Evaluation of fracture toughness of ZrO2 and Si3N4 engineering ceramics following CO2 and fibre laser surface treatment

The fracture toughness property (K_1C) of Si₃N₄ and ZrO₂ engineering ceramics was investigated by means of CO₂ and a fibre laser surface treatment. Near surface modifications in the hardness were investigated by employing the Vickers indentation method. Crack lengths and the crack geometry were then measured by using the optical microscopy. A co-ordinate measuring machine was used to investigate the diamond indentations and to measure the lengths of the cracks. Thereafter, computational and analytical methods were employed to determine the K_1C. An increase in the K_1C of both ceramics was found by the CO₂ and the fibre laser surface treatment in comparison to the as-received surfaces. The K_1C of the CO₂ laser radiated surface of the Si₃N₄ was over 3% higher in comparison to that of the fibre laser treated surface. This was by softening of the near surface layer of the Si₃N₄ which comprised of lowering of hardness, which in turn increased the crack resistance. The effects were not similar in ZrO₂ ceramic to that of the Si₃N₄ as the fibre laser radiation in this case had produced an increase of 34% compared to that of the CO₂ laser radiation. This occurred due to propagation of lower crack resulting from the Vickers indentation test during the fibre laser surface treatment which inherently affected the end K_1C through an induced compressive stress layer. The K_1C modification of the two ceramics treated by the CO₂ and the fibre laser was also believed to be influenced by the different laser wavelength and its absorption co-efficient, the beam delivery system as well as the differences in the brightness of the two lasers used.     

Si3N4的晶体化和ZrN/Si3N4纳米多层膜的超硬效应

研究了Si₃N₄层在ZrN/Si₃N₄纳米多层膜中的晶化现象及其对多层膜微结构与力学性能的影响. 一系列不同Si₃N₄层厚度的ZrN/Si₃N₄纳米多层膜通过反应磁控溅射法制备. 利用X射线衍射仪、高分辨透射电子显微镜和微力学探针表征了多层膜的微结构和力学性能. 结果表明，由于受到ZrN调制层晶体结构的模板作用，溅射条件下以非晶态存在的Si₃N₄层在其厚度小于0.9 nm时被强制晶化为NaCl结构的赝晶体，ZrN/Si₃N₄纳米多层膜形成共格外延生长的柱状晶，并相应地产生硬度升高的超硬效应. Si₃N₄随层厚的进一步增加又转变为非晶态，多层膜的共格生长结构因而受到破坏，其硬度也随之降低.     

Si3N4在h-AlN上的晶体化与AlN/Si3N4纳米多层膜的超硬效应

采用反应磁控溅射法制备了一系列具有不同Si₃N₄层厚度的AlN/Si₃N₄纳米多层膜,利用X射线衍射仪、高分辨透射电子显微镜和微力学探针表征了多层膜的微结构和力学性能.研究了Si₃N₄层在AlN/Si₃N₄纳米多层膜中的晶化现象及其对多层膜生长结构与力学性能的影响.结果表明,在六方纤锌矿结构的晶体AlN调制层的模板作用下,通常溅射条件下以非晶态存在的Si₃N₄层在其厚度小于约1nm时被强制晶化为结构与AlN相同的赝形晶体,AlN/Si₃N₄纳米多层膜形成共格外延生长的结构,相应地,多层膜产生硬度升高的超硬效应.Si₃N₄随层厚的进一步增加又转变为非晶态,多层膜的共格生长结构因而受到破坏,其硬度也随之降低.分析认为,AlN/Si₃N₄纳米多层膜超硬效应的产生与多层膜共格外延生长所形成的拉压交变应力场导致的两调制层模量差的增大有关. 关键词： 3N₄纳米多层膜')" href="#">AlN/Si₃N₄纳米多层膜 外延生长 赝晶体 超硬效应     

AlN/Si3N4纳米多层膜的外延生长与力学性能

采用射频磁控溅射方法制备单层AlN, Si₃N₄薄膜和不同调制周期的AlN/Si₃N₄纳米多层膜.采用X射线衍射仪、高分辨透射电子显微镜和纳米压痕仪对薄膜进行表征.结果发现,多层膜中Si₃N₄层的晶体结构和多层膜的硬度依赖于Si₃N₄层的厚度.当AlN层厚度为4.0nm、 Si₃N₄层厚度 关键词： 3N₄纳米多层膜')" href="#">AlN/Si₃N₄纳米多层膜 外延生长 应力场 超硬效应     

Investigation of cutting of engineering ceramics with Q-switched pulse CO2 laser

In this paper, the cutting of Si₃N₄ engineering ceramics with Q-switched pulse CO₂ laser is studied. Considering the influence of the cut front shape on the absorption of the laser beam, a simplified 2D mathematic model is developed based on a pulsed laser vaporization cut process. This model is based on the conservation of energy. The experimental results show that it would realize crack-free cutting by using high-speed and multi-pass feed cutting process.     

Preparation, characterization and luminescence properties of porous Si3N4 ceramics with Eu2O3 as sintering additive

Porous Si₃N₄ ceramics with photoluminescence properties were prepared by pressureless sintering using α-Si₃N₄ powder as raw material and Eu₂O₃ as sintering additive. Chemical composition, phase formation, microstructure and photoluminescence properties of porous Si₃N₄ ceramics were studied by X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), scanning electron microscopy (SEM) and photoluminescence measurements (PL/PLE). The results show that single Eu₂O₃ additive promotes α→β transformation but not significant densification. A broad band emission center at 570 nm assigned to Eu²⁺ is observed, Eu³⁺ in Eu₂O₃ is (partially) converted to Eu²⁺ by reaction with Si₃N₄, which results in a lower β aspect ratio and β-content compared to the other Ln (Ln=lanthanide) oxide additives.     

Magnetic characterization of Mn5SiB2 and Mn5Si3 phases

In this work the Mn₅Si₃ and Mn₅SiB₂ phases were produced via arc melting and heat treatment at 1000 °C for 50 h under argon. A detailed microstructure characterization indicated the formation of single-phase Mn₅Si₃ and near single-phase Mn₅SiB₂ microstructures. The magnetic behavior of the Mn₅Si₃ phase was investigated and the results are in agreement with previous data from the literature, which indicates the existence of two anti-ferromagnetic structures for temperatures below 98 K. The Mn₅SiB₂ phase shows a ferromagnetic behavior presenting a saturation magnetization M_s of about 5.35×10⁵ A/m (0.67 T) at room temperature and an estimated Curie temperature between 470 and 490 K. In addition, AC susceptibility data indicates no evidence of any other magnetic ordering in 4-300 K temperature range. The magnetization values are smaller than that calculated using the magnetic moment from previous literature NMR results. This result suggests a probable ferrimagnetic arrangement of the Mn moments.     

Crystallization of amorphous Si3N4 and superhardness effect in HfC/Si3N4 nanomultilayers

HfC/Si₃N₄ nanomultilayers with various thicknesses of Si₃N₄ layer have been prepared by reactive magnetron sputtering. Microstructure and mechanical properties of the multilayers have been investigated. The results show that amorphous Si₃N₄ is forced to crystallize and grow coherently with HfC when the Si₃N₄ layer thickness is less than 0.95 nm, correspondingly the multilayers exhibit strong columnar structure and achieve a significantly enhanced hardness with the maximum of 38.2 GPa. Further increasing Si₃N₄ layer thickness leads to the formation of amorphous Si₃N₄, which blocks the coherent growth of multilayer, and thus the hardness of multilayer decreases quickly.     

Thermal expansion and magnetostriction in Pr(n+2)(n+1)Nin(n−1)+2Sin(n+1) compounds

Thermal expansion and magnetostriction of members of a homologous series of compounds based on the alloy series Pr_(n+2)(n+1)Ni_n(n−1)+2Si_n(n+1) have been measured. The crystal structures of these compounds are closely interrelated because they form trigonal prismatic columns in which the number of trigonal prisms that form the base of the trigonal columns is determined by the value of n in the chemical formula. Two compositions were investigated, Pr₅Ni₂Si₃ and Pr₁₅Ni₇Si₁₀, corresponding to n=3$n=3$ and n=4,$n=4,$ respectively. The results were analyzed and used to determine the location of magnetic phase transitions by calculating the magnetic contribution to thermal expansion using the Gruneisen–Debye theory. This allowed more precise determination of the magnetic transition temperatures than could be achieved using the total thermal expansion. The results show two phase transitions in each material, one corresponding to the Curie temperature and the other at a lower temperature exhibiting characteristics of a spin reorientation transition.     

非晶Fe73.5Cu1Nb3Si13.5B9合金激光纳米化的超精细结构研究

在CO₂激光功率为50—300W、扫描速度为20mm/s、激光散光斑为20mm照射条件下 ，诱导非 晶Fe_735Cu₁Nb₃Si_135B9带中发生结构重组，产生定量纳米α-F e(Si)晶相形成双相组织结构材料. 利用穆斯堡尔谱研究了非晶Fe_735C u₁Nb₃Si_135B₉合金激光纳米化的 超精细结构. 实验结果表明，激光诱导非晶 Fe_735Cu₁Nb₃Si_135B ₉纳米化后，其超精细磁场的分布随 着激光功率变 化由单峰向双峰变化，在高功率辐照时， 出现了双峰分布，并且峰位向高场移动. 高激光 功率辐照非晶Fe_735Cu₁Nb₃Si_{135B9合金纳米晶化相有四种超精细结 构，即2个超精细磁场较小的初晶相和2个超精细磁场较大的纳米晶化相. 其中超精细磁场较 大(17—25MA/m)的α-Fe(Si)相为DO3结构. 关键词： 激光 纳米晶α-Fe（Si) 735}Cu₁Nb< sub>3Si_135B₉')" href="#">非晶Fe_735Cu₁Nb< sub>3Si_135B₉ 超精细结构 超精细磁场     

Laser surface remelting of plasma sprayed nanostructured Al2O3-13wt%TiO2 coatings on titanium alloy

Plasma sprayed nanostructured coatings were successfully fabricated on a titanium alloy (Ti-6Al-4V) substrate using the as-prepared nanostructured Al₂O₃-13wt%TiO₂ feedstock. A CO₂ laser was used to remelt the plasma sprayed coatings. The effects of laser remelting on the phase constituents, microstructure and properties of the ceramic coatings were investigated. The laser remelted coatings (LRmC) possessed a much denser and more homogenous structure and excellent metallurgical bonding to the substrate. The average porosity of the LRmC was reduced to 0.9%, compared with 6.2% of the as-sprayed coatings. The net-like structure in the as-prepared feedstock remained in the coatings before and after laser remelting. The metastable γ-Al₂O₃ phase in the as-sprayed coatings transformed to stable α-Al₂O₃ during laser remelting. The LRmC could remain nanostructure. The microhardness of the coatings was enhanced to 1000-1400 HV_0.3 after laser remelting, which was much higher than that of the plasma sprayed coatings and 2-3 times higher that of the substrate. Significant decreases in surface roughness were also found in the LRmC.     

Laser synthesis of thin layers of In4Se3, In4Te3 and modification of their structure and characteristics

Trends of structural modifications and phase composition occurring in In₄Se₃ thin films and In₄Se₃-In₄Te₃ epitaxial heterojunctions under laser irradiations have been investigated. Dynamics of the layer structure modification, depending on laser modes, i.e. pulse duration τ = 2-4 ms, irradiation intensity I₀ = 10-50 kW/cm², number of pulses N = 5-50, was studied by electron microscopy. An increase in laser influence promotes enlargement of the layer grains and transformation of their polycrystalline structure towards higher degree of stoichiometry. As a result of laser solid restructuring heterojunctions of In₄Se₃-In₄Te₃, being photosensitive within 1.0-2.0 μm and showing fast time of response, have been obtained. Laser modification of structure enables one to optimize electrical and optical properties of functional elements on the base of thin films and layers of In₄Se₃, In₄Te₃, widely used as infrared detectors and filters.     

激光辐照非晶Fe73.5Cu1Nb3Si13.5B 9微量晶化的穆斯堡尔谱研究

在激光功率为40—160W、扫描速度为10mm/s、激光光斑为20mm照射条件下,用CO ₂激 光辐照非晶Fe_73.5Cu₁Nb₃Si_13.5B_{9< /sub>产生微量晶化.利用透射穆斯堡尔谱 （TMS）技术分析了原始态和晶化后样品的超精细结构.确定了穆斯堡尔谱的基本参数——化 学位移(IS)、四极分裂(QS)、内磁场(Hhf)随激光功率变化的规律.分析表明，CO2关键词： 激光辐照 微量晶化 73.5Cu1Nb3 Si13.5B9')" href="#">非晶Fe73.5Cu1Nb3 Si13.5B9 穆斯堡尔谱}     

Effect of annealing temperature on microstructure, hardness and adhesion properties of TiSixNy superhard coatings

A series of TiSi_xN_y superhard coatings with different Si contents were prepared on M42 steel substrates using two Ti and two Si targets by reactive magnetron sputtering at 500 °C. These samples were subsequently vacuum-annealed at 500, 600, 700, 800 and 900 °C, respectively. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), microindenter, Rockwell hardness tester and scratch tester were applied to investigate the microstructure, phase configuration, hardness and adhesion properties of as-deposited and annealed samples. The results indicated that there were two bonds, TiN and Si₃N₄, in all presently deposited TiSi_xN_y thin films, that structure was nanocomposite of nanocrystalline (nc-) TiN embedded into amorphous Si₃N₄ matrices. Annealing treatment below 900 °C played a little role in microstructure and hardness of the coatings although it greatly affected those of steel substrates. The film-substrate adhesion strength was slightly increased, followed by an abrupt decrease with increasing annealing temperature. Its value got to the maximum at 600 °C. Annealing had little effect on the friction coefficient with its value varying in the range of 0.39-0.40.     

The effect of different temperature annealing on phase relation of LaFe11.5Si1.5 and the magnetocaloric effects of La0.8Ce0.2Fe11.5−xCoxSi1.5 alloys

The phase relation of LaFe_11.5Si_1.5 alloys annealed at different high-temperature from 1223 K (5 h) to 1673 K (0.5 h) has been studied. The powder X-ray diffraction (XRD) patterns show that large amount of 1:13 phase begins to form in the matrix alloy consisting of α-Fe and LaFeSi phases when the annealing temperature is 1423 K. In the temperature range from 1423  to 1523 K, α-Fe and LaFeSi phases rapidly decrease to form 1:13 phase, and LaFeSi phase is rarely observed in the XRD pattern of LaFe_11.5Si_1.5 alloy annealed at 1523 K. With annealing temperature increasing from 1573  to 1673 K, the LaFeSi phase is detected again in the LaFe_11.5Si_1.5 alloy, and there is La₅Si₃ phase when the annealing temperature reaches 1673 K. There almost is no change in the XRD patterns of LaFe_11.5Si_1.5 alloys annealed at 1523 K for 3-5 h. According to this result, the La_0.8Ce_0.2Fe_11.5−xCo_xSi_1.5 (0≤×≤0.7) alloys are annealed at 1523 K (3 h). The analysis of XRD patterns shows that La_0.8Ce_0.2Fe_11.5xCo_xSi_1.5 alloys consist of the NaZn₁₃-type main phase and α-Fe impurity phase. With the increase of Co content from x=0 to 0.7, the Curie temperature T_C increases from 180 to 266 K. Because the increase of Co content can weaken the itinerant electron metamagnetic transition, the order of the magnetic transition at T_C changes from first to second-order between x=0.3 and 0.5. Although the magnetic entropy change decreases from 34.9 to 6.8 J/kg K with increasing Co concentration at a low magnetic field of 0-2 T, the thermal and magnetic hysteresis loss reduces remarkably, which is very important for the magnetic refrigerant near room temperature.     

Characterization and compositional study of a ZrO2 engineering ceramic irradiated with a fibre laser beam

Fibre laser surface treatment (FLST) of a cold isostatic pressed (CIP) ZrO₂ engineering ceramic (ZEC) was performed using various processing gas compositions. This is the first time that a surface treatment of ZEC has been employed hitherto by using the fibre laser (FL) radiation to observe the changes on and within the surface of the engineering ceramic; in particular, material removal, surface topography, chemical composition, changes in the surface hardness and distribution of the heat affected zone (HAZ). Bonding of the grain boundaries was found through surface melting with all FL irradiated samples to some extent, but the effect was more marked on the sample FL irradiated with an Ar assist gas and proved to be the most effective combination for modifying the surface morphology. The surface finish and the material removal were varied with the changes in the gas composition. Maximum material removal was observed when an O₂ assist gas was employed on account of the O₂ generating an exothermic reaction. This in turn, produced excessive heating. The compositional analysis revealed a chemical change occurring within the FL irradiated surfaces, regardless of the assist gas used, with the ZEC transforming to zirconia carbide (ZrC).     

Field and temperature induced colossal strain in Gd5(SixGe1−x)4

Gd₅(Si_xGe_1−x)₄, known for its giant magnetocaloric effect, also exhibits a colossal strain of the order of 10,000 ppm for a single crystal near its coupled first-order magnetic-structural phase transition, which occurs near room temperature for the compositions 0.41≤x≤0.575. Such colossal strain can be utilised for both magnetic sensor and actuator applications. In this study, various measurements have been carried out on strain as a function of magnetic field strength and as a function of temperature on single crystal Gd₅Si₂Ge₂ (x=0.5), and polycrystalline Gd₅Si_1.95Ge_2.05 (x=0.487) and Gd₅Si_2.09Ge_1.91 (x=0.52). Additionally a giant magnetostriction/thermally induced strain of the order of 1800 ppm in polycrystalline Gd₅Si_2.09Ge_1.91 was observed at its first order phase transition on varying temperature using a Peltier cell without the use of bulky equipment such as cryostat or superconducting magnet.     

Radiation damage effects on power VDMOS devices with composite SiO2–Si3N4 films

Total dose effects and single event effects on radiation-hardened power vertical double-diffusion metal oxide semiconductor (VDMOS) devices with composite SiO₂-–Si₃N₄ film gate are investigated. The relationships among the important electrical parameters of the samples with different thickness SiO₂-–Si₃N₄ films, such as threshold voltage, breakdown voltage, and on-state resistance in accumulated dose, are discussed. The total dose experiment results show that the breakdown voltage and the on-state resistance barely change with the accumulated dose. However, the relationships between the threshold voltages of the samples and the accumulated dose are more complex, not only positive drift, but also negative drift. At the end of the total dose experiment, we select the group of samples which have the smaller threshold voltage shift to carry out the single event effect studies. We find that the samples with appropriate thickness ratio SiO₂-–Si₃N₄ films have a good radiation-hardening ability. This method may be useful in solving both the SEGR and the total dose problems with the composite SiO₂-–Si₃N₄ films.     

γ-Si3N4在高压下的电子结构和物理性质研究

采用基于密度泛函平面波赝势方法(PWP)和广义梯度近似(GGA-PW91)，计算了不同压强下γ-Si₃N₄的电子结构、光学性质和力学性质.基于计算结果，分析讨论了γ-Si₃N₄各物理参数随外压力的变化规律.计算表明，γ-Si₃N₄是一种适合于在高压条件下工作的材料.     

Microstructure of laser melted Al18B4O33w/2024Al composite

The microstructure of a laser treated Al₁₈B₄O₃₃w/2024Al composite has been investigated using transmission electron microscope (TEM), low-angle (glancing angle) X-ray diffraction (XRD) techniques. Various surface microstructures were observed in the laser treated composite. The Al₁₈B₄O₃₃ whisker on the surface of the composite was decomposed during laser surface melting, various decomposition products were studied in the laser treated composite. Eutectic phases and the precipitation in the matrix of the composite with laser-treated were observed. The main phases detected in the molten zone were aluminum and decomposition products Al₂O₃. The effect of laser treatment on the hardness of the composite was also examined. A surface hardness of 400 Hv was noted.