Nanoindentation analysis of TiN,TiAlN,and TiAlSiN coatings prepared by cathode ion plating

The TiN,TiAlN and TiAlSiN coatings were deposited on H13 hot-worked mold steel by cathodic arc ion plating(CAIP).The morphologies,phase compositions,and nanoindentation parameters,such as creep hardness,elastic modulus and plastic deformation energy of the coatings were analyzed with field emission scanning electron microscopy(FESEM),X-ray diffraction(XRD) and nanoindentation testing,respectively,and the test results were compared with equation describing the indentation model.The results show that the TiN,TiAlN and TiAlSiN coating surfaces were dense and composed of TiN,TiN + TiAlN,TiN + Si3N4 + TiAlN phases,respectively.There was no spalling or cracking on the indentation surface.The creep hardness of the TiN,TiAlN and TiAlSiN coatings was 7.33,13.5,and 15.2 GPa,respectively;the corresponding hardness measured by nanoindentation was 7.09,15.6,and 21.7 GPa,respectively;and the corresponding elastic modulus was 201.93,172.79,and 162.77 GPa,respectively.The contact depth and elastic modulus calculated by the indentation model were close to those of the test results,but the remaining indentation parameters showed discrepancies.The sequence of plastic deformation energy was TiN TiAlNTiAlSiN.     

Structure and properties of Ti-Si-N coatings synthesized by combining cathode arc and middle-frequency magnetron sputtering

Ti-Si-N composite coatings were synthesized on a novel combining cathode and middle-frequency magnetron sputtering system, designed on an industrial scale. Ti was produced from the arc target and Si from magnetron target during deposition. The influences of negative bias voltage and Si content on the hardness and microstructure of the coatings were investigated. The composite coatings prepared under optimized conditions were characterized to be nc-TiN/a-Si₃N₄ structure with grain sizes of TiN ranging from 8–15 nm and exhibited a high hardness of 40 GPa. The enhancement of the hardness is suggested to be caused by the nanograin-amorphous structure effects.     

AFM Analysis of TiN,TiAlN, and TiAlSiN Coatings Prepared by Cathodic Arc Ion Plating

The TiN, TiAlN, and TiAlSiN coatings were prepared on YT14 cutting tool surface with CAIP(cathode arc ion plating), the surface morphologies and phases were analyzed with FESEM(field emission scanning electron microscopy), and XRD(X-ray diffraction), respectively, and the coating parameters such as 3D surface micro-topography, grain size, surface height, hierarchy, profile height, and power spectral density, etc, were measured with AFM(atomic force microscope). The results show that the phases of TiN, TiAlN, and TiAlSiN coatings are TiN, TiN+TiAlN, TiN+Si_3N_4+TiAlN, respectively, while the surface roughness Sa of TiN, TiAlN, and TiAlSiN coatings is 75.3, 98.9, and 42.1 nm, respectively, and the roughness depth Sk is 209, 389, and 54 nm, respectively, the sequence of average grain sizes is TiAlNTiNTiAlSiN. The surface bearing index Sbi of TiN, TiAlN, and TiAlSiN coatings is 0.884, 1.01, and 0.37, respectively, and the sequence of surface bearing capability is TiAlNTiNTiAlSiN. At the lower wavelength(102-103 nm), the power spectral densities have a certain correlation, and the sequence of TiNTiAlNTiAlSiN, while the correlation is low at the higher wavelength(103 nm).     

Structure and performance of TiC-containing diamond-like carbon nanocomposite coatings deposited by rectangular cathodic arc ion-plating

TiC-containing diamond-like carbon (TiC-DLC) nanocomposite coatings were deposited by a rectangular cathodic arc ion-plating system using C₂H₂ as reacting gas. Raman spectroscopy and transmission electron microscopy analysis show that with increasing flow rate of C₂H₂, the structure of nanocomposite coatings changes from TiC nanograin-containing to graphite nanograin-containing DLC. The hardness measurements show that the hardness decreases from 28 GPa to 18 GPa with increasing C₂H₂ flow rate. The scratch test show that a high critical load (>40 N) was obtained and exhibited a good adhesion between the coating and the substrate. Wear experiment shows that the friction coefficient of TiC-DLC nanocomposite coatings decreases with increasing C₂H₂. A low friction coefficient of 0.07 was obtained at 480 sccm C₂H₂.     

Fabrication of in situ Ti2AlN/TiAl composites by reaction hot pressing and their properties

Ti2AIN/TiAI composites with different volume fractions of reinforcement were successfully fabricated by hot-pressing sintering method （reaction hot pressing） using Ti, Al and TiN powders as starting materials. The synthesis process includes four stages： first, the reactions between Al and Ti powers and between Al and TiN powders respectively occur and result in TiAl3 phase; secondly, AI powders in the sample are exhausted; the remaining Ti cores react with TiAl3 layer to form Ti-Al intermetallics; moreover, a few Ti2AlN particles precipitate from the TiAl3 phase; thirdly, Ti-Al intermetallics react with the remaining Ti cores to form Ti3Al and TiAl phases. TiAl phase and original TiN powers are in direct contact each other; finally, the residual TiN powers react with TiAl phase and result in a plenty of TizAIN phase. Compared with TiAl matrix, the hardness, elastic modulus and high-temperature compressive strength of Ti2AlN/TiAl composite are improved obviously and they are all enhanced with increasing the volume fraction of Ti2AlN phase.     

用PCVD法制备抗高温氧化涂层的研究

研究了用ＰＣＶＤ法所制备的ＴｉＮ,ＴｉＡ１Ｎ及ＴｉＳｉＮ硬质涂层的抗高温氧化性及ＴｉＮ涂层在双氧水介质中的抗氧化性。结果表明,ＴｉＡ１Ｎ,ＴｉＳｉＮ涂层在空气中的抗高温氧化性可达７００℃以上, ＴｉＮ涂层可达６００℃。在双氧水介质中, ＰＣＶＤ－ＴｉＮ涂层仍具有较强的抗氧化能力, 且优于ＰＶＤ－ＴｉＮ 涂层     

脉冲N离子束轰击对TiAlN膜层显微硬度影响的研究

采用俄罗斯UVN 0.5D2I脉冲离子束辅助电弧离子镀沉积设备,在高速钢W18Cr4V基材上沉积TiAlN膜层。研究了膜层沉积之前N离子束轰击基材以及膜层沉积过程中N离子束辅助轰击对TiAlN膜层显微硬度的影响。结果表明:膜层沉积之前,N离子轰击得到高度洁净的表面,使基材的显微硬度由原来的900HV0.01提高到1230HV0.01。膜层沉积过程中,脉冲N离子束轰击,消除了膜层中的硬度"软点"及阴影效应,增加(Ti,Al)N相的含量,膜层的内部产生了压应力,这些因素显著提高了膜层的硬度,膜层的最高硬度为2530HV0.01。但轰击能量不能过高,否则会降低膜层的显微硬度。     

Moisture-proof and enhanced effect of inorganic coating on porous Si<Subscript>3</Subscript>N<Subscript>4</Subscript> ceramic

Inorganic coating was fabricated on the surface of the porous Si₃N₄ ceramic by polymer derived (PD) and spraying technology, via using vinyl-polysilazane (PSN-1) as a preceramic polymer and Si₃N₄ and lithium aluminosilicate (LAS) powders as fillers. The phase and microstructure of the coatings were analyzed by X-ray diffraction (XRD) analysis and scanning electron microscopy (SEM), respectively. The effect of the coatings on mechanical property and humidity resistance of the porous Si₃N₄ ceramic was investigated. The experimental results showed that we successfully fabricated the uniform and dense coating which preferably combined with the substrate upon the addition of fillers. The bending strength of the porous Si₃N₄ ceramic sprayed the coating increased by more than 18%, and the surface hardness increased by 1.7 times. The apparent porosity of the materials reduced by an average of 97.7%, and water absorption was below 0.5%. Therefore, the prepared coating with preferable density had an obviously moisture-proof and enhanced effect on the porous Si₃N₄ ceramic.     

用PCVD法制备(TiAl)N膜的研究

本文介绍了在PCVD设备中用固态AlCl_3制备(TiAl)N膜。结果表明,(TiAl)N膜的含Al量与AlCl_3的蒸发温度成正比,但膜内Cl含量却无明显变化。(TiAl)N膜保持了TiN膜的面心立方晶体结构,但其晶格常数变小,织构变弱,组织略有细化。(TiAl)N膜的显微硬度略高于或等于TiN膜的硬度,但抗高温氧化性有较大幅度提高。     

Microstructure and mechanical properties of TiAlSiN nano-composite coatings deposited by ion beam assisted deposition

TiAlSiN nano-composite coatings with Silicon contents from 4.1 to 23.9 at.% were deposited on Silicon wafers. The nanohardness, microstructure, and adhesion force of the coatings were deeply affected by Silicon contents. The TiAlSiN with 9.0 at.% Silicon has a maximum hardness of 40.9 GPa, a highest adhesion force of 67 N and a lowest friction coefficient of 0.5. Microstructures show that Silicon doping increases the hardness of coating due to solid solution hardening effect and grain boundary enhancement effect. The amorphous Si3N4 matrix, which contains(Ti,Al)N nano-crystals, is formed as the Silicon content is increased. The matrix contributes to the nano-hardness and helps to resist surface oxidization. Especially, the matrix induces low surface roughness and decreases the friction coefficient.     

Effects of N<Subscript>2</Subscript> pressure on the structural and electrical properties of tin films deposited by laser molecular beam epitaxy

Titanium nitride (TiN) films were deposited on Si(100) substrates by laser molecular beam epitaxy(LMBE), and their properties of structure and resistivity with varying N₂ pressure were investigated. The results showed that atomically flat TiN films with layer-by-layer growth mode were successfully grown on Si(100) substrates, and (200) was the preferred orientation. With the increasing of N₂ pressure, the N/Ti ratio gradually increased and the diffraction peak progressively shifted towards lower diffraction angle. At pressure of 0.1 Pa, stoichiometric TiN film was formed which exhibited the characteristic diffraction angle of (200) plane. All films showed high reflectance to infrared spectrum and the films with overstoichiometry and understoichiometry had a higher resistivity owing to the surface particles and lattice distortion, while the stoichiometric TiN film depicted the minimum resistivity, around 19 μΩ·cm.     

Influence of potential on structure and properties of microarc oxidation coating on Mg alloy

In order to obtain optimizing microarc oxidation coating on Mg alloy from a friendly-enviormental electrolyte free of Cr⁶⁺ and PO ₄ ³⁻ , constant potential regime was applied to produce it. The influence of potential on the morphology, composition, structure and other properties, such as microhardness and corrosion resistance were investigated by scanning electron microscopy (SEM), energy dispersive spectroscope (EDS), X-ray diffraction (XRD), hardness tester and electrochemical method. The results clearly show that oxidation potential plays an important role in the formation of coating’s structure and properties. The microarc oxidation coating is smooth and white, which consists of two layers. The external layer is loose and porous and enriched in Al and Si. Moreover, its content of Al and Si increases with the increasing operated potential. While the inner layer is compact and the content of Al and Si are lower than that of the external layer. The coating is composed of several phases and the major phases are MgAl₂O₄ and MgO, and the minor phases are Al₂O₃ and SiO₂ when the potential is higher. The microhardness of coating is obtained the maximum at the potential of 45 V, so does the corrosion resistance.     

Erosion-Corrosion Behaviors of High Velocity Arc Sprayed Fe-Al/Cr3 C2 Coating

1 IntroductionArc Spraying (AS) is a technique that utilizes anelectric arc as the heat source to melt wires into droplets ,which are subsequentlysprayed ontosubstrates bytheflowof compressed air . High Velocity Arc Spraying (HVAS)technology was developed on the basis of AS. Aspecialtube designed according to the principle of aerodynamicswas mounted at the exit of compressed air .Thenthe hightemperature fuel air or compressed air was accelerated bythe tube .Hence ,a higher velocityand be…     

Influence of Si Content on Properties of Ti_(1-x)Si_xN Coatings

To investigate the evolution of microstructure and wear behavior of TiSiN coatings with the variation of Si in targets and lays the foundation for its controllable mass production, Ti_(1-x)Si_xN composite coatings were deposited onto Si(100) and cemented carbide substrates using TiSi targets with different Si content by cathodic arc ion plating. The influences of Si on the microstructure and mechanical properties were studied. Nano-amorphous composite structure appeared in the Ti_(1-x)Si_xN coatings when Si content in TiSi target was higher than 5 at%. However, further increase of Si content in TiSi target exhibited a negligible effect on the microstructure of Ti_(1-x)Si_xN coatings. Hardness and deformation resistance were correlated to the content of Si in TiSi targets. Maximum hardness was obtained as the Si content in target increased up to 20 at%. Friction coefficient and wear rate significantly decreased with addition of Si in TiN coating, and then dually increased with the increase of Si content in targets.     

Effects of Al addition on the microstructure and properties of Nb/Nb5Si3 in situ composites fabricated via spark plasma sintering

Dense Nb/Nb5Si3 composites were fabricated via spark plasma sintering technology using Nb, Si, and Al elemental powders as raw materials. The microstructttres of the synthesised composites were analyzed through scanning electron microscopy, X-ray diffraction, and electron probe microanalysis. The results show that the composites consisted of residual Nb particle phase and Nb5Si3 phase. The microstructure of the Nb/ Nb5Si3 in situ composites was evidently affected by Al addition, which prompted the formation of the Al3Nb10Si3 phase. In addition, the Rockwell hardness of the composites decreased with the increase in AI additions. The Rockwell hardness of Nb-20Si is 60HRC, which decreased to approximately 52.7 HRC when the Al content increased to 15 at%. The oxidation resistance of the Nb/NbsSi3 in situ composites significantly improved with the increase in Al addition.     

Preparation and sintering of nano Fe coated Si3N4 composite powders

Fe/Si₃N₄ composite powder was synthesized by the heterogeneous precipitation-thermal reduction process, and then pressed into flakes under a pressure of 10 MPa. Flakes were sintered by pressureless and hot-pressing at 1 600 °C under 0.1 MPa N₂. The chemical composition, phases and microstructure of composite powder and sintered flakes were investigated by energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results show that the structure of composite powders is Si₃N₄ coated by nano Fe. The crystal phases of sintered flakes by pressureless are Fe(Si) compound, SiC and Si₃N₄. The crystal phases of the sintered samples by hot-pressing are Fe, Fe(Si) compound and Si₃N₄. It is found that crystal phases flakes obtained by pressureless and hot-pressing are very different. Foundation item: Project(50804016) supported by the National Natural Science Foundation of China     

First-Principles Study of the High-Temperature Behaviors of the Willemite-Ⅱ and Post-Phenacite Phases of Silicon Nitride

The structural and elastic properties of the recently-discovered wⅡ- and δ-Si_3N_4 are investigated through the plane-wave pseudo-potential method within ultrasoft pseudopotentials.The elastic constants show that wⅡ- and δ-Si_3N_4 are mechanically stable in the pressure ranges of 0-50 GPa and 40-50 GPa,respectively.The α→wⅡ phase transition can be observed at 18.6 GPa and 300 K.The β→δ phase transformation occurs at pressures of 29.6,32.1,35.9,39.6,41.8,and 44.1 GPa when the temperatures are100,200,300,400,500,and 600 K,respectively.The results show that the interactions among the N-2s,Si-3s,3p bands(lower valence band) and the Si-3p,N-2p bands(upper valence band) play an important role in the stabilities of the wⅡ and S phases.Moreover,several thermodynamic parameters(thermal expansion,free energy,bulk modulus and heat capacity) of δ-Si_3N_4 are also obtained.Some interesting features are found in these properties.δ-Si_3N_4 is predicted to be a negative thermal expansion material.The adiabatic bulk modulus decreases with applied pressure,but a majority of materials show the opposite trend.Further experimental investigations with higher precisions may be required to determine the fundamental properties of wⅡ- andδ-Si_3N_4.     

不同Al含量的Ti/Al合金靶对磁控溅射离子镀TiAlN薄膜力学性能的影响

采用不同Al含量的Ti/Al合金靶材在硬质合金刀具上沉积TiAlN薄膜,研究靶材中不同的Al含量对TiAlN薄膜表面粗糙度、硬度以及膜基结合力等性能的影响,通过显微硬度仪、划痕仪、金相显微镜和XRD等仪器分别对薄膜的硬度、结合力、组织结构等主要性能进行测试分析。实验结果表明:随着Ti/Al合金靶中Al含量的增加,TiAlN薄膜的硬度先增加后减小,膜基结合力逐渐增加;当Al在Ti/Al合金靶材中所占的比值为2:3时,TiAlN薄膜的硬度、耐磨性等综合力学性能最佳。     

Synthesis of nanoscale multilayered ZrN/W coatings by ion beam assisted deposition

ZrN/W multilayered coatings with different modulation periods at the nanoscale have been synthesized at different N+ beam bombarding energies using IBAD. Various characterization techniques such as XRD, AES, nano indenter and profiler were employed to investigate the influence of modulation period and bombarding energy on microstructure and mechanical properties of the coatings. The results showed that all superlattice coatings had better mechanical properties than the monolithic ZrN and W coatings. At an optimal condition with 300 eV N+ beam bombarding energy and 8―9 nm modulation period, XRD pattern possessed a sig- nificantly structural mixture of strong ZrN (111), W (110), as well as weak ZrN (220) textures in the multilayered coating. The optimal condition resulted in higher hardness (26 GPa), elastic modulus (310 GPa) and fracture resistance of the coat- ing than other conditions.     

Synthesis of ZrAlN coatings with thermal stability at high temperature

Dry machining will result in elevated temperatures at the tool surface (800—1000℃). So, coating materials that can provide protection for cutting tools at these temperatures are of great technological interests. ZrAlN coating is proposed to possess high-temperature stable structural and mechanical properties due to the addition of the alloying element. ZrAlN coatings were grown using a dc reactive magnetron sputtering. The XRD and nano indenter were employed to investigate the effects of reaction gas partial pressure and substrate bias on structural and mechanical properties, as well as high-temperature stability. The ZrAlN coating, when deposited under optimum conditions (-37 V substrate bias and 2×10-5 Pa N2 partial pressure), showed smooth surface with thermal stable hardness. Its internal stress was relaxed from 2.2 to 0.7 GPa after anneal- ing. Formation of Al2O3 and ZrO2 crystalline phases should be related to thermal stability of the coatings.