添加BaTiO3的热压烧结Si3N4陶瓷的力学和介电性能

本研究以Al₂O₃和Nd₂O₃为烧结助剂, 采用热压烧结法制备Si₃N₄陶瓷, 系统研究了添加BaTiO₃对Si₃N₄陶瓷力学和介电性能的影响。研究结果表明, 随着BaTiO₃含量的增加, 相对密度、抗弯强度和维氏硬度都随之降低, 而断裂韧性有所升高; 即使添加5wt%~20wt%的BaTiO₃, Si₃N₄陶瓷的抗弯强度依然可以保持在600 MPa以上。Si₃N₄陶瓷的介电常数可以提高到9.26~11.50, 而介电损耗保持在10^-3量级。在Si₃N₄陶瓷中未检测到BaTiO₃结晶相, 可以认为Si₃N₄陶瓷介电常数的提高主要来源于烧结过程中形成的TiN。这些结果有助于拓展Si₃N₄陶瓷的应用领域。     

BN含量对多孔BN/Si3N4陶瓷结构和性能的影响

以氮化硅(Si₃N₄)为基体, 氮化硼(BN)为添加剂, 叔丁醇为溶剂, 采用凝胶注模成型与无压烧结工艺(温度为1750 ℃、保温时间为1.5 h、流动N₂气氛), 成功制备出具有一定强度和低介电常数的多孔BN/Si₃N₄陶瓷。在浆料中初始固相含量固定为15%体积分数的基础上, 研究了BN含量对多孔Si₃N₄陶瓷材料的气孔率、物相组成及显微结构的影响, 分析了抗弯强度、介电常数与结构之间的关系。结果表明, 通过改变BN含量可制备出气孔率为55.1%~66.2%的多孔Si₃N₄陶瓷; 多孔BN/Si₃N₄复合陶瓷的介电常数随着BN含量的增加而减小, 为3.39~2.25; 抗弯强度随BN含量提高而有所下降, BN质量分数为2.5%时, 抗弯强度最高, 为(74.8±4.25) MPa。     

1450℃反应烧结Fe3Si-Si3N4复合耐火材料的相组成

以Si粉和Fe₃Si-Si₃N₄为原料,在高纯N₂气氛下制备Si₃N₄/Fe₃Si-Si₃N₄复合材料。氮化烧成后Si₃N₄结合Fe₃Si-Si₃N₄复合耐火材料试样中物相为Si₃N₄、Fe₂Si、FeSi和Si₂N₂O。其中Si₂N₂O含量约6%,且在试样中心和外部分布不均匀。Fe₃Si-Si₃N₄原料是Fe₃Si和Si₃N₄两相共存材料,热力学评估和材料的微观结构分析表明,Fe₃Si和部分Si粉形成新的低熔点硅铁合金,使靠近试样表面部位的部分开口气孔被液态硅铁合金所堵塞或填充,试样中心部位的微量氧不能迁移至外部,N₂中微量氧将Fe₃Si-Si₃N₄原料中Si₃N₄氧化,形成Si₂N₂O包裹,导致试样中心Si₂N₂O含量比边缘部位高。Si₂N₂O的形成使体系氧分压降至Si₃N₄稳定存在的氧分压时,Si粉直接氮化形成柱状Si₃N₄,而非纤维状Si₃N₄,同时在1 450℃氮化烧成条件下,Fe的存在促进了α-Si₃N₄向β-Si₃N₄的转变。     

复合烧结助剂对Si3N4陶瓷力学性能和热导率的影响

Si₃N₄陶瓷因兼具优异的力学和热学性能, 成为第三代半导体陶瓷基板的首选材料之一。本研究以7种不同离子半径的稀土氧化物(RE₂O₃, RE=Sc、Lu、Yb、Y、Gd、Nd、La)与非氧化物(MgSiN₂)作复合烧结助剂, 通过热压烧结和退火热处理制备了高强、高热导Si₃N₄陶瓷, 并系统研究了复合烧结助剂中RE₂O₃种类对Si₃N₄陶瓷物相组成、微结构、力学性能和热导率的影响规律。热压后Si₃N₄陶瓷力学性能优越, 其中添加Nd₂O₃-MgSiN₂的样品弯曲强度达到(1115±49) MPa。退火处理后Si₃N₄陶瓷的热导率得到大幅提升, 呈现出随稀土离子半径减小而逐渐增大的规律, 其中添加Sc₂O₃-MgSiN₂的样品退火后的热导率从54.7 W·m^-1·K^-1提升至80.7 W·m^-1·K^-1, 提升了47.6%。该结果表明, 相较于国际上通用的Y₂O₃-MgSiN₂和Yb₂O₃-MgSiN₂烧结助剂组合, Sc₂O₃-MgSiN₂有望成为制备高强度、高热导Si₃N₄陶瓷的新型复合助剂。     

Si3N4对碳/碳复合材料表面SiC涂层耐磨性的影响

为了提高碳/碳复合材料表面SiC涂层的耐磨性,采用包埋法和氮化处理制备SiC/Si₃N₄涂层。通过X射线衍射仪（XRD）、扫描电子显微镜（SEM）、能谱分析仪（EDS）及摩擦磨损试验,分别评价SiC涂层与SiC/Si₃N₄涂层的表面形貌、物相组成、磨损形貌及摩擦磨损性能,并研究涂层显微组织结构与磨损机理之间的联系。结果表明：SiC/Si₃N₄涂层由Si₃N₄相、SiC相和C相组成,涂层平整且致密;SiC/Si₃N₄涂层的摩擦系数低于0.05且更稳定;SiC涂层高摩擦系数值的主要磨损机制是黏着磨损和磨料磨损;SiC/Si₃N₄涂层中形成了一层较薄的润滑膜,并在摩擦磨损的后续阶段降低摩擦系数。Si₃N₄相的引入可以有效改善SiC涂层的表面结构,使得SiC涂层摩擦系数更小且更稳定,从而提高...     

氮化硼纳米管增强氮化硅复合材料的裂纹扩展阻力行为

用氮化硼纳米管(BNNT)增强氮化硅(Si₃N₄)陶瓷制备了BNNT/Si₃N₄复合材料, 利用三点弯曲强度及单边切口梁(SENB)法测定了BNNT/Si₃N₄复合材料的弯曲强度和断裂韧性。通过SEM观察了BNNT/Si₃N₄复合材料微观形貌。基于BNNT增强Si₃N₄陶瓷复合材料的裂纹扩展阻力计算公式, 构建了BNNT对Si₃N₄陶瓷裂纹屏蔽区的裂纹扩展阻力的数学模型。用该模型的计算结果与Si₃N₄陶瓷的裂纹扩展阻力进行了对比。结果表明: BNNT/Si₃N₄复合材料的弯曲强度和断裂韧性明显高于Si₃N₄陶瓷, 说明BNNT对Si₃N₄陶瓷的裂纹扩展有阻力作用, 摩擦拔出是Si₃N₄陶瓷抗裂纹扩展能力提高的主要原因; BNNT对Si₃N₄陶瓷有明显的升值阻力曲线行为。通过有限元模拟裂纹尖端应力分布, 发现BNNT使Si₃N₄陶瓷裂纹尖端的最大应力转移到纳米管上, 而且BNNT降低了Si₃N₄陶瓷裂纹尖端的应力, 对Si₃N₄陶瓷尖端的裂纹有屏蔽作用, 从而提高了Si₃N₄陶瓷的裂纹扩展阻力。     

界面反应对Cu35Ni25Co25Cr15多主元合金/金刚石复合材料磨损性能的影响

金刚石超硬磨具在高端芯片加工、3C陶瓷等领域发挥的作用日益重要,粘结相与金刚石的界面结合情况在很大程度上影响了金刚石超硬复合材料的力学和磨损性能。为了研究粘结相和金刚石的界面结合情况,采用放电等离子烧结方法制备了Cu₃₅Ni₂₅Co₂₅Cr₁₅多主元合金/金刚石复合材料,通过热力学计算和实验研究了粘结相和金刚石颗粒的界面反应。结果表明：烧结过程中,金属粘结相中的Cr元素与金刚石在界面处发生了化学反应,生成Cr-C化合物,且Cr-C化合物层的厚度随着烧结温度的升高而增加。当烧结温度达到950℃时,Cr-C化合物反应层均匀连续,厚度大约为1.1μm。复合材料粘结相与金刚石颗粒的粘结系数随着Cr-C化合物层厚度的增加而增大。摩擦磨损测试表明,在900℃和950℃烧结的样品表面,粘结相在摩擦过程中首先被磨除,金刚石随后露出,而Cr-C界面反应层有助于保持对金刚石颗粒的把持能力,提高复合材料的磨削性能。因此,适当的界面反应可提升金刚石复合材料的服役性能。     

(SiC,TiB2)/B4C复合材料的烧结机理

研究了在热压条件下制备 (SiC, TiB₂)/ B₄C复合材料的烧结机理。认为烧结助剂的加入使本体系成为液相烧结,同时粉料的微细颗粒对复合材料的烧结致密也有重要贡献。分析和测量了制取的复合材料的相组成、显微结构和力学性能。结果表明,采用B₄C与Si₃N₄和少量SiC、TiC为原料,Al₂O₃＋Y₂O₃为烧结助剂,在烧结温度1800~1880℃,压力30 MPa的热压条件下烧结反应生成了SiC、TiB₂和少量的BN,制取了(SiC, TiB₂)/B₄C复合材料。所形成的晶体显微结构为层片状。制得的试样的硬度、抗弯强度和断裂韧性分别可达HRA88.6、540 MPa和5.6 MPa·m1/2。      

基于第二抗热震因子的BNNTs/Si3N4复合材料抗热震性能评价

利用Kingery抗热震断裂理论构建了氮化硼纳米管（BNNTs）强韧化陶瓷复合材料的第二抗热震因子模型,通过真空热压烧结法制备了BNNTs质量分数分别为0.5wt%、1.0wt%、1.5wt%和2.0wt%的BNNTs/Si₃N₄复合材料,并采用预制裂纹法测试了复合材料的抗热震性能,测试结果证实了在平稳状态下模型的正确性。结果表明,BNNTs的存在使复合材料第二抗热震因子增大,抗热震性能提升。分布在晶界上的BNNTs起到裂纹钉扎、桥联和裂纹偏转作用,增加了裂纹扩展的阻力,从而有效提高了BNNTs/Si₃N₄复合材料抗热震断裂能力。     

用聚碳硅烷为先驱体制备SiC/Si3N4纳米复相陶瓷

采用聚碳硅烷(PCS) 为先驱体, 利用原位生长法制备SiC/Si₃N₄ 纳米复相陶瓷, 其室温弯曲强度和断裂韧性达到了637M Pa 和8. 10M Pa·m1/2 。研究了材料微观结构的形成及断裂机理,指出在微观结构的形成过程中, 控制SiC 纳米微晶的生成和B-Si₃N₄ 柱状晶的生长是关键, 而增韧补强的主要原因在于形成了晶内型结构和长径比大(大于7. 5) 的Si₃N₄ 柱状晶, 从而改变了断裂机理。      

SPS制备氮化硅/锌铝基复合材料的组织和性能研究

通过放电等离子烧结工艺制备了氮化硅/锌铝基复合材料,重点探讨了氮化硅添加量对氮化硅/锌铝基复合材料致密度、硬度和摩擦性能的影响.采用扫描电子显微镜(SEM)及电子探针X射线显微分析仪(EPMA)对样品的微观组织进行了分析,并使用显微硬度仪、旋转摩擦试验仪对其性能进行了研究.结果表明:氮化硅在样品中分散均匀,且氮化硅的加...     

Preparation of porous Fe2O3/SiO2 nanocomposite abrasives and their chemical mechanical polishing behaviors on hard disk substrates

Abrasives play an important role in chemical mechanical polishing (CMP) processes. Compact solid silica particles, which have been widely used as abrasive in CMP slurries, may cause surface defects because of their high hardness. Porous silica abrasive exhibits better surface planarization and fewer scratches than traditional solid silica abrasive during the polishing of hard disk substrates. However, the improvement in material removal rate (MRR) was not significant. Therefore, porous Fe₂O₃/SiO₂ nanocomposite abrasives were prepared and their CMP performances on hard disk substrates were investigated. Experiment results indicate that the MRR of slurry containing porous Fe₂O₃/SiO₂ nanocomposite abrasives is obviously higher than that of slurry containing pure porous silica abrasive under the same testing conditions. MRR increases with the increase of the molar content of iron in porous Fe₂O₃/SiO₂ nanocomposite abrasives. Moreover, surfaces polished by slurries containing the porous Fe₂O₃/SiO₂ nanocomposite abrasives exhibit lower surface roughness, fewer scratches as well as lower topographical variations than that by pure porous silica abrasive.     

Si3N4/hBN复相陶瓷的研究现状及进展

Si3N4/hBN复相陶瓷凭借优良的综合力学性能,逐渐成为人们研究的热点。从制备工艺和性能出发阐述了国内外Si3N4/hBN复相陶瓷的研究现状,分析了各种制备方法的优缺点以及hBN含量对Si3N4/hBN复相陶瓷的可加工性能、力学性能、介电性能、摩擦学性能的影响,并指出简化工艺、降低烧结温度、hBN含量与性能定量表征等可能是今后的发展方向。     

Machinability study of abrasive aqua jet parameters on hybrid metal matrix composite

The present work involves investigation of the abrasive aqua jet (AAJ) machining of hybrid metal matrix which consists of Al 6063 reinforced with boron carbide (B₄C) and zirconium silicate (ZrSiO₄) in the form of particulates in the proportion of 5% B₄C and 5% ZrSiO₄. The Response surface method using a central composite design was adopted for conducting experiments by changing the aqua jet pressure, abrasive flow rate, and traverse rate. The results were taken with different types of abrasives of various mesh sizes in this study, which were analyzed using response surface graphs. The striation effect on the bottom-machined surfaces was also examined using the striation length and its frequency. Surface topography and morphology were analyzed on the AAJ-machined composite kerf wall cut surfaces. The machined surface exhibited the inherent characteristics of AAJ which included wear tracks, and contamination generated in the metal surface. The experimental results revealed that higher abrasive flow rate (400 g/min), lower traverse rate (30 mm/min), and higher aqua jet pressure (300 MPa), the production of a higher material removal rate, lower surface roughness and kerf taper angle.     

Study on particle-stabilized Si3N4 ceramic foams

The stability of bubbles and the microstructures of sintered Si₃N₄ ceramic foams produced by direct foaming method were investigated. The bubbles produced by short-chain amphiphiles (propyl gallate) have higher stability as compared with that produced by long-chain surfactants (TritonX-114). Si₃N₄ ceramic foams using short-chain amphiphile are particle-stabilized one, the pore cells are spherical and closed, and cell surfaces are smooth and dense. The pore cells of sintered Si₃N₄ ceramic foams using TritonX-114 foaming are coarse and large, and pore cells are polyhedral. High gas-pressure sintering is conducive to the development of the whisker-like microstructures in Si₃N₄ ceramic foams. The sintered Si₃N₄ ceramic foams with the whisker-like microstructure are quite promising for improving the mechanical strength of the ceramics by a simple and safe way.     

Effect of Si3N4-particles addition in Ag-Cu-Ti filler alloy on Si3N4/TiAl brazed joint

A novel composite filler alloy was developed by introducing Si₃N_4p (p = particles) into Ag-Cu-Ti filler alloy. The brazing of Si₃N₄ ceramics and TiAl intermetallics was carried out using this composite filler alloy. The typical interfacial microstructure of brazed joints was: TiAl/AlCu₂Ti reaction layer/Ag_(s,s) + Al₄Cu₉ + Ti₅Si_3p + TiN_p/TiN + Ti₅Si₃ reaction layer/Si₃N₄. Effects of Si₃N_4p content in composite filler alloy on the interfacial microstructure and joining properties were investigated. The distribution of Ti₅Si_3p and TiN_p compounds in Ag-based solid solution led to the decrease of the mismatch of the coefficient of thermal expansion (CTE) and the Young's modulus between Si₃N₄ and TiAl substrate. The maximum shear strength of 115 MPa was obtained when 3 wt.% Si₃N_4p was added in the composite filler alloy. The fracture analysis showed that the addition of Si₃N_4p could improve the mechanical properties of the joint.     

Feasibility study of a flexible grinding method for precision machining of the TiAl-based alloy

This study presents detailed experimental investigations on precision machining of the TiAl-based alloy with an abrasive belt flexible grinding method. Subsequently, the feasibility of this precision machining method is evaluated with respect to the material removal rate, abrasive wear, machined surface roughness, and residual stress. The material removal rate and surface roughness were determined as experimental indicators and were measured via a three-coordinate measuring instrument and surface profiler, respectively. Micro-morphologies of the machined surface and worn abrasive belt were investigated via a scanning electron microscope. The residual stress distributions in the machined surface layer were detected by using an X-ray diffractometer. The experimental results revealed that the aforementioned evaluation indicators satisfied the desired requirements, thereby indicating that the abrasive belt flexible grinding technique was suitable for precision machining of the TiAl-based alloy. Additionally, the optimal combinations of grinding parameters were determined to obtain desirable material removal rate and machined surface roughness. The basic wear processes and characteristics of the abrasive belt were thoroughly examined. The formation of desirable residual compressive stresses in the machined surface layer was mainly attributed to low frequency and small amplitude vibration knocking at the grinding interface.     

Si3N4和52100钢对磨副材料对CrN薄膜干摩擦学行为的影响

利用阴极电弧离子镀技术在316L不锈钢基体上制备了CrN薄膜。采用扫描电子显微镜(SEM)、X射线衍射仪(XRD)、纳米压痕仪对CrN薄膜的形貌、成分和力学性能进行了表征。为了研究Si_3N_4和52100钢对磨副材料对CrN薄膜和316L不锈钢干摩擦行为的影响,在2N、5N、8N三种载荷下,将CrN薄膜和316L不锈钢基体与Si_3N_4陶瓷球和52100钢球分别进行了往复式滑动干摩擦实验。采用扫描电子显微镜观察了磨痕的微观形貌,并对CrN薄膜和316L不锈钢基体的磨损机制进行了分析。结果表明:CrN薄膜表面平整,缺陷较少;CrN薄膜的纳米硬度约为28GPa,弹性模量约为350GPa;与Si_3N_4陶瓷球相比,CrN薄膜与52100钢球摩擦时摩擦因数相对较小(保持在0.7左右)且更加稳定;316L不锈钢的摩擦因数远大于CrN薄膜且波动较大;对磨球为Si_3N_4陶瓷球时,CrN薄膜的主要磨损机制为磨粒磨损,伴有少量的氧化和黏着磨损,316L不锈钢的磨损机制主要为磨粒磨损和塑性变形,伴有少量的氧化和黏着磨损;对磨球为52100钢球时,CrN薄膜的主要磨损机制为黏着磨损,伴有少量的氧化,316L不锈钢的磨损机制主要为黏着磨损,伴有少量的氧化和磨粒磨损。CrN薄膜与两种对磨球的磨损量均小于316L不锈钢基体的磨损量,说明CrN薄膜有效提高了基体的耐磨性。     

Properties of polyimide/Al2O3 and Si3N4 deposited thin films

Polyimide (PI) nanocomposites with different proportions of Al₂O₃ were prepared via two-step reaction. Silicon nitride (Si₃N₄) was deposited on PI composite films by a RF magnetron sputtering system and used as a gas barrier to investigate the water vapor transmission rate (WVTR). The thermal stability and mechanical properties of a pure PI film can be improved obviously by adding adequate content of Al₂O₃. At lower sputtering pressure (4 mTorr), the PI/Al₂O₃ hybrid film deposited with Si₃N₄ barrier film exhibits denser structure and lower root mean square (RMS) surface roughness (0.494 nm) as well as performs better in preventing the transmission of water vapor. The lowest WVTR value was obtained from the sample, 4 wt.%Al₂O₃-PI hybrid film deposited with Si₃N₄ barrier film with the thickness of 100 nm, before and after bending test. The interface bonding, Al-N and Al-O-Si, was confirmed with the XPS composition-depth profile.     

Structure of double interfaces system of Si3N4/SiO2/Si irradiated by γ-rays

The interfacial structures of double interfaces system of Si₃N₄/SiO₂/Si were examined using X-ray photoelectron spectroscopy (XPS) before and after ⁶⁰Co radiation. The experimental results demonstrate that there existed two interfaces, one consisted of Si₃N₄ and SiO₂, while another was made of Si and SiO₂, the interface between SiO₂ and Si was extended towards the interface of the Si₃N₄/SiO₂ meanwhile the center of the former interface was removed in the direction of the latter interface by ⁶⁰Co. The concentration of silicon in the Si₃N₄ state (BE 101.8 eV) was decreased with the variation of radiation dosage as well as bias field within the SiO₂-Si interface, remarkably. The mechanism for the experimental results is analyzed.