Ti-B-C-N纳米复合薄膜结构及力学性能研究

利用反应磁控溅射方法在单晶硅和高速钢(W18Cr4V)基片上制备出不同C含量Ti-B-C-N纳米复合薄膜. 使用X射线衍射和高分辨透射电子显微镜研究了Ti-B-C-N纳米复合薄膜的组织和微观结构,用纳米压痕仪测试了它们的硬度和弹性模量. 结果表明,利用往真空室通入C₂H₂气体的方法制备得到的Ti-B-C-N纳米复合薄膜中,在所研究成分范围内只发现TiN基的纳米晶. 当C₂H₂流量较小时,C元素的加入可以促进Ti-B-C 关键词： Ti-B-C-N薄膜 磁控溅射 微观结构 力学性能     

Microstructure and mechanical properties of neoprene-montmorillonite nanocomposites

To investigate the microstructure and mechanical properties of neoprene-montmorillonite nanocomposite, three modified montmorillonite are used. An X-ray diffractometer is used to measure the corresponding change in d-spacing. Scanning electron microscopy is employed to investigate the morphology of the various composites. Transmission electron microscopy is employed to investigate the composite of montmorillonite and neoprene. The results indicate that the addition of montmorillonite enhances the mechanical properties of neoprene significantly.     

Influence of reactive gas and temperature on structural properties of magnetron sputtered CrSiN coatings

CrSiN coatings were deposited on stainless steel (Grade: SA304) and silicon Si(1 0 0) substrates, with varying argon-nitrogen gas proportions and deposition temperature, using reactive magnetron sputtering technique in the present work. The influence of sputtering (Ar) and reactive gas proportions (N₂) and temperature on the structural properties of the CrSiN coating was investigated. A small amount of silicon content (3.67 at.% Si) plays a crucial role in addition to the nitrogen content for the formation of different phases in the CrSiN coatings as observed in the present work. For example, the coating with comparatively low nitrogen content, 40% N₂, during deposition, formed a crystalline structure consisting of nano-crystalline CrN which is separated by an amorphous SiN phase, as evident from X-ray diffraction (XRD) and transmission electron microscopy (TEM), respectively. The formation of CrN(1 1 1) and Cr₂N(1 1 1) phases has occurred at 30% N₂ with 3.67% Si content, which transformed in to CrN(1 1 1) and CrN(2 0 0) with increase in N₂ content but with same Si content. The surface topography and morphology of the coatings were analyzed by atomic force microscopy (AFM) and field emission scanning electron microscopy (FESEM), respectively. A less columnar growth is observed in CrSiN coatings deposited at low argon content, Ar:N₂ (20:80), and with 3.67 at.% Si in the coatings. However, it becomes dense with increase in nitrogen content and temperature. The XRD analysis showed that the intensity of a dominating peak (1 1 1) is decreasing from (80:20) to (60:40) argon:nitrogen environment. With a further increase of nitrogen content, from (60:40), in the sputtering gas mixture, to (40:60) argon-nitrogen, there is a sudden increase in (1 1 1) peak and above (40:60), the peak reduction rate is very slow than the previous one. The (1 1 1) and (2 0 0) peak intensity variations are very limited due to high nitrogen content, above 50%, and considerable amount of Si atoms, 3.67 at.%, present in the CrN coatings.     

Microstructure and selected properties of hot-work tool steel with PVD coatings after laser surface treatment

The paper presents the effect of HPD laser treatment on the microstructure and selected properties of the PVD CrN, (Ti,Al) and Ti(C,N) coatings deposited onto hot-work tool steel substrates. The microstructure and surface topography of the investigated samples are characteristic of the diversified morphology connected with the applied laser beam power. Employment of laser beam at 0.7 kW power to the laser treatment of samples with Ti(C,N) coatings causes clear coating adhesion growth because of the diffusive processes induced by heat release. Because of the higher value of the (Ti,Al)N absorption coefficient one can state that the observed substrate materials change and finally coatings destruction in case of those samples is the most noticeable. The moderate effect of the laser beam treatment of the hot-work tool steel with the PVD coating was observed for CrN coatings. However, for laser beam power above 0.5 kW differences in the thermal expansion coefficients of the substrate materials and coatings generate coating crackings.     

Effect of gas flow ratio on the microstructure and mechanical properties of boron phosphide films prepared by reactive magnetron sputtering

Boron phosphide films were grown on silicon substrate by radio frequency reactive magnetron sputtering using boron target and hydrogen phosphine at different gas flow ratios (PH₃/Ar) at lower temperature. The chemical composition, microstructure and mechanical properties were characterized by X-ray photoelectron spectroscopy, X-ray diffraction, Raman spectrum, FTIR spectrum, surface profilometer and nano-indenter. The results indicate that the atomic ratio (P/B) rises from 1.06 up to 1.52 with the gas flow ratio increasing from 3/50 to 15/50. Simultaneously, the hardness and Young's modulus decrease from 25.4 GPa to 22.5 GPa, and 250.4 GPa to 238.4 GPa, respectively. Microstructure transforms from microcrystalline state to amorphous state along with the gas flow ratio increasing. Furthermore higher gas flow ratio leads to lower stress. The BP film prepared at the gas flow ratio of 3/50 can be contributed with the best properties.     

Deposition and characterization of TiAlSiN nanocomposite coatings prepared by reactive pulsed direct current unbalanced magnetron sputtering

This work reports the performance of high speed steel drill bits coated with TiAlSiN nanocomposite coating at different Si contents (5.5-8.1 at.%) prepared using a four-cathode reactive pulsed direct current unbalanced magnetron sputtering system. The surface morphology of the as-deposited coatings was characterized using field emission scanning electron microscopy. The crystallographic structure, chemical composition and bonding structure were evaluated using X-ray diffraction, energy-dispersive X-ray analysis, X-ray photoelectron spectroscopy, respectively. The corrosion behavior, mechanical properties and thermal stability of TiAlSiN nanocomposite coatings were also studied using potentiodynamic polarization, nanoindentation and Raman spectroscopy, respectively. The TiAlSiN coating thickness was approximately 2.5-2.9 μm. These coatings exhibited a maximum hardness of 38 GPa at a silicon content of approximately 6.9 at.% and were stable in air up to 850 °C. For the performance evaluation, the TiAlSiN coated drills were tested under accelerated machining conditions by drilling a 12 mm thick 304 stainless steel plate. Under dry conditions the uncoated drill bits failed after drilling 50 holes, whereas, TiAlSiN coated drill bits (Si = 5.5 at.%) drilled 714 holes before failure. Results indicated that for TiAlSiN coated drill bits the tool life increased by a factor of more than 14.     

Structural and mechanical properties of multi-element (TiVCrZrHf)N coatings by reactive magnetron sputtering

In this study, (TiVCrZrHf)N multi-component coatings with quinary metallic elements were deposited by reactive magnetron sputtering system. The composition, structure, and mechanical properties of the coatings deposited at different N₂ flow rates were investigated. The (TiVCrZrHf)N coatings deposited at N₂ flow rates of 0, 1, and 2 SCCM showed an amorphous structure, whereas those deposited at N₂ flow rates of 4 and 6 SCCM showed a simple face-centered cubic solid solution structure. A saturated nitride coating was obtained for N₂ flow of 4 SCCM and higher. By increasing N₂ flow to 4 SCCM, the hardness and modulus reached a maximum value of 23.8 ± 0.8 and 267.3 ± 4.0 GPa, respectively.     

Microstructure and mechanical properties of selective laser melted magnesium

The effects of laser processing parameters on the microstructure and mechanical properties of selective laser-melted magnesium were investigated. The results show that the microstructure characteristics of the laser-melted samples are dependent on the grain size of SLM magnesium. The grains in the molten zone coarsen as the laser energy density increases. In addition, the average hardness values of the molten zone decreases significantly with an increase of the laser energy densities and then decreased slowly at a relatively high laser energy density irrespective of mode of irradiation. The hardness value was obtained from 0.59 to 0.95 GPa and corresponding elastic modulus ranging from 27 to 33 GPa. The present selective laser-melted magnesium parts are promising for biomedical applications since the mechanical properties are more closely matched with human bone than other metallic biomaterials.     

Molecular structure and optical properties of PTFE-based nanocomposite polymer-metal coatings

The molecular organization of polytetrafluoroethylene (PTFE) thin coatings with incorporated Ag, Cu, and Mo nanoparticles that are deposited from an active gas component has been studied. Polyethylene terephtalate film coated by aluminium served as a substrate. The active gas component was produced by electron beam dispersion of original components in vacuum. The effect of metal particle size and its nature on the molecular structure of coatings have been investigated. Dichroism of thin nanocomposite coatings has been examined by polarized Fourier transform infrared spectroscopy using an attenuated total reflection unit. The morphology of the coatings has been analyzed by transmission (TEM), atomic-force (AFM), and scanning electron (SEM) microscopy. It is found that introduction of a metal (Ag or Cu) yields oriented layers at a lesser efficient thickness of a coating. The surface plasmon resonance of such structures was studied by measuring optical absorption of the coatings in the ultraviolet and visible ranges. The results show that the composite coatings containing Ag clusters are diameter less than 30 nm and absorb within the short-wave range from 400 to 550 nm.     

Characterization and properties Ti-Al-Si-N nanocomposite coatings prepared by middle frequency magnetron sputtering

TiN-containing amorphous Ti-Al-Si-N (nc-TiN/a-Si₃N₄ or a-AlN) nanocomposite coatings were deposited by using a modified closed field twin unbalanced magnetron sputtering system which is arc assisted and consists of two circles of targets, at a substrate temperature of 300 °C. XRD, XPS and High-resolution TEM experiments showed that the coatings contain TiN nanocrystals embedded in the amorphous Si₃N₄ or AlN matrix. The coatings exhibit good mechanical properties that are greatly influenced by the Si contents. The hardness of the Ti-Al-Si-N coatings deposited at Si targets currents of 5, 8, 10, and 12 A were 45, 47, 54 and 46 GPa, respectively. The high hardness of the deposited Ti-Al-Si-N coatings may be own to the plastic distortion and dislocation blocking by the nanocrystalline structure. On the other hand, the friction coefficient decreases monotonously with increasing Si contents. This result would be caused by tribo-chemical reactions, which often take place in many ceramics, e.g. Si₃N₄ reacts with H₂O to produce SiO₂ or Si(OH)₂ tribolay-layer.     

Nanostructured two-phase nc-TiN/a-(TiB2, BN) nanocomposite thin films

Thin films of Ti-B-N with different N contents were deposited on Si(1 0 0) at room temperature by reactive unbalanced close-field dc-magnetron sputtering using three Ti targets and one TiB₂ target in an Ar-N₂ gas mixture. The effect of N content on bonding structure, microstructure, phase configuration, surface roughness and mechanical properties have been investigated using X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), cross-sectional scanning electron microscopy (SEM), plan-view and cross-sectional high-resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and microindentation measurements. It was found that the N content significantly affected phase segregation and microstructure. The nitrogen-free TiB_0.65 films showed an amorphous compound consisting of Ti and TiB₂ (Ti-TiB₂). After adding about 28 at.% N, Ti was preferentially bonded to N to form TiN, accompanying with formation of small amounts of TiB and BN bonds. At this stage they combined TiB₂ to form a two-phase nanocomposite with microstructures comprising of nanocrystalline (nc-) TiN phase in nitrogen-containing amorphous (a-) TiB₂ matrix. Addition of more N promoted formation of BN bonding at cost of TiB₂, which resulted in formation of nanocomposite nc-TiN/a-(TiB₂, BN) thin films. A small grain less than 8 nm in size was found at low N content, and the grain size increased with increasing N content. A low microhardness value of about 20 GPa was obtained in the amorphous Ti-TiB₂ compound, and a maximum microhardness value of about 50 GPa was achieved in nc-TiN/a-TiB₂. A decrease of microhardness took place after formation of BN (i.e. amorphous matrix composed by both TiB₂ and BN) with further increasing N content, and a hardness value of about 35 GPa was followed at high N contents. The surface roughness strongly depended on the phase configuration. The higher the mole fraction of nanocrystalline TiN phase, the rougher the surface became.     

Microstructure and properties of TiC-Fe36Ni cermet coatings by reactive plasma spraying using sucrose as carbonaceous precursor

This study is aimed to introduce an innovative precursor pyrolysis process to prepare Ti-Fe-Ni-C compound powder and to discuss and evaluate the relationship between microstructure and properties of TiC-Fe36Ni cermet coatings in-situ synthesized by reactive plasma spraying (RPS) of these compound powders. The main characteristic of the pyrolysis process is that sucrose (C12H22O11) is used as a source of carbon as well as a binder to bind reactive constituent particles. The compound powder with high bonding strength can avoid the problem that reactive constituent particles are separated during spraying. The TiC-Fe36Ni cermet coatings present typical splat-like morphology of thermally sprayed coatings and consist of two different areas: one is a composite reinforcement area where spherical fine TiC particles (100-500 nm) homogeneously distribute within the Fe36Ni matrix; the other is an area of TiC accumulation. The surface hardness of the coatings reaches about 90 ± 2 (HR15N). The maximum and average microhardness values of the coatings are 1930 HV_0.2 (Vicker Hardness) and 1640 HV_0.2, respectively. The average bonding strength of the coatings is about 62.3 MPa. The wear resistance property of the coatings is much more than that of Ni60 alloys coatings.     

Microstructure, mechanical properties, and oxidation resistance of nanocomposite Ti-Si-N coatings

Ti-Si-N coatings with different silicon contents (0-12 at.%) were deposited onto Si(1 0 0) wafer, AISI M42 high speed steel, and stainless steel plate, respectively. These coatings were characterized and analyzed by using a variety of analytical techniques, such as XRD, AES, SEM, XPS, nanoindentation measurements, Rockwell C-type indentation tester, and scratch tester. The results revealed that the hardness was strongly correlated to the amount of silicon addition into a growing TiN film. The maximum hardness of 47.1 GPa was achieved as the Si content was 8.6 at.%. In the mechanical and oxidation resistance measurements, the Ti-Si-N coatings showed three distinct behaviors. (i) The coatings with Si contents of no more than 8.6 at.% performed good adhesion strength quality onto the HSS substrates. (ii) The fracture toughness of the coatings decreased with the increase in Si content. (iii) The Ti-Si-N coating with 8.6 at.% Si showed the excellent oxidation resistance behavior. The cutting performance under using coolant conditions was also evaluated by a conventional drilling machine. The drills with Ti-Si-N coatings performed much better than the drills with TiN coating and the uncoated drills.     

Effect of nitrogen flow ratios on the structure and mechanical properties of (TiVCrZrY)N coatings prepared by reactive magnetron sputtering

This study reports the influence of growth conditions on the characteristics of (TiVCrZrY)N coatings prepared by reactive magnetron sputtering at various N₂-to-total (N₂ + Ar) flow ratio, which is R_N. The crystal structures, microstructure, and mechanical properties for different R_N were characterized by electron spectroscopy for chemical analysis, X-ray diffraction, atomic force microscopy, field-emission-scanning electron microscopy, transmission electron microscopy, and nanoindentation. The results indicate that the TiVCrZrY alloy and nitride coatings have hexagonal close-packed (hcp)-type and sodium chloride (NaCl)-type solid-solution structures, respectively. The voids in the coatings are eliminated and the growth of the columnar crystal structures is inhibited along with an increasing R_N. As a consequence, highly packed equiaxed amorphous structures with smooth surfaces are formed. The coatings accordingly achieved a pronounce hardness of 17.5 GPa when R_N = 100%.     

Study of the microstructure and mechanical properties of white clam shell

The microstructure and mechanical properties of white clam shell were investigated, respectively. It can be divided into horny layer, prismatic layer and nacreous layer. Crossed-lamellar structure was the microstructural characteristic. The extension direction of lamellae in prismatic layer was different from that in nacreous layer, which formed an angle on the interface between prismatic layer and nacreous layer. The phase component of three layers was CaCO₃ with crystallization morphology of aragonite, which confirmed the crossed-lamellar structural characteristic. White calm shell exhibited perfect mechanical properties. The microhardness values of three layers were 273 HV, 240 HV and 300 HV, respectively. The average values of flexure and compression strength were 110.2 MPa and 80.1 MPa, respectively. The macroscopical cracks crossed the lamellae and finally terminated within the length range of about 80 μm. It was the microstructure characteristics, the angle on the interface between prismatic and nacreous layer and the hardness diversity among the different layers that enhanced mechanical properties of white calm shell.     

Annealing effect on microstructure and mechanical properties of amorphous Al-C-N films

Al-C-N thin films with different Al contents were deposited on Si (1 0 0) substrates by closed-field unbalanced reactive magnetron sputtering in the mixture of argon and nitrogen gases. These films were subsequently vacuum-annealed at 700 °C and 1000 °C, respectively. The microstructures of as-deposited and annealed films were characterized by X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM); while the hardness and elastic modulus values were measured by nano-indention method. The results indicated that the microstructure of both as-deposited and annealed Al-C-N films strongly depended on Al content. For thin films at low Al content, film delamination rather than crystallization occurred after the sample was annealed at 1000 °C. For thin films at high Al content, annealing led to the formation of AlN nanocrystallites, which produced nanocomposites of AlN embedded into amorphous matrices. Both the density and size of AlN nanocrystallites were found to decrease with increasing depth from the film surface. With increasing of annealing temperature, both hardness and elastic modulus values were decreased; this trend was decreased at high Al content. Annealing did not change elastic recovery property of Al-C-N thin films.     

Microstructure and mechanical properties of Al2O3-Al composite coatings deposited by plasma spraying

Al₂O₃ and Al₂O₃-Al composite coatings were prepared by plasma spraying. Phase composition of powders and as-sprayed coatings was determined by X-ray diffraction (XRD), while optical microscopy (OM) and scanning electron microscopy (SEM) were employed to investigate the morphology of impacted droplets, polished and fractured surface, and the element distribution in terms of wavelength-dispersive spectrometer (WDS). Mechanical properties including microhardness, adhesion and bending strength, fracture toughness and sliding wear rate were evaluated. The results indicated that the addition of Al into Al₂O₃ was beneficial to decrease the splashing of impinging droplets and to increase the deposition efficiency. The Al₂O₃-Al composite coating exhibited homogeneously dispersed pores and the co-sprayed Al particles were considered to be distributed in the splat boundary. Compared with Al₂O₃ coating, the composite coating showed slightly lower hardness, whereas the coexistence of metal Al phase and Al₂O₃ ceramic phase effectively improved the toughness, strength and wear resistance of coatings.     

Evaluation of Nanostructured coating layers formed on Ni balls during mechanical alloying of Cu powder

A novel coating method utilizing mechanical alloying was used to deposit a nickel-copper solid solution on the surface of nickel balls in a planetary ball mill. Mechanically milled copper powders were deposited by cold welding on the activated surface of the nickel balls. The impact of the nickel balls causes surface wear, leading to formation of mixed layered particles of copper-nickel and rewelding. In addition, diffusion takes place through the coating layer to form a Ni-Cu solid solution. The hardness of the coating reached a threefold increase (HV_0.01594) in comparison with the substrate hardness. Microstructural characterization of the coating surface performed using an optical microscope, SEM, and EPMA indicates that, with appropriate processing conditions, a thick, fully dense coating can be metallurgically bonded to the nickel balls. XRD results revealed the presence of a solid solution and nanocrystalline structure.     

Influence of substrate bias voltage on structure and properties of the CrAlN films deposited by unbalanced magnetron sputtering

The CrAlN films were deposited on silicon and stainless steel substrates by unbalanced magnetron sputtering system. The influence of substrate bias on deposition rate, composition, structure, morphology and properties of the CrAlN films was investigated. The results showed that, with the increase of the substrate bias voltage, the deposition rate decreased accompanied by a change of the preferred orientation of the CrAlN film from (2 2 0) to (2 0 0). The grain size and the average surface roughness of the CrAlN films declined as the bias voltage increases above −100 V. The morphology of the films changed from obviously columnar to dense glass-like structure with the increase of the bias voltage from −50 to −250 V. Meanwhile, the films deposited at moderate bias voltage had better mechanical and tribological properties, while the films deposited at higher bias voltage showed better corrosion resistance. It was found that the corrosion resistance improvement was not only attributed to the low pinhole density of the film, but also to chemical composition of films.     

Porosity and effective mechanical properties of plasma-sprayed Ni-based alloy coatings

The aim of this paper was to address the relationship between the porosity and micro-mechanical properties of the Ni-based alloy coatings which were prepared by a novel plasma-spraying system. The porosity and the mechanical properties of the coatings varied through changing the spraying parameters. Experimental results showed that the measured data of porosity, Young’s modulus and micro-hardness of the coating exhibited high scattering and followed the Weibull distribution. From statistic trend, the micro-hardness and Young’s modulus of the coating decreased with increasing the porosity of the coating. Moreover, generally, with increasing the micro-hardness of the coating, Young’s modulus of the coating increased.