Low-temperature hot-press sintering of AlN ceramics with MgO–CaO–Al2O3–SiO2 glass additives for ceramic heater applications

Aluminum nitride (AlN) is used a ceramic heater material for the semiconductor industry. Because extremely high temperatures are required to achieve dense AlN components, sintering aids such as Y₂O₃ are typically added to reduce the sintering temperature and time. To further reduce the sintering temperature, in this study, a low-melting-temperature glass (MgO–CaO–Al₂O₃–SiO₂; MCAS) was used as a sintering additive for AlN. With MCAS addition, fully dense AlN was obtained by hot-press sintering at 1500 °C for 3 h at 30 MPa. The mechanical properties, thermal conductivity, and volume resistance of the sintered AlN–MCAS sample were evaluated and compared with those of a reference sample (AlN prepared with 5 wt% Y2O3 sintering aid sintered at 1750 °C for 8 h at 10 MPa). The thermal conductivity of AlN prepared with 0.5 wt% MCAS was 91.2 W/m?K, which was 84.8 W/m?K lower than that of the reference sample at 25 °C; however, the difference in thermal conductivity between the samples was only 14.2 W/m?K at the ceramic-heater operating temperature of 500 °C. The flexural strength of AlN–MCAS was 550 MPa, which was higher than that of the reference sample (425 MPa); this was attributed to the smaller grain size achieved by low-temperature sintering. The volume resistance of AlN–MCAS was lower than that of the reference sample in the range of 200–400 °C. However, the resistivity of the proposed AlN–MCAS sample was higher than that of the reference sample (500 °C) owing to grain-boundary scattering of phonons. In summary, the proposed sintering strategy produces AlN materials for heater applications with low production cost, while achieving the properties required by the semiconductor industry.     

Enhanced thermal stability of a sputtered titanium-nitride film as a diffusion barrier for capacitor-bottom electrodes

The effect of a thin RuO_x layer formed on the Ru/TiN/doped poly-Si/Si stack structure was compared with that on the RuO_x/TiN/doped poly-Si/Si stack structure over the post-deposition annealing temperature ranges of 450–600°C. The Ru/TiN/poly-Si/Si contact system exhibited linear behavior at forward bias with a small increase in the total resistance up to 600°C. The RuO_x/TiN/poly-Si/Si contact system exhibited nonlinear characteristics under forward bias at 450°C, which is attributed to no formation of a thin RuO_x layer at the RuO_x surface and porous-amorphous microstructure. In the former case, the addition of oxygen at the surface layer of the Ru film by pre-annealing leads to the formation of a thin RuO_x layer and chemically strong Ru-O bonds. This results from the retardation of oxygen diffusion caused by the discontinuity of diffusion paths. In particular, the RuO_x layer in a nonstoichiometric state is changed to the RuO₂-crystalline phase in a stoichiometric state after post-deposition annealing; this phase can act as an oxygen-capture layer. Therefore, it appears that the electrical properties of the Ru/TiN/poly-Si/Si contact system are better than those of the RuO_x/TiN/poly-Si/Si contact system.     

PVD涂层工艺在M3滚刀上的应用

对M3滚刀进行了物理气相沉积 (PVD)工艺试验。经高温耐磨试验和切削试验证明 ,M3滚刀经TiN涂层后 ,其耐磨性和使用寿命显著提高。     

Effect of Rare Earth Element Cerium on Mechanical Properties and Morphology of TiN Coating Prepared by Arc Ion Plating

TiN coatings were deposited on polished substrates of W18Cr4V high speed steel by means of vacuum arc ion plating. The effect of cerium on adhesion between TiN coating and substrate was studied. The microstructures and composition of TiN coatings were also investigated by means of scanning electron microscope (SEM), Auger electron spectroscopy (AES), and X-ray diffraction (XRD) technique. It was found that cerium is an effective modifying agent and the addition of suitable amount of cerium to TiN coatings can produce relatively excellent properties such as micro-hardness, wear resistance, oxidation resistance and porosity. The experimental results show that the added cerium in TiN coatings makesa contribution to form the preferred direction along with a (111 ) or (222) close packed face, which may be one of the reasons that improves some properties mentioned above.     

Combination of coating and heat treatment processes

For a proper use of coated tools and components excellent coating properties as well as excellent substrate properties of the coating/substrate composite are necessary. A well known example is the load support of hard steel substrates for thin wear resistant coatings. Therefore coating processes must be combined with heat treatment processes of the substrates, whereby several practical processing constraints like order and compatibility of the applied treatment procedures must be considered. The combination of CVD-coating plus laser beam hardening is an example of a post coating heat treatment. Applications may be possible for large forming tools made of high alloyed tool steels, which nowadays are usually through hardened after CVD-coating. Laser beam hardening offers the possibility, to harden only the highly loaded edges of the tools. The advantages of this combination are short process time, less distortion and compressive residual stresses in the substrate surface. CVD-coatings can endure laser beam hardening with suitable parameters. The influence of CVD TiN-coated steel substrates and laser beam hardening parameters on microstructures and properties of coating/substrate compounds have been investigated. Special attention was paid to overlapping hardening zones, which may occur at the start and end points of a laser hardened track. In summary, the combination of coating and heat treatment processes show a high potential to produce coating/substrate compounds with excellent coating properties as well as excellent substrate properties.     

Influence of growth rate on the structural and morphological properties of TiN, ZrN and TiN/ZrN multilayers

The effect of the deposition rate on the structural and morphological properties of TiN and ZrN single layers and TiN/ZrN multilayers deposited by radiofrequency reactive magnetron sputtering has been studied. The total pressure was kept constant and the growth rate variation was obtained by small difference of nitrogen concentration in the fed gas. The decreasing deposition rate results in a structural change in the thin films from (111) orientation to (100) one. As consequence the surface morphology becomes smoother. Films roughness is strongly related with texture and it decreases with an increase in the (100) X-ray diffraction line intensity. In order to achieve a clear interpretation of our experimental results, the ratio between the N⁺ ions of the plasma and the atoms number reaching the substrate was considered. At high deposition rate with respect to the N⁺ concentration, the chemical potential of transition metal on (100) growth surface is higher than (111) one favouring the (111) orientation of the films. On the contrary, when the growth rate is low with respect to the nitrogen concentration, the chemical potential of transition metal on (111) growth surface is higher than the (100) one leading to a preferential growth in the (100) direction.     

脉冲激光LGA法钛表面氮化及其XRD和SEM微观分析

用调Ｑ－ＹＡＧ和ＸｅＣｌ脉冲激光在钛表面以激光气体合金化方法生成氮化钛层，用Ｘ射线衍射仪分析了不同激光能量、不同Ｎ２气压不同作用脉冲数等条件下ＴｉＮ的结晶取向、结晶形态、氮化程度，用扫描电镜观察了它们的微观结构，对脉冲激光的ＬＧＡ法机理进行了探讨，也发现了用ＬＧＡ法对Ｍｏ的氮化生成Ｍｏ２Ｎ．     

Ti/Al Interaction and Austenite Grain Control in Crankshaft Manufacturing with 38MnSiVS5 Steel

38MnSiVS5 steel is similar to 38MnVS6 steel (EN), the difference being the addition of a small Ti content. Typical Ti and Al contents in the chemical composition of 38MnSiVS5 steel are Ti=0.020 and Al=0.035 mass%. Both elements combine easily with nitrogen, especially Ti, and it has been observed that relatively high Al levels are harmful for austenite grain size control at reheating temperatures. In this work 38MnSiVS5 steel is used to manufacture a large number of castings, varying only the Ti and Al contents and obtaining ingots with a different Ti/Al ratio in each case. The results show that abnormal growth of the austenitic grain occurs irrespective of the Ti and Al contents, due fundamentally to the partial dissolution and coarsening of TiN precipitates. However, the steels with high Al contents present worse behaviour due to the formation of a second type of precipitates, namely AIN, which quickly dissolve between 1000 and 1100°C, causing a drastic decline in local pinning forces that gives rise to more pronounced abnormal growth of the affected grains.     

等离子体浸没式离子注入-离子束增强沉积TiN膜研究

本文采用一种新型的等离子体浸没式离子注入 离子束增强沉积的技术(PIII IBAD),在Cr12MoV钢基体上制备出了TiN膜,对沉积膜的组织进行了光电子能谱分析,并对沉积膜进行了硬度检测、摩擦试验及磨痕形貌分析。试验结果表明,沉积膜中的组织为TiN、TiO2和Ti2O3,TiN膜具有高达Hv3200的高硬度和极其优良的摩擦性能。