加然后趋于平缓,Cr含量先是基本保持不变然后线性减少.在N流量不超过20 mL/min时,薄膜保持较高的硬度(＞30 GPa)与弹性模量(＞500 GPa);当N流量超过20 mL/min时,薄膜硬度与弹性模量急剧下降,在N流量为100 mL/min时硬度与弹性模量仅为13.6与190.8 GPa.     

脉冲偏压对电弧离子镀非晶氧化钛薄膜性能的影响

用脉冲偏压电弧离子镀技术在玻璃基片上制备均匀透明的氧化钛薄膜，通过改变脉冲偏压幅值，考察其对氧化钛薄膜性能的影响。结果表明，沉积态薄膜为非晶态；脉冲偏压对薄膜性能有明显的影响。随偏压的增加，薄膜厚度、硬度和弹性模量均先增大后减小，前者峰值出现在-100-200V负偏压范围，后两者则在-150～250v范围：-300v偏压时的薄膜硬度最高；达到原子级表面光滑度，RRMs为0．113nm，薄膜折射率也最高，在λn=550nm达到已有报道的最高值2．51，此时薄膜具有最好的综合性能。文中对脉冲偏压对薄膜性能的影响机理也进行了分析。     

Effects of nitrogen pressure and pulse bias voltage on the properties of Cr-N coatings deposited by arc ion plating

Cr-N coatings were deposited on 1Cr18Ni9Ti stainless steel in the pure N₂ atmosphere by arc ion plating (AIP). The relationships between deposition parameters and coating properties were investigated. X-ray diffraction showed a phase transformation from CrN + Cr₂N + Cr → CrN + Cr → CrN and the CrN preferred orientation changed from (200) to (220) as N₂ pressure increased. Increasing bias voltage led to CrN preferred orientation changed from (200) to (220) and the formation of Cr₂N. XPS results indicated that chemical composition of the coatings changed as N₂ pressure increased but it changed little with bias voltage. The lower melting point of chromium nitride formed on target surface induced the increase of macroparticles and deposition rate with increasing N₂ pressure; and bias voltage had an obvious effect on reducing macroparticles of the Cr-N coatings. Residual stresses were measured by substrate curvature technique, and the changing tendency coincided with the microhardness of the coatings.     

Effects of incorporation of Si or Hf on the microstructure and mechanical properties of Ti-Al-N films prepared by arc ion plating (AIP)

Ti-Al-N, Ti-Al-Si-N and Ti-Al-Hf-N films were deposited on 1Cr11Ni2W2MoV stainless steel by arc ion plating (AIP) with a Ti₇₀Al₃₀, a Ti₆₀Al₃₀Si₁₀ and a Ti₆₈Al₃₀Hf₂ cathode, respectively. The effects of Si or Hf addition on the composition, microstructure and mechanical properties of the Ti-Al-N films were investigated by EPMA, TEM, SEM, XRD, micro-hardness and wear tests. The results show that all the deposited films possessed B1 structure. With the incorporation of Si or Hf, the texture of Ti-Al-N films remarkably changed from preferred orientation of (220) to mixture broadened orientations of (111), (200) and (220), the mean crystallite size of Ti-Al-N decreased from ~ 90 nm to ~ 30 and ~ 15 nm and no peaks of crystalline Si₃N₄ were detected from XRD analyses. Due to the addition of Si or Hf, the micro-hardness of Ti-Al-N films increased remarkably from 23.5 Gpa to 33.6 or 29.5 GPa, and the wear resistance was also enhanced. The effects of incorporation of Si or Hf on the microstructure and mechanical properties of Ti-Al-N films are discussed.     

Influence of Si content and growth condition on the microstructure and mechanical properties of Ti-Si-N nanocomposite films

Thin films of Ti-Si-N have been prepared by ion beam assisted deposition (IBAD) from two Ti and Si targets. The silicon concentration in the deposited coatings is varied between 0 and 23.7 at.%. The influence of Si content and growth conditions on the microstructure and mechanical properties were investigated using XPS, AFM, XRD and nanoindenter. These nanocomposite coatings exhibit improved mechanical properties in comparison with TiN deposited under the same condition. The hardness measured by nanoindentation reached 42 GPa in Ti-Si-N films containing 11.32 at.% of Si, whereas TiN films only had a value of about 18 GPa. AFM showed that the finest grain size of Ti-Si-N appeared to be 5 nm when Si content was 11.32 at.%. From XPS and XRD results, the microstructures of the high hardness samples were found to consist of nanocrystal TiN grains and amorphous Si₃N₄.     

Influence of pulse parameters on the microstructure and microhardness of nickel electrodeposits

Square-wave cathodic current modulation was used to electrodeposit fine-grained nickel from an additive-free and saccharin-containing Watts bath. The influence of pulse on-time, off-time, peak current density and saccharin on the grain size, surface morphology, crystal orientation, and microhardness was determined. The study showed that at constant off-time and peak current density, the crystal size of the deposits was found initially to decrease with pulse on-time before it started to increase with further increase in on-time. The crystal orientation progressively changed from a (111) texture at the on-time of 0.1 ms to a strong (200) texture at an on-time of 8 ms. An increase in the pulse off-time at constant on-time and peak current density resulted in a progressive increase in crystal size. However, the crystal orientation remained unaffected with increasing off-time. An increase in peak current density resulted in considerable refinement in crystal size of the deposits. The crystal orientation progressively changed from an almost random distribution at the lowest peak current density of 0.2 A/m² to a strong (200) texture at a peak current density of 2.0 A/m². The nanocrystalline nickel with grain size in the order of 30 nm can be produced from saccharin-containing Watts' baths. In contrast, when using an organic-free Watts' bath and similar pulse-plating conditions, the grain size can only be refined down to about 80-100 nm. The microhardness of deposits is related with grain size: when the grain size is large, the microhardness is consistent with Hall-Petch law (HPL); when the grain size is ultrafine, “nano-effect” would be generated, the microhardness is against HPL.     

Effect of bias voltage on microstructure and nanomechanical properties of Ti films

In order to investigate nanomechanical properties of nanostructured Ti metallic material, pure Ti films were prepared by magnetron sputtering at the bias voltage of 0-140 V. The microstructure of Ti films was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM). It is interesting to find that the microstructure of pure Ti films was characterized by the composite structure of amorphous-like matrix embodied with nanocrystallines, and the crystallization was improved with the increase of bias voltage. The hardness of Ti films measured by nanoindentation tests shows a linear relationship with grain sizes in the scale of 6-15 nm. However, the pure Ti films exhibit a soft tendency characterized by a smaller slope of Hall-Petch relationship. In addition, the effect of bias voltage on the growth orientation of Ti films was discussed.     

Effect of substrate bias voltage on the texture and microstructure of Cu thin films deposited by ion beam deposition

Cu thin films deposited by non-mass separated ion beam deposition under various substrate bias voltages were investigated. The film textures and microstructure were analyzed by X-ray diffraction and field emission scanning electron microscopy, and the resistivity of the film was measured with the Van der Pauw method. It was found that the optimum negative substrate bias voltage for Cu films was −50 V. The Cu films deposited without substrate bias voltage showed a columnar grain structure with small grains and random orientation. However, when a substrate bias voltage of −50 V was applied, the Cu films had a non-columnar structure with a strong (111) texture and large grains. The electrical resistivity of the Cu films decreased remarkably with increasing negative substrate bias voltage, and reaching a minimum value of 1.8±0.13 μΩ cm at the substrate bias voltage of −50V.     

基片偏压对电弧离子镀ZrN薄膜微结构和表面形貌的影响(英文)

在不同的基片偏压下利用电弧离子镀技术制备氮化锆薄膜,以考察基片偏压对氮化锆薄膜微结构和表面形貌的影响。利用XRD、EPMA和FE-SEM等技术对不同偏压时得到ZrN薄膜的相结构、成分和表面形貌进行表征。结果表明,薄膜中存在立方氮化锆和六方纯锆相;随着基片偏压的增大,薄膜的择优取向由(111)变为(200),最后变为(111),晶粒尺寸由30nm减小至15nm。同时发现,随着基片偏压的增大,薄膜微结构由明显的柱状特征变为致密的等轴晶特征,表明由偏压增强的离子轰击能有效抑制柱状晶生长;薄膜沉积速率和锆氮摩尔比随着基片偏压的增大先增大后减小,在-50V时达到最大。     

调质结构对Ti-TiN-Zr-ZrN多层膜力学性能影响

采用真空阴极电弧离子镀技术,在TC11钛合金和单晶Si片表面分别沉积不同调制周期、不同R_Ti/TiN:R_Zr/ZrN调制比和不同厚度的Ti-TiN-Zr-ZrN多层膜。用扫描电镜、X射线衍射仪、划痕仪、显微硬度计和应力测试仪分析测试了多层膜的截面形貌、厚度、结合力、硬度和残余应力;重点研究了调制周期、调制比和膜层厚度等调制结构的改变对多层膜残余应力和相关性能的影响。结果表明：增加调制周期,则残余应力降低,结合力和硬度均增大;降低RTi/TiN:RZr/ZrN调制比,则残余应力增大,结合力下降,硬度增加;增大多层膜厚度,则残余应力略有上升,结合力和硬度都提高,当膜层厚度达到7.54μm后,硬度稳定在30Gpa左右。     

Effect of bias voltage on microstructure and properties of Ti-doped graphite-like carbon films synthesized by magnetron sputtering

Ti-doped graphite-like carbon (GLC) films with different microstructures and compositions were fabricated using magnetron sputtering technique. The influence of bias voltages on microstructure, hardness, internal stress, adhesion strength and tribological properties of the as-deposited GLC films were systemically investigated. The results showed that with increasing bias voltage, the graphite-like structure component (sp² bond) in the GLC films increased, and the films gradually became much smoother and denser. The nanohardness and compressive internal stress increased significantly with the increase of bias voltage up to −300 V and were constant after −400 V. GLC films deposited with bias voltages in the range of -300--400 V exhibited optimum adhesion strength with the substrates. Both the friction coefficients and the wear rates of GLC films in ambient air and water decreased with increasing voltages in the lower bias range (0--300 V), however, they were constant for higher bias values (beyond −300 V) . In addition, the wear rate of GLC films under water-lubricated condition was significantly higher for voltages below −300 V but lower at high voltage than that under dry friction condition. The excellent tribological performance of Ti-doped GLC films prepared at higher bias voltages of −300--400 V are attributed to their high hardness, tribo-induced lubricating top-layers and planar (2D) graphite-like structure.