Microstructure and mechanical properties of pulsed DC magnetron sputtered nanocomposite Cr-Cu-N thin films

The nanocomposite Cr-Cu-N thin films have been deposited at a substrate temperature of 250 °C by a bipolar asymmetric pulsed DC reactive magnetron sputtering process. Different Cu contents ranging from 0.4 to 14.9 at.% were achieved. The structures of Cr-Cu-N thin films were analyzed by XRD. The surface and cross sectional morphologies of thin films were examined by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The nanoindentation and scratch tests were adopted to evaluate the mechanical and tribological properties of Cr-Cu-N coatings. The influences of Cu content on the structure, mechanical and tribological properties of Cr-Cu-N coatings were explored. It is observed that the columnar structure no longer exists when the Cu content exceeds 10.9 at.%. The stability of CrN phase in the coating is influenced by the Cu content. The scratching coefficient of thin films decreases with increasing Cu content. Sufficient adhesion and tribological properties of Cr-Cu-N coatings are achieved. The maximum average hardness around 20 GPa and scratching coefficient around 0.1 are found in the coatings with around 2.1 to 2.6 at.% Cu in this work.     

热处理对氮化铝化学镀铜组织性能的影响

目的优化化学镀铜氮化铝(AlN)基板的综合性能,掌握热处理对其镀层致密度、界面结合强度和热导率的作用机理,并对划痕膜层失效行为进行分析。方法采用化学镀铜法实现AlN陶瓷基板表面金属化,对其进行200~500℃热处理。利用X射线衍射仪、扫描电镜、激光导热仪,对Cu-AlN基板的物相结构、显微形貌、热学性能进行分析。采用划痕法对镀层结合力进行评价,并通过划痕形貌对膜层失效行为进行分析。结果未热处理的Cu-AlN基板表面存在鼓泡现象,结合强度为24.7 N,热导率为156.8 W/(m K)。热处理消除了Cu-AlN基板的鼓泡现象,300℃热处理的Cu-AlN基板综合性能优异,表面Cu颗粒分布均匀,结构较为致密,结合强度为32.6 N,热导率达163.8 W/(m K);当500℃热处理时,Cu-AlN基板表面存在氧化现象,形成CuO,结合强度急剧降低为18.5 N,热导率为161.2 W/(m K)。Cu-AlN基板的基膜失效方式为点剥离,随着载荷的增加,点剥离增多,膜层开裂,AlN逐渐裸露,Cu膜层磨损形貌宏观上表现为由塑性变形引起的犁沟磨损,芯部发生拉伸变形,边界呈现卷曲变形。结论对Cu-AlN进行合理热处理,可改善镀层表面组织与致密度,提高结合强度和导热性能。     

Microstructure and wear properties of TiC/FeCrBSi surface composite coating prepared by laser cladding

Titanium carbide particles reinforced Fe-based surface composite coatings were fabricated by laser cladding using a 5 kW CO₂ laser. The microstructure, phase structure and wear properties were investigated by means of scanning electron microscopy, transmission electron microscopy and X-ray diffraction, as well as dry sliding wear test. The results showed that TiC carbides were formed via in situ reaction between ferrotitanium and graphite in the molten pool during the laser-clad process. The morphology of TiC is mainly cubic and dendritic form; and the TiC carbides were distributed uniformly in the composite coating. The TiC/matrix interface was found to be free from cracks and deleterious phases. The coatings reinforced by TiC particles revealed higher wear resistance and lower friction coefficient than that of the substrate and FeCrBSi laser-clad coating.     

Evaluation of adhesion and fatigue of MoS2-Nb solid-lubricant films deposited by pulsed-dc magnetron sputtering

The thin film deposition for tribological applications becomes more and more widespread. The tribological performance of the overlay coatings correlates with coating-substrate adhesion. Hence, it is important to measure adhesive strength. The scratch adhesion test for thin films is extensively used. In this work, MoS₂-Nb coatings deposited by closed-field unbalanced magnetron sputtering (CFUBMS) have been scratch tested in two modes. A multi-mode operation was used as sliding-fatigue, like multi-pass scratching in the same track at different fractions of critical load (unidirectional sliding) and a standard mode using progressive load operation. Failure mechanisms are discussed according to examination of response of very dense microstructure and the adhesion value. The critical load to the first failure (L_C1) was 15 N but the final adhesion value from the film and substrate interface was 120 N (L_C2) as function of the coating thinning. The coefficient of friction (COF) from the multi-scratch for MoS₂-Nb started at a very high value of around 0.067, 0.073, and 0.093 under 5, 8, and 15 N loads respectively and then drops to 0.006, 0.035, and 0.065 at the end of the 1000 cycles. The most significant finding in the test is that when the multi-scratch passes reached to 1000 cycles, micro scale fatigue failures disappeared.     

Effects of Cu and Cu/Ti interlayer on adhesion of diamond film

Diamond film were deposited on the cemented WC + 6% Co substrates by a microwave plasma chemical vapor deposition (CVD) system. The effects of Cu and Cu/Ti as interlayer on adhesion of diamond film were investigated. The surface morphology and composition of the film and microstructure of film/substrate interface were examined by scanning electron microscopy (SEM), X-ray diffraction (XRD), electron probe microanalysis (EPMA) and Raman spectrometer, respectively. The adhesion of diamond film was evaluated by indentation adhesion testing. The results show that Cu/Ti would be a suitable interlayer system to improve film adhesion. It was considered that Cu atoms replaced most voids left by leached Co, recovered the surface strength and toughness, and inhibited the diffusion of Co to the substrate surface. Ti atoms act as promoter for diamond nucleation, and the formation of TiC enhanced the adhesion of diamond film. Furthermore, Cu/Ti interlayer system restrained the growth of diamond grain and promoted the formation of nano-crystalline, which increased the contact area of the film/substrate interface.     

The effect of substrate composition on the electrochemical and mechanical properties of PEO coatings on Mg alloys

Plasma electrolytic oxidation (PEO) is a unique surface treatment technology which is based on anodic oxidation forming ceramic oxide coatings on the surface of light alloys such as Mg, Al and Ti. In the present study, PEO coatings prepared on AZ91D, AZ31B, AM60B and AM50B Mg alloys have been investigated. Surface morphology and elemental composition of coatings were determined using scanning electron microscope (SEM) equipped with energy dispersive spectrometer (EDS). SEM results showed that the coating exhibited a porous top surface layer and a subsequent dense layer with micro-pores and shrinkage cracks. Phase analysis of coatings was carried out by X-ray diffraction (XRD). XRD analyses indicated that PEO coatings on AZ alloys had higher amount of Periclase (MgO) followed by the presence of Spinel (MgAl₂O₄) e.g. on the AZ91D alloy compared to that on AM series alloys. In order to examine the effect of substrate composition on adhesion strength of PEO coating scratch tests were carried out. Electrochemical corrosion tests were undertaken by means of potentiodynamic polarization technique in 3.5% NaCl solution at room temperature (20 ± 2 °C). Corrosion test results indicated that the corrosion rates of coated Mg alloys decreased by nearly two orders of magnitude as compared to bare Mg alloys. PEO coatings on AZ series alloys showed better corrosion resistance and higher adhesion properties than AM series alloys. In addition to the PEO processing parameters, such are mainly attributes of the compositional variations of the substrate alloys which are responsible for the formation, phase contents and structural properties of the PEO coatings.     

Elevated temperature repetitive micro-scratch testing of AlCrN,TiAlN and AlTiN PVD coatings

In developing advanced wear-resistant coatings for tribologically extreme highly loaded applications such as high speed metal cutting a critical requirement is to investigate their behaviour at elevated temperature since the cutting process generates frictional heat which can raise the temperature in the cutting zone to 700–900 °C or more. High temperature micro-tribological tests provide severe tests for coatings that can simulate high contact pressure sliding/abrasive contacts at elevated temperature. In this study ramped load micro-scratch tests and repetitive micro-scratch tests were performed at 25 and 500 °C on commercial monolayer coatings (AlCrN, TiAlN and AlTiN) deposited on cemented carbide cutting tool inserts. AlCrN exhibited the highest critical load for film failure in front of the moving scratch probe at both temperatures but it was prone to an unloading failure behind the moving probe. Scanning electron microscopy showed significant chipping outside the scratch track which was more extensive for AlCrN at both room and elevated temperature. Chipping was more localised on TiAlN although this coating showed the lowest critical loads at both test temperatures. EDX analysis of scratch tracks after coating failure showed tribo-oxidation of the cemented carbide substrate. AlTiN showed improved scratch resistance at higher temperature. The von Mises, tensile and shear stresses acting on the coating and substrate sides of the interface were evaluated analytically to determine the main stresses acting on the interface. At 1 N there are high stresses near the coating-substrate interface. Repetitive scratch tests at this load can be considered as a sub-critical load micro-scale wear test which is more sensitive to adhesion differences than the ramped load scratch test. The analytical modelling showed that a dramatic improvement in the performance of AlTiN in the 1 N test at 500 °C could be explained by the stress distribution in contact resulting in a change in yield location due to the high temperature mechanical properties. The increase in critical load with temperature on AlTiN and AlCrN is primarily a result of the changing stress distribution in the highly loaded sliding contact rather than an improvement in adhesion strength.     

Q235钢表面氩弧熔覆TiC复合涂层的组织与性能

以Ti粉、C粉、Fe粉为原料,利用氩弧熔覆技术在Q235钢表面原位合成了TiC增强Fe基复合涂层,分析了涂层的显微组织和物相,测定了涂层的硬度。结果表明:复合涂层与基体界面无气孔、裂纹,呈冶金结合;熔覆层组织由树枝晶、等轴晶组成,TiC主要分布于晶粒内和晶界处;涂层显微硬度随TiC含量的增加而增大。     

Corrosion and Nano-mechanical Behaviors of Magnetron Sputtered Al-Mo Gradient Coated Steel

A gradient three-layer Al-Mo coating was deposited on steel using magnetron sputtering method. The corrosion and nano-mechanical properties of the coating were examined by electrochemical impedance spectroscopy and nano-indentation tests and compared with the conventional electroplated cadmium and IVD aluminum coatings. Electrochemical impedance spectroscopy was performed by immersing the coated specimens in 3.5% NaCl solution, and the impedance behavior was recorded as a function of immersion time. The mechanical properties (hardness and elastic modulus) were obtained from each indentation as a function of the penetration depth across the coating cross section. The adhesion resistance of the coatings was evaluated by scratch tests on the coated surface using nano-indentation method. The results show that the gradient Al-Mo coating exhibits better corrosion resistance than the other coatings in view of the better microstructure. The impedance results were modeled using appropriate electrical equivalent circuits for all the coated systems. The uniform, smooth and dense Al-Mo coating obtained by magnetron sputtering exhibits good adhesion with the steel substrate as per scratch test method. The poor corrosion resistance of the later coatings was shown to be due to the defects/cracks as well as the lesser adhesion of the coatings with steel. The hardness and elastic modulus of the Al-Mo coating are found to be high when compared to the other coatings.     

Rolling contact fatigue and mechanical properties of titanium carbide film synthesized on bearing steel surface

The effect of plasma immersion ion implantation and deposition (PIII&D) titanium carbide (TiC) film on the rolling contact fatigue (RCF) life of coated on AISI52100 bearing steel surface is studied experimentally. Testing include plan-view optical microscopy (OM), X-ray diffraction (XRD), friction and wear behaviors, rolling contact fatigue life and nano-indentation measurements. XRD patterns show that titanium carbide phase is formed in the film, and the microhardness of treated samples is higher than that of substrate. Rolling contact fatigue failure tracks were observed using conventional light microscope. Surface wear and adhesive delamination existed. Results indicate that the maximum RCF life of the treated sample prolong by 6.5 times at a Hertzian stress level of 5.1 GPa and 90% confidence level, respectively. Comparison with the substrate, the maximum microhardness of treated specimen is increased by 28.4%. The friction coefficient decreased from 0.95 to 0.15 under identical wear conditions. This remarkable fatigue performance appears to be due to a combination of improved microstructure, adhesion, hardness and surface topography. Therefore, the PIII&D is regarded as one of the promising technologies for improving the RCF life of bearing.     

溶胶凝胶法在铝基片上沉积Si0x薄膜及结合性能

为了获得性能良好的蛋白质芯片的固相载体,采用溶胶-凝胶工艺并结合旋转涂布技术在Al基片上沉积硅氧化物薄膜,考察了薄膜的表面形貌、组成、结构以及与基片的结合性能.结果表明:酸性溶胶在Al基片上沉积薄膜容易产生较多较大的裂纹,严重影响薄膜的表面性能;以浓氨水为催化剂获得的碱性溶胶在Al基片上涂膜,干燥过程中产生的内应力较小,获得的SiOx薄膜表面较均匀,虽然仍存在少量裂纹,但较细小.添加少量DMF于碱性溶胶中可获得比表面积大、无裂缝、与基片结合强度较高的均匀非晶态硅氧化物薄膜,有望作为蛋白质芯片的固相载体.     

TC4合金表面氩弧熔覆TiCp/Ti基复合涂层组织及耐磨性

利用氩弧熔覆技术在TC4合金表面制备出TiC增强的Ti基复合涂层。利用SEM、XRD和EDS分析了熔覆涂层的显微组织;利用显微硬度仪测试了复合涂层的显微硬度;利用摩擦磨损试验机测试了涂层在室温干滑动磨损条件下的耐磨性能。结果表明:氩弧熔覆涂层组织均匀致密,熔覆层与基体呈冶金结合,涂层中有大量的TiC树枝晶和条块状TiC颗粒;复合涂层明显改善了TC4合金的表面硬度,HV平均硬度可达9GPa;复合涂层室温干滑动磨损机制为磨粒磨损和轻微粘着磨损。     

钛过渡层与硬质合金基体表面结合状况对金刚石薄膜附着力的影响

以WC-6％Co为基体,采用磁控溅射法,在原始试样、酸腐蚀试样以及酸蚀后进行氢等离子体脱碳处理的试样上制备Ti过渡层,然后碳化过渡层为TiC。在热丝化学气相沉积装置中,制备金刚石薄膜。研究三种不同试样上的金刚石薄膜与基体的附着力。结果表明,在原始试样上的金刚石薄膜在冷却过程中自动脱落;在经等离子体处理后的试样上,金刚石薄膜与基体间附着力高于在经酸蚀处理的试样上的金刚石薄膜与基体附着力。造成这种现象的主要原因可能是等离子体脱碳还原处理降低WC晶粒表面能,增强Ti与WC间的结合强度,导致TiC过渡层与WC基体结合强度增加,从而增加金刚石薄膜附着力。     

钛合金表面氩弧熔覆TiC增强复合涂层组织与性能分析

把石墨粉末预涂在钛合金表面上,利用氩弧熔覆技术成功制备出原位自生TiC增强的金属基复合涂层。利用扫描电镜、X射线衍射仪和能谱仪分析了熔覆涂层的显微组织,探讨了增强相TiC的生成机制;利用显微硬度仪测试了复合涂层的显微硬度并用磨损试验机考察了其在室温干滑动磨损条件下的耐磨性能。结果表明,氩弧熔覆涂层组织均匀致密,原位自生TiC呈树枝晶和细碎的条状均匀地分布于整个涂层中;由TiC增强的复合涂层明显地改善了钛合金的表面硬度．平均硬度约为700HV0．2且沿层深方向呈梯度分布;涂层在室温干滑动磨损条件下的耐磨性明显优于基体,约为钛合金的10．5倍．     

钛合金表面激光熔化沉积钛基复合材料涂层的组织及性能

通过激光熔化沉积TA15+30%TiC(体积分数)混合粉末,在TA15钛合金表面制备出钛基复合材料涂层,分析了涂层的组织、硬度及界面结合强度。结果表明,激光熔化沉积过程中原始TiC颗粒发生溶解,并在凝固过程中重新析出细小的TiC,TiC有等轴状及枝晶两种形态,涂层中存在部分未熔的TiC颗粒;涂层硬度达HRC 60;涂层与基体界面为完全冶金结合,涂层的界面结合强度大于310 MPa,抗剪切强度为330 MPa;经弯曲及热震试验后,涂层未出现剥落现象,表明涂层与基体具有很好的相容性     

氧的掺入对化学气相沉积TiCN涂层的影响

本文采用X射线衍射仪(XRD)、高分辨扫描电镜(HRSEM)、显微维氏硬度计、声发射划痕仪,研究了以化学气相沉积(CVD)法制备的TiCN和TiCNO涂层。通过对比涂层的相结构、组织形貌、硬度及结合强度,分析氧的掺入对TiCN涂层显微结构和力学性能,特别是结合强度的影响。结果表明:CVD制备的TiC0.81N0.48涂层截面呈柱状结构,硬度和结合强度分别为2 063 HV及127 N。掺入氧后的TiC0.61N0.44O0.15和TiC0.52N0.25O0.1涂层没有出现新的物相,为面心立方结构的TiCNO固溶体,具有(111)织构;氧的掺入细化了晶粒,使涂层转变为致密结构;其硬度分别提高至2 207 HV和2 753 HV,但与基体结合强度分别下降至88 N和63 N。     

锆合金表面涂层耐高温高压动水腐蚀性能的研究

目的 提高锆合金在高温高压环境中耐动水腐蚀性能。方法 利用多弧离子镀技术（MAIP）在Zr-4合金表面分别制备了Al2O3涂层和Cr/TiAlN复合涂层,利用磁控溅射技术（MS）在Zr-4合金表面制备了TiN涂层。通过堆外高压釜实验,对比研究了三种不同涂层的耐高温高压动水腐蚀性能,利用自动划痕仪检测膜基结合力,利用XRD分析涂层的物相成分,利用SEM观察涂层腐蚀前后的微观形貌,利用EDS对涂层元素种类与含量进行分析。结果 多弧离子镀技术制备的Al2O3涂层和Cr/TiAlN涂层致密度较高,但表面存在少量大颗粒与微孔洞;磁控溅射技术制备的TiN涂层均匀平整,表面大颗粒较少。Al2O3涂层、TiN涂层和Cr/TiAlN涂层可承受的临界载荷分别为26、16、26.5 N。在实验条件下,Cr/TiAlN涂层和TiN涂层表面均发生了剥落或腐蚀现象,且这两种试样表面均检测出大量的ZrO2,而Al2O3涂层几乎未被破坏,基体得到了充分防护。结论 利用多弧离子镀技术在Zr-4合金表面制备的Al2O3涂层和Cr/TiAlN涂层的膜基结合力较高,利用磁控溅射技术制备的TiN涂层的膜基结合性能较差,其中Al2O3涂层具备良好的耐腐蚀性能,在高温高压动水腐蚀环境中能够有效地保护锆合金基体。     

Enhanced tribological properties of PECVD DLC coated thermally sprayed coatings

This research investigates the enhancement of the tribological properties of various thermally-sprayed coatings (APS Ni-50Cr, APS Al₂O₃-13%TiO₂ and HVOF WC-17Co) on steel substrate, achieved through the deposition of a thin DLC-based film. Higher adhesive strength between thin films and thermally-sprayed coatings compared to the simple thin film/carbon steel system was found by scratch testing. Dry sliding ball-on-disk tests performed under lower contact pressure conditions (5 N normal load, 6 mm diameter alumina ball) indicated a significant decrease in wear rates and friction coefficients of thermally-sprayed coatings when the thin DLC-based film is employed; little differences exist between the tribological behaviour of the various thin film/thermal spray coating systems and that of DLC-based film on carbon steel. Under higher contact pressure conditions (10 N normal load, 3 mm diameter alumina ball), the thin film/WC-Co system exhibited the best wear performance. These results indicate the superior tribological performance of DLC/thermal spray coating systems, especially under severe contact conditions.     

Dependence of characteristics of LaB6 films on DC magnetron sputtering power

Lanthanum hexaboride(LaB₆) thin films were deposited on glass substrate by DC magnetron sputtering technology, and the AFM, XRD and scratch tests were used to characterize the deposited films. Influences of sputtering power on the microstructure and the bonding strength between the film and substrate were investigated. AFM observation proves that the dense films are obtained, and the surface roughness is below 4.3 nm. The LaB₆ film shows the crystalline structure with the grain less than 100 nm. The XRD pattern identifies that the crystal structure of the films is in accordance with that of bulk LaB₆, and the (100) crystal face is dominated. The average grain size decreases firstly and then increases with increasing power, and reaches the minimum of 40 nm when the sputtering power is 44 W. Moreover, the intensity of peaks in XRD pattern increases firstly and decreases afterward with increasing power. When the sputtering power is 50 W, the peak intensity reaches the maximum, showing an intense relationship between the power and crystal structures. The scratch test shows that interface bonding strength of the film/substrate is higher at the power of 44 W than the others, due to the formation of the nanosized crystals and their improved surface energy.     

Improvement of a-C:H film adhesion by intermediate layers and sputter cleaning procedures on stainless steel, alumina and cemented carbide

The adhesion of amorphous hydrogenated carbon (a-C:H) films deposited in a radio frequency (r.f.) plasma discharge on stainless steel, alumina and cemented carbide with different intermediate layers (Ni, Ti and TiC) and sputter cleaning procedures was studied. The composition of the carbon films and the intermediate layers as well as the interface between the coating and the substrate was determined by secondary ion mass spectroscopy (SIMS). The adhesion experiments were carried out using a scratch tester. Tested specimens were also studied by scanning electron microscopy (SEM) to reveal the morphology of the coatings and the scratches.

Without any intermediate layer, the a-C:H coatings generally had insufficient adhesion to the substrate materials studied. For stainless steel and cemented carbide substrates, the TiC intermediate layer and, for alumina substrates, the titanium intermediate layer gave the best adhesion values evaluated by the scratch test. Also, the sputter cleaning of the substrates prior to deposition was necessary for sufficient adhesion of the coating. The intermediate layers also change the failure mode of the coating in the scratch test in some cases.