反应磁控溅射(CrMoTaNbVTi)N多主元薄膜的微观组织与机械性能研究

本文采用直流反应磁控溅射方法,通过溅射（CrMoTaNbV）镶嵌靶和纯Ti靶制备了(CrMoTaNbVTi)N多主元氮化物薄膜。研究了不同氮气流量比RN对(CrMoTaNbVTi)N薄膜的微观结构、力学性能和摩擦学性能的影响。结果表明,当RN=0% 和10%时薄膜为简单的体心立方结构,当RN=20%、30% 和40%时为简单的面心立方结构。随着氮气流量比RN的增大,表面颗粒逐渐减小,断面柱状晶更为致密,同时(CrMoTaNbVTi)N薄膜的残余应力、膜基结合力、硬度和弹性模量逐渐增大,且当RN=40%时达到最大值,分别为-3.3 GPa, 352 mN, 25.6±1.2 GPa 和 278.8±11.2 GP。RN =40%制备的氮化物薄膜具有最小的比磨损率,相较合金薄膜降低了约1个数量级,表现出优异的耐磨损性能。     

AlCrTaTiZrN_x高熵合金纳米涂层的微观组织和力学性能研究

通过热压方法制备AlCrTaTiZr高熵合金合金靶材,采用磁控溅射方法在抛光后Si基体表面制备AlCrTaTiZrNx高熵合金涂层,并用扫描电镜、X射线衍射和纳米压痕仪等研究了靶成分、相结构及涂层的微观形貌、成分和常规力学性能。结果表明,AlCrTaTiZr高熵合金靶材为体心立方结构,AlCrTaTiZrNx高熵合金薄膜均匀致密,未通入氮气的薄膜为非晶态,通入氮气的薄膜晶体结构均为简单的面心立方结构。当氮气流量百分比为10%时,薄膜力学性能最好,其硬度和杨氏模量分别达到了22.9GPa和234.77GPa。     

不同氮气流量AlCrTaTiZr高熵合金氮化物薄膜扩散阻挡性能研究

目的 提高铜互连扩散阻挡层的失效温度。方法 采用磁控溅射方法制备了不同氮气流量下的Cu/AlCrTaTiZrNx/Si高熵合金薄膜体系,使用真空退火炉对Cu/AlCrTaTiZrNx/Si高熵合金薄膜体系分别进行600、700、800、900 ℃的真空退火,并利用扫描电子显微镜（SEM）、原子力显微镜（AFM）、X 射线衍射仪（XRD）以及透射电子显微镜（TEM）等表征手段对薄膜的组织结构、三维形貌等进行表征。结果 不通入氮气时,高熵合金薄膜为非晶状态。随着氮气流量的增加,薄膜的结晶性越来越好,薄膜为FCC结构。随着氮气流量的增加,高熵合金薄膜表面粗糙度呈现下降的趋势,在氮气流量为20%时,高熵合金氮化物薄膜的致密性最好。Cu/AlCrTaTiZrN20/Si薄膜体系的扩散阻挡层结构主要为非晶包裹的纳米晶结构。薄膜在800 ℃退火后,没有Cu-Si化合物存在,薄膜方阻为0.0937Ω/□;在900 ℃退火后,Cu/AlCrTaTiZrN20/Si薄膜体系中Si基体部分出现不规则五边形状的大颗晶粒Cu-Si化合物。结论 AlCrTaTiZrNx高熵合金氮化物薄膜的扩散阻挡性能随着氮气流量的增加,呈现先增加后降低的趋势。在氮气流量为20%时,高熵合金氮化物薄膜的扩散阻挡性能最优,800 ℃高温退火后仍发挥阻挡作用。     

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.     

COMPOSITION, MICROSTRUCTURE AND PROPERTIES OF C–N–Cr FILMS DEPOSITED BY PULSED BIAS ARC ION PLATING

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.     

EFFECT OF NITROGEN CONTENT ON THE MICROSTRUCTURE AND PROPERTIES OF CNx FILMS DEPOSITED BY PULSED BIAS

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氮含量的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.     

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.     

轴向磁场对电弧离子镀TiN薄膜组织结构及力学性能的影响

为了研究轴向磁场对薄膜结构及力学性能的影响规律,采用电弧离子镀方法在高速钢基体上沉积了TiN薄膜,利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、轮廓仪和纳米压痕仪考察了外加轴向磁场对薄膜化学成分、组织结构、硬度及弹性模量的影响。结果表明:外加轴向磁场对TiN薄膜的组织结构及力学性能有明显影响。磁场强度越高,薄膜表面颗粒及溅射坑越大,薄膜表面粗糙度增大;薄膜中N含量随着磁场强度增加而增大,而Ti含量则显示出相反的趋势;磁场对薄膜择优取向有明显影响,随着磁场强度增加,薄膜(111)取向增强,而后逐渐转变为(220)择优;薄膜硬度和弹性模量随着磁场强度增加先增加而后降低,在磁场强度为50Gs时分别达到最大值28.4GPa与415.4GPa。     

氮氩比对模具钢表面镀CrAlN薄膜形貌和性能的影响

目的 提高H13模具钢的表面性能,延长模具使用寿命.方法 采用多弧离子镀技术,以氮气作为反应气体,通过改变氮气流量的方法制备出不同原子含量的CrAlN薄膜,研究氮氩比对CrAlN薄膜表面形貌、组织结构、硬度、结合力、抗高温氧化性及耐腐蚀性的影响.结果 随着氮氩比增加,CrAlN薄膜表面大颗粒数量减少,大颗粒尺寸变小,薄...     

氮氩流量比对磁控溅射CrAgCeN涂层摩擦学性能的影响

目的 研究不同氮氩流量比对磁控溅射制备CrAgCeN涂层微观组织结构和摩擦学性能的影响。方法 采用扫描电子显微镜、X射线衍射仪对涂层表面形貌、成分和微观组织进行分析。采用纳米压痕仪、球盘式摩擦磨损试验机和白光干涉三维形貌仪,测试涂层的力学性能和摩擦学性能。结果 在给定的氮氩流量比下,CrAgCeN涂层主要有CrN、Cr₂N、Ag、AgN₃和Ce相构成,引入Ce、Ag可改变组织结构,随着氮氩流量比的增加,CrAgCeN涂层表面形貌由三角锥状转变为球状,在氮氩流量比为1.5时,涂层组织更加致密。涂层硬度和弹性模量随着氮氩流量比的增加呈现先升高后降低的趋势,在氮氩流量比为1.5时,硬度(H)和弹性模量(E)最大,分别为14.1 GPa和213.8 GPa;H/E值最高,为0.066,反映涂层具有较好的抗塑性变形能力。随着氮氩流量比的增加,摩擦因数和磨损率先减小后增大,在氮氩流量比为1.5时,涂层的摩擦因数和磨损率最小,分别为0.381和1.1×10^-6 mm³/(N·m),相比于氮氩流量比为0.6、1、3...     

AlCrTaTiZrV高熵合金氮化物扩散阻挡层的制备及其热稳定性

为研究氮气含量的变化对AlCrTaTiZrV高熵合金薄膜性能的影响,检验在最佳氮气含量下厚度为15 nm的(AlCrTaTiZrV)N扩散阻挡层的热稳定性。采用直流磁控溅射设备在N型Si(111)基底上溅射不同氮气含量的高熵合金氮化物;选取最佳氮气含量为制备条件,在硅基底上沉积15 nm厚的AlCrTaTiZrVN₁₀高熵合金氮化物为扩散阻挡层,并在阻挡层顶部沉积50 nm厚度的Cu膜,最终形成Si/AlCrTaTiZrVN₁₀/Cu三层堆叠结构。利用真空退火炉将Si/AlCrTaTiZrVN₁₀/Cu薄膜体系在500 ℃下进行不同时间的退火处理,用以模拟恶劣的工作环境。利用场发射扫描电子显微镜(FESEM)、原子力显微镜(AFM)、X射线衍射仪(XRD)及四探针电阻测试仪(FPP)对试样的表面形貌、粗糙度、物相组成及方块电阻和进行表征。试验结果为:当氮气含量低于10%时,高熵合金氮化物薄膜为非晶结构。当氮气含量为20%时,高熵合金氮化物薄膜呈现FCC结构,并随着氮气含量的增加,薄膜的结晶性得到提高。薄膜表面的粗糙度在氮气含量为10%时最低,R_a仅为0.124 nm。三层堆叠结构500 ℃退火8 h后,Cu表面发生团聚,薄膜的方阻维持在较低的0.070 Ω/□,且并未发现Cu-Si化合物。厚度为15 nm的非晶结构AlCrTaTiZrVN₁₀薄膜在500 ℃退火8 h后,依旧可以抑制Cu的扩散,表现出了优异的热稳定性及扩散阻挡性能。     

The effect of deposition conditions on the properties of TiN thin films prepared by filtered cathodic vacuum-arc technique

Thin TiN films were deposited at ambient temperature on silicon substrates using the filtered cathodic vacuum-arc technique. The nitrogen flow rate, deposition rate and substrate bias were varied systematically to investigate their effect on the mechanical and structural properties of the films. It was found that an increase in the nitrogen flow rate results in an increased hardness, surface roughness and grain size. The increased ion bombardment due to the higher amount of nitrogen ions makes film nucleation favourable on the denser (111) orientation. An increase in deposition rate results in an increase of stress, hardness and surface roughness. This is due to the increase in the momentum transfer resulting in film densification. Increasing the negative substrate bias decreases both the film stress and the hardness, which can be attributed to ion-induced stress-relief behaviour at higher momentum-energy transfer. The results demonstrate the dominant influence of ion-energy flux on the properties of the films.     

Phase evolution of tantalum nitride and tantalum carbide films with PBII parameters

Tantalum nitride and tantalum carbide films were fabricated using magnetron sputtering of tantalum followed by nitrogen and carbon plasma-based ion implantation (N-PBII and C-PBII). The phase evolution and morphology of the films were studied using glancing angle X-ray diffraction (GXRD) and transmission electron microscopy (TEM). It was found that the main phase in the tantalum nitride films was crystalline TaN_0.1 whose grain size increases with increasing implantation voltage and phase content increases with increasing implantation dose. In the tantalum carbide film, the main phase was Ta₂C. TaC phase also appeared as the implantation dose increased. XRD results from various glancing angles show that the phases with high nitrogen or carbon content, Ta₄N₅ and TaC, are present in the surface of the films. X-ray photoelectron spectra (XPS) from the tantalum carbide film reveal that the surface carbon content is higher than that of the inner film.     

Characterisation and tribological evaluation of nitrogen-containing molybdenum–copper PVD metallic nanocomposite films

This paper reports on the structural, mechanical and tribological properties of molybdenum–copper nanocomposite films ‘doped’ with small amounts of nitrogen, which contain either no nitride phase (i.e. the nitrogen is held in interstitial solid solution, mainly in molybdenum) or small amounts of lower nitrides (i.e. Mo₂N). All films were deposited on Si wafers, AISI M2 high speed steel and AISI 316 stainless steel by reactive sputtering using a hot-filament-enhanced dc unbalanced magnetron system. A systematic approach was adopted to investigate the evolution of metal/metal and ceramic/metal phase combinations with increasing nitrogen content (up to 40 at.% N) in the film. Coating composition and microstructure were determined by cross-sectional TEM, SEM and XPS. XRD was used to identify (where possible) metallic and metal-nitride phases. Mechanical properties such as hardness and elastic modulus were determined by low load Knoop and instrumented Vickers indentation measurements. Reciprocating sliding, micro-abrasion and impact tests were performed to assess tribological performance.

It was found that increasing the nitrogen gas flow rate from 0 to 15 sccm (and therefore nitrogen content in the film from 0 to 24 at.% N), refined significantly the coating microstructure from columnar to a dense and more equiaxed morphology, increasing the hardness whilst maintaining (almost constant) elastic modulus values, close to that of molybdenum metal. Further increases in the nitrogen gas flow rate resulted in films that appeared to contain significant fractions of the Mo₂N ceramic phase. SEM and cross-sectional TEM analyses of the film deposited at a nitrogen flow rate of 20 sccm (containing 36 at.% N) demonstrated a microstructure consisting of 50–100 nm wide columns, which contain small regions of contrast in dark-field images, of the order of 3–5 nm wide. A maximum hardness of 32 GPa and the highest hardness/modulus ratio was however found in the (predominantly metallic) film deposited at a nitrogen gas flow rate of 15 sccm. This film also performed best in both micro-abrasion and impact wear tests; in contrast, the ‘ceramic’ film (deposited at 20 sccm nitrogen flow rate) performed better in reciprocating sliding wear.     

Microstructure,Mechanical, and Tribological Properties of CNx Thin Films Prepared by Reactive Magnetron Sputtering

The microstructure,mechanical,and tribological properties of the carbon nitride(CN_x) thin films with different nitrogen contents deposited on high-speed steel substrates by reactive magnetron sputtering were studied.CN_x films with nitrogen contents from 10.7 to 28.2 at.%had an amorphous structure composing of the carbon bonds of sp~2C-C,sp~2C-N,and sp~3C-N.The TiN inter-layer cause the adhesion of CN_x films enhancement.The more nitrogen concentration led to larger film hardness and friction coefficient against GCr15 steel balls,but the wear rates decreased.     

Surface nitridation of titanium metal by means of a gas tunnel type plasma jet

The surface nitridation of titanium was carried out at a low pressure in nitrogen atmosphere using a gas tunnel type plasma jet. The titanium nitride (TiN) film, 10 μm thick and 2000 HV, could be formed in 10 s. The structure of the TiN film was investigated by XRD. The Vickers hardness on the surface of the film was measured. The effects of deposition conditions on the properties of TiN films (TiN thickness,Vickers hardness, etc.) were investigated, and the advantage of this deposition method was identified from those results.     

Effects of nitrogen content on structure and mechanical properties of multi-element (AlCrNbSiTiV)N coating

AlCrNbSiTiV metallic and nitride films were deposited by reactive radio-frequency unbalanced magnetron sputtering. The composition, microstructure and mechanical properties of the coatings deposited at different nitrogen flow rates were evaluated. The deposited AlCrNbSiTiV metallic film has an amorphous structure. The nitride films, regardless of the nitrogen flow ratio, were found to have only an FCC structure register on the XRD profiles. A Stoichiometric nitride ratio, i.e. (Al,Cr,Nb,Si,Ti,V)₅₀ N₅₀ is attained for a nitrogen flow ratio (R_N) of 10% and higher. At the lowest nitrogen flow ratio there is a preferred (200) orientation; however the films become less textured at higher nitrogen flow ratios. Nano-grained structures are obtained for all flow ratios, with grain sizes ranging from 8.7 to 12.3 nm. At the highest nitrogen flow rates the coatings have a compressive stress of around 4.5 GPa. The (Al,Cr,Nb,Si,Ti,V)₅₀ N₅₀ nitride coatings have both a high hardness and elastic modulus of 41 and 360 GPa, respectively. The maximum H/E ratio occurs at a nitrogen flow ratio of 20%.     

N2流量比对复合磁控溅射Zr-B-N薄膜结构和性能的影响

目的 在反应沉积时补充金属离子,增加薄膜中金属氮化物硬质相的数量,优化复合磁控溅射Zr-B-N薄膜的制备工艺,揭示N2流量比（N2/(N2+Ar)）对Zr-B-N薄膜结构和性能的影响规律,进一步强化Zr-B-N纳米复合薄膜。方法 采用高功率脉冲磁控溅射和脉冲直流磁控溅射复合镀膜技术沉积Zr-B-N薄膜,借助X射线衍射仪、能谱仪、扫描电镜、纳米压痕仪、划痕测试仪和摩擦试验机,研究N2流量比对Zr-B-N薄膜成分、微观结构、力学性能和摩擦性能的影响。结果 Zr-B-N薄膜具有典型的纳米复合结构,即BN非晶层包裹着ZrB2、Zr3N4、Zr2N、ZrN等纳米晶,所有Zr-B-N薄膜均沿（100）晶面择优生长。随着N2流量的增加,（100）晶面的衍射峰宽化加剧;薄膜硬度由36.2 GPa下降到21.0 GPa;膜/基结合力逐渐增强,临界载荷从34.8 N增加到55.8 N;摩擦系数逐渐增大。当N2流量比为42.9%时,摩擦系数相对较低,约为0.48,归因于薄膜内形成了沿（220）晶面生长的ZrN相,从而起到了良好的减摩作用。结论 当N2流量比为42.9%时,Zr-B-N薄膜具有纳米复合结构和良好的各项性能。     

铝质基体上Ti(C,N)/TiN多元多层膜工艺参数研究

首先在大范围内调节负偏压和基体温度两个参数，实现在铝质材料基体上沉积与基体结合良好的TiN膜，在此基础上通过调节N2、C2H2工作气氛流量比及Ti(C，N)、TiN膜层的层数，沉积了3类不同的膜，并对其力学与摩擦学性能进行了考察。结果表明：在(N2 C2H2)总流量一定的情况下，C2H2流量增大，则使Ti(C，N)膜层中含C量增多，膜层硬度提高，但韧性变差，表面变粗糙；在总厚基本不变的情况下，层数增多，单层变薄，使膜材晶粒细化，硬度提高，韧性变好。在3类膜中，1#膜C2H2流量适当且膜层数最多(6层)，其摩擦学性能表现最好，临界荷载为76N，显徼硬度为1911HV0.1，与基体相比，耐磨性提高了10倍多。     

稀土含量对Ti6Al4V钛合金等离子渗氮层组织和摩擦学性能的影响

目的研究稀土含量对Ti6Al4V钛合金表面等离子体渗氮层结构和性能的影响。方法运用等离子表面改性技术对Ti6Al4V(TC4)钛合金进行等离子渗氮处理,渗氮过程中通入不同含量的稀土作为催渗剂,以获得钛合金表面强化层。利用金相显微镜和扫描电子显微镜(SEM)观察渗氮层组织,用X射线衍射仪(XRD)分析渗层相组成,用能谱仪(EDS)检测渗层的化学成分,用维氏显微硬度计测量渗层的显微硬度,用球-盘式摩擦磨损试验机和三维轮廓仪检测渗层的摩擦磨损性能。结果TC4钛合金表面等离子渗氮层结构包括表面化合物层(主要成分为δ-TiN)和扩散层(主要为N原子扩散形成的N-Ti固溶体),加入稀土可以促进N原子向基体的扩散,提高渗氮速度。渗层厚度增加,硬度和耐磨性能提高,扩散层使钛合金基体与化合物层之间的硬度梯度更加平缓。当稀土通入速率为60 mL/min时,渗层厚度可达155μm,表面硬度为1275HV0.05,摩擦系数降到0.27,磨损率明显降低。结论钛合金等离子渗氮过程中加入稀土可以有效提高渗速,改善渗氮层硬度,提高材料表面的耐磨性能。