MICROSTRUCTURE OF Ti－B－NFILM AND INTERFACEFORMED BY N ION BOMBARDMENTON A Ti－B FILM

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Composition and structure of Ti-C/DLC graded composite films

The Ti-C→DLC gradient composite films were characterized systematically.The elemental depth profile and elemental chemical state evolution were determined by X-ray photoelectron spectroscopy (XPS).The transmission electron microscope (TEM) and high-resolution transmission electron microscopy (HRTEM) were used to study the structure of interfacial zone between DLC film and Ti-C layers.Results show that there are composition transition zone between DLC film and either Ti-C layer or steel substrate on condition that pre-deposited Ti layers on the steel substrate then plasma based bias deposited DLC films.In Ti-C graded layer,the chemical state of titanium and carbon are changed gradually.The structures of zone in Ti-C layer near the DLC film is consisted of random oriented nanocrystallines TiC dispersed in amorphous DLC matrix.The structure of the zone between DLC film and Ti-C graded layer is gradually changed too.     

Si和Y掺杂对(Ti,Al)N涂层结构和性能的影响

分别在未施加偏压和施加-100 V偏压条件下,利用磁控溅射技术在压气机叶片用1Cr11Ni2W2MoV热强不锈钢基体上沉积了Ti_0.3Al_0.7N和Ti_0.39Al_0.55Si_0.05Y_0.01N硬质涂层.实验结果表明,施加偏压及Si和Y掺杂明显改变了涂层的相结构,提高了涂层致密度,施加-100 V偏压且添加Si和Y的涂层为非晶结构,表面更加均匀致密.950℃氧化实验表明:Ti_0.39Al_0.55Si_0.05Y_0.01N涂层表面形成极薄且致密的Al₂O₃保护性氧化膜,大大降低了氧化速率.施加-100 V偏压的（Ti,Al）N和（Ti,Al,Si,Y）N沉积态涂层与未施加偏压的相应涂层相比,硬度均降低,尤其是（Ti,Al,Si,Y）N涂层变化显著.经950℃热处理,施加偏压的（Ti,Al,Si,Y）N涂层硬度略有降低,这是由于形成了硬度较低的B4相,而未施加偏压的（Ti,Al,Si,Y）N涂层硬度显著提高,这归因于B1相固溶体的分解.划痕测试结果表明,在实验载荷（50N）下,所有涂层均未出现连续性的剥落.     

SiC颗粒增强铝基复合材料基材上制备(Ti,Al)N涂层的研究

利用电弧离子镀技术在SiCp／2024Al基体上制备(Ti，Al)N涂层．研究了偏压对涂层的相组成、晶格常数和成分的影响及不同过渡层对涂层与基体结合性能的影响．结果表明，在较小偏压下，(Ti，Al)N涂层呈(111)择优取向；偏压在-150V时，涂层无择优取向；但随偏压继续升高，出现(200)和(220)择优取向．在添加Ti过渡层时，涂层与基体形成致密均匀的良好结合．同时通过设计梯度涂层，获得了厚度达105um的无裂纹(Ti，Al)N涂层．     

磁控溅射ZrSiN涂层对钛瓷结合强度的影响

探讨采用射频磁共溅射氮硅锆(ZrSiN)涂层作为扩散阻挡层(钛与瓷间的中间层),增强钛/瓷结合强度的可行性.结果表明:ZrSiN是含纳米结晶相ZrN和非晶相SiNx的纳米复合扩散阻挡层.无ZrSiN扩散阻挡层的钛经热循环后表面明显氧化,有ZrSiN扩散阻挡层处理后的钛表面经热循环后没有氧化钛,只有锆、硅、氮和氧元素,表明ZrSiN扩散阻挡层可有效阻挡钛在瓷烧结温度下氧化.三点弯曲试验表明ZrSiN涂层还可提高钛瓷结合强度.高硅含量的ZrSiN涂层处理的钛瓷结合强度更高,这与非晶相SiNx增多有关.     

MAIP镀TiN工艺对膜基结合的影响

本文介绍了用多弧离子镀膜（MAIP）技术在高速钢基片表面镀TiN工艺。通过离子轰击清洁和加热后,工件施加高的偏压并同时打开弧源,在膜基界面形成Ti、N、Fe、W、Mo的交混层。这层伪扩散层的存在,提高了膜基结合强度,为该膜的应用奠定了良好的基础。     

沉积偏压对AlCrTiN纳米复合涂层力学与抗高温氧化性能的影响

沉积偏压对涂层的结构与性能具有重要影响,为研究其对AlCrTiN纳米复合涂层成分、组织结构、力学与抗高温氧化性能的影响规律,采用磁控溅射技术,改变沉积偏压(-30、-60、-90、-120 V)制备四种AlCrTiN纳米复合涂层。利用X射线衍射仪、扫描电子显微镜、纳米压痕仪等仪器表征涂层的组织结构、成分、力学性能和抗高温氧化性能。研究结果表明：不同偏压下制备的AlCrTiN纳米复合涂层均为NaCl型fcc-(Al,Cr,Ti)N相结构。随着沉积偏压增大,涂层由沿(111)晶面择优生长转变为无明显的择优生长取向,晶粒尺寸降低,残余应力和硬度增大。偏压为-90 V与-120 V时,涂层表面更加致密,具有更高的硬度和弹性模量。在800℃与900℃氧化1 h后,所有涂层表面均生成一层连续致密的Al₂O₃膜。随着沉积偏压增加,氧化膜厚度逐渐降低,表明抗高温氧化性能逐渐增强,这是因为高偏压下涂层组织更致密,且晶粒更细小。研究成果对AlCrTiN纳米复合涂层的综合性能提升与工程化应用具有一定指导意义。     

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。     

Influence of substrate bias on microstructure and morphology of ZrN thin films deposited by arc ion plating

Zirconium nitride thin films were fabricated using arc ion plating under negative substrate biases to investigate the influence of substrate bias on the ZrN films. The phase, composition, and surface morphology of the ZrN ?lms, with respect to substrate bias, were studied by XRD, EPMA, and FE-SEM, respectively. The results show that cubic ZrN and hexagonal Zr phases form in the ZrN films. The competition between surface energy and strain energy makes the preferred orientation change from (111) to (200) and then back to highly (111) preferred orientation as a function of substrate bias. With the increase of bias voltage, the crystallite size of ZrN films reduces from 30 to 15 nm. Meanwhile, the film microstructure evolves from an apparent columnar structure to a highly dense equiaxed structure, indicating that the ion bombardment enhanced by substrate bias can suppress the columnar growth in the ZrN films. Deposition rate and mole ratio of Zr to N increase with the increase of bias voltage and reach the maximum at –50 V, and then show a decline trend when bias voltage further increases.     

渗硼对Ti(C,N)基金属陶瓷组织和性能的影响

采用粉末冶金法制备了纳米改性Ti(C,N)基金属陶瓷,并用固体粉末法对其进行了渗硼处理。研究了渗硼处理对Ti(C,N)基金属陶瓷微观组织以及抗弯强度和硬度的影响。结果表明:渗硼处理使Ti(C,N)基金属陶瓷中生成了CoB、TiB2、MoB2和石墨相。金属陶瓷的渗硼层由硼化物层、扩散层和基体区组成,厚度为100～140μm。硼化物层主要由CoB组成,扩散层含有较多孔隙,基体区存在富硼的渗硼影响区,影响区具有与Ti(C,N)基金属陶瓷近似的微观组织,但金属相含量较少。渗硼处理使Ti(C,N)基金属陶瓷的抗弯强度降低,主要是由材料中产生的热应力、组织应力以及组织变化引起的。Ti(C,N)基金属陶瓷的表面硬度提高48.7%。在由渗硼层表面向内部100～140μm范围内,硬度呈下降趋势。     

调制脉冲磁控溅射峰值靶功率密度对纯Ti镀层沉积行为的影响

调制脉冲磁控溅射可通过改变强/弱离化阶段的脉冲强度和占空比等电场参量,大幅调控镀料粒子的离化率、沉积能量和数量,可实现对沉积镀层形核与生长过程的精确把控。本文在非平衡闭合磁场条件下,采用调制脉冲磁控溅射技术,通过对其强离化脉冲阶段的脉冲宽度和靶功率进行调控获得持续增大的峰值靶功率密度,并在此条件下制备多组纯Ti镀层,对其微观形貌和力学性能进行了检测分析。研究结果表明,当强离化脉冲阶段的峰值靶功率密度由0.15 kW×cm-2持续增大至0.86 kW×cm-2时,所制备的纯Ti镀层具有11nm的平均晶粒尺寸、较其他峰值靶功率密度条件下制备镀层更为致密的组织结构、平整的表面质量（表面粗糙度Ra为11nm）和良好的力学性能。     

脉冲偏压对（Ti，Al）N／TiN／（Ti，Al）N多层复合涂层成分和硬度的影响

采用脉冲偏压多弧离子镀技术在Hss-Al高速钢上涂镀（Ti,Al）N/TiN/（Ti,Al）N多层复合涂层。所用设备为复合八阵弧离子镀膜生长系统。简要介绍了多层复合膜的镀层工艺过程。鉴于复合涂层中的Al含量对涂层的性能特别是抗磨损性能有极重要的影响。实验中重点考察了脉冲偏压幅对Al含量的影响。同时测试了复合涂层的Vickers硬度与偏压幅值的关系。研究结果推出,随着脉冲偏压幅值的增加,涂层中Al含量先增加,然后减少,偏压幅值为-150V时,Al含量高达36.41at%,偏压幅与涂声能显微硬度的关系有相似的规律,在偏压幅值为-150V时,7层复合膜的Vickers硬度达2750MPa左右,10层复合膜的硬度约2880MPa。     

MICROSTRUCTURE AND INDENTATION BEHAVIOUR OF MULTILAYER Ti-N FILM

The microstructure of Ti/TiN multilayer film was studied.It was shown by trans-mission electron microscopy of cross-sectional sample and respective secondary neutralsmass-spectroscopy depth profiling that the film has a periodic alternate multilayeredstructure:substrate /FeTi/Ti/Ti_2N/TiN/Ti_2N/Ti/Ti_2N/TiN...Ti/Ti_2N/TiN,whereFeTi and Ti_2N were the transition layers formed during ion plating.Cross-sectionalfracture surface of indentation samples had been obtained and studied with scanningelectron microscopy.It was shown that the multilayer film deformed during indentation,formed an indentation pit and a pile-up of materials around the indentation pit.As theapplied load increased deformation region extended beyond the film/substratc interfaceand into the substrate,the interlayer crack in the film and hole formation at the film/substrate interface were initiated.It is also shown that the multilayered Ti/TiN filmoffered better toughness in comparison with single layer TiN film.     

中频对靶磁控溅射合成TiN/Ti多层膜

利用新型中频对靶磁控溅射技术合成了一系列TiN／Ti多层膜．考察了不同Ti间隔层对多层膜硬度和结合力的影响,分析了膜表面大颗粒和坑的形成机理;利用正交实验法和方差分析探讨了靶电流、气体压力和基体偏压对薄膜表面缺陷密度的影响,对工艺参数进行了优化．结果表明,靶电流对缺陷密度的影响最大,气体压力次之,基体偏压对缺陷密度影响最小;当靶电流I=20A、气体压力ρ（Ar＋N2）=0．31Pa、基体偏压Vbias=-16m--300V和Ti间隔层厚度x-=0．12μm时,制备出硬度HV0．2N=2250、膜基间结合力（临界载荷）Lc=48N和表面缺陷密度ρs=58mm^-2的高质量TiN／Ti多层膜．     

Deposition of dense and smooth Ti films using ECR plasma-assisted magnetron sputtering

We report high quality Ti films grown in a novel electron cyclotron resonance (ECR) plasma-assisted magnetron sputtering (PMS) deposition system. The films are compared with films deposited by conventional direct current (DC) magnetron sputtering. Using ECR-PMS, the argon plasma bombardment energy and Ti film deposition rate can be controlled separately, with the substrate bias voltage under feedback control. Results from SEM, AFM, XRD and PAS (scanning electron microscopy, atomic force microscopy, X-ray diffraction and positron annihilation spectroscopy) show that the properties of Ti films prepared by ECR-PMS are greatly improved compared with conventional sputtering. SEM and AFM confirmed that ECR-PMS Ti films have a dense, smooth, mirror-like surface. Increasing the substrate bias of the ECR plasma from − 23 V to − 120 V while keeping a fixed sputtering bias voltage of − 40 V, the intensity of the (100) reflection of Ti film was a little strengthened, but (002) remained strongly preferred orientation. The XRD peak broadening of ECR-PMS Ti films is more than for conventional magnetron sputtering, due to grain refinement induced by Ar ion bombardment. Doppler broadening of PAS analysis reveals that the Ti films have fewer vacancy defects compared with films prepared by the conventional magnetron.     

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。     

微晶/纳米金刚石复合涂层的沉积与表征

采用偏压增强热丝CVD(HFCVD)法,通过引入惰性气体Ar,在经过甲醇新预处理方法处理后的硬质合金衬底表面成功沉积了微晶/纳米金刚石复合涂层。对金刚石复合涂层的表面形貌、成分、表面粗糙度进行了分析和研究。研究结果表明:新的预处理方法能够提高金刚石薄膜与衬底之间的附着强度。Ar的引入使得金刚石薄膜二次形核率更高,颗粒也更加细小,纳米金刚石复合涂层不但具有高的附着强度,而且具有非常低的表面粗糙度。对于拓展纳米金刚石涂层在精密加工领域中的应用具有一定的作用。     

静电纺丝制备连续SiC亚微米/纳米纤维

采用镶嵌靶反应磁控溅射技术,通过调节氮分压及基体偏压在M2高速钢基体表面制备了一系列耐热的(Ti,Al)N硬质薄膜,并用XRD,EDS及纳米压入法、划痕法等方法研究了(Ti,Al)N薄膜的成分、相结构与力学性能的关系。结果表明,氮分压和基体偏压对(Ti,Al)N薄膜取向及Ti、Al、N原子含量有明显影响,从而导致薄膜硬度及膜基结合性能发生变化。研究中,在氮分压为33.3×10-3Pa、基体偏压为-100V时制备的(Ti,Al)N薄膜力学性能最优,其纳米硬度为43.4GPa,达到40GPa超硬薄膜的要求。     

The Properties and Applications of MoS_2/Ti Composite Coatings in Dry Cutting and Forming

MOLYBDENUM DISULFIDE COATIGS have beensuccessfully used in vacuum and aerospaceenvironments in the past30years.In recent years,theapplication of MoS2coatings in ambient or high humidenvironments has been drawing increasing attentions.The main obstacle to the use of MoS coating inambient conditions is its sensitivity to humidity.Fig.1shows the cases that may degrade the humidityresistance of MoSx coatings,such as the columnarstructure,low density,edge orientation of the coatings;and…     

激光表面合金化原位制备Ti-Cu纳米晶金属间化合物涂层

利用激光表面合金化技术以铜粉为初始原料,在纯钛表面通过激光表面合金化原位反应成功制备了Ti-Cu纳米晶金属间化合物涂层。采用X-射线衍射仪(XRD)和高分辨透射电镜(HRTEM)分析了涂层的组成和组织结构,测试了涂层在不同载荷下的摩擦磨损性能。结果表明:通过激光表面合金化制备的涂层主要成分为Ti和金属间化合物TiCu、TiCu3、Ti3Cu相。涂层含有纳米晶Ti-Cu金属间化合物,晶粒尺寸为10~500nm。Ti-Cu金属间化合物涂层的摩擦因数随载荷增加而减小,体积磨损率在10-6~10-5 mm3/Nm数量级范围并随载荷的增加而增大,与纯钛底材相比,Ti-Cu金属间化合物涂层具有良好的耐磨性。