常压烧结制备Al2O3/TiCN复合陶瓷材料

采用常压烧结的方法制备Al_2O_3/TiCN复合陶瓷,研究了试样成分、烧结温度对试样相对密度、抗弯强度、断裂韧性、Vickers硬度等力学性能的影响。结果表明:采用Al_2O_3 TiCN作为埋粉、氩气保护、在烧结温度低于1650℃,保温时间为1h时,烧结试样的相对密度最高为98.0％,其抗弯强度、断裂韧性、及硬度分别达到最大值,为851 MPa,5.94 MPa·m~(1/2),21.12 MPa。显微结构分析表明:TiCN颗粒弥散在Al_2O_3晶界处,晶粒细小,多在1 μm左右,分布均匀,TiCN与Al_2O_3颗粒相互交织在一起,抑制晶粒生长,从而起到了增韧补强作用,有利于材料力学性能的提高。从压痕裂纹尖端的扩展的扫描电镜照片可以看出:基体与增强相多个晶粒构成的裂纹桥联行为;而有的则在其初始或(和)末端与其他次主裂纹相互作用,形成裂纹偏转、分支与桥联的共存区,主要起作用的是TiCN颗粒弥散增韧机制,它将纯Al_2O_3陶瓷的断裂韧度从3.59 MPa·m~(1/2)提高到5.94 MPa·m~(1/2)。     

Al2O3-Mi3Al复合材料的机械性能研究

金属间化合物已被用来作为第二相物质增韧增强陶瓷材料。本文研究了Ni3 Al增强Al2 O3 复合材料的热压烧结与性能。含有 1 0Vol% (体积百分数 )Ni3 Al的复合材料在 1 3 50℃、2 5MPa热压 60min其相对密度达到 98%。在不同温度下测试了材料的弹性模量、抗弯强度及断裂韧性 ,并利用扫描电镜对相应试样的显微结构与增强机理进行了分析。     

3Y-ZrO2/Fe3Al复合材料的抗热震性能

采用残余强度法测试了单相3Y—ZrO2及3Y—ZrO2/Fe3Al复合材料的抗热震性能,并用诸抗热震参数(R,R'和R"')分析了抗热震性能与材料热力学性能参数之间的关系,同时分析了R阻力曲线与抗热震性能之间的相关性。结果表明:由于相变增韧与桥联增韧的协同作用,复合材料断裂韧性的明显提高,从而使临界热震温差△θc由单相3Y—ZrO2的220℃提高至3Y—ZrO2/30％(in volume)Fe3Al复合材料的450℃。R曲线中韧性初始值K0的升高预示着启动裂纹生长的能量的增大,对应于热震作用下裂纹成核能的提高及△θc的增大。R曲线愈陡,热震作用下裂纹扩展受到的阻力越大,材料的抗热震损伤能力越好。     

Al2O3/Cr3C2/(W,Ti)C陶瓷材料的力学性能及微观结构

用热压烧结工艺在1 700℃,28 MPa保温保压30 min及N2气氛条件下,制备了添加不同含量Cr3C2和(W,Ti)C颗粒的Al2O3/CraC2/(W,Ti)C复合陶瓷材料.对复合陶瓷的力学性能进行测试.用环境扫描电镜、透射电镜和能谱分析仪对复合陶瓷的显微结构进行观察.结果表明与纯Al2O3相比,70Al2O3/10Cr3C2/20(W,Ti)C复合陶瓷材料的显微组织更均匀细化,具有良好的综合力学性能,其断裂韧性自纯Al2Oa陶瓷的4.0 MPa·m1/2提高到8.92 MPa·m1/2.分析发现其内部位错机制、纳米颗粒的淀析、裂纹扩展路径偏转、沿晶断裂、韧窝及解理撕裂等是材料断裂韧性提高的主要原因.     

烧结工艺对Ti/Al2O3复合材料性能的影响

利用放电等离子烧结技术探讨了烧结工艺对40%(体积分数)Ti/Al2O3复合材料性能的影响。实验结果表明,复合材料的性能受烧结温度的影响最为显著,过度延长保温时间会使晶粒发生异常长大,材料性能降低。烧结温度1300℃,保温时间8min制备的复合材料力学性能最佳,其弯曲强度、断裂韧性、显微硬度和相对密度分别为1002.22MPa,19.73MPa·m1/2,18.14GPa和99.74%。     

热压温度和时间对Fe_3Al/Al_2O_3纳米复相陶瓷结构和性能的影响

以自制的纳米晶Fe3Al(有序DO3结构)为增强相,纳米粉Al2O3为基体相,采用热压烧结制备了Fe3Al/Al2O3纳米复相陶瓷,研究了热压温度和时间对复相陶瓷显微结构和力学性能的影响。结果表明:复相陶瓷的相组成为Fe3Al和Al2O3。热压温度为1400℃时,部分晶粒尺寸从0.5μm增大到1μm,板片状Al2O3晶粒消失;热压时间为60min时,晶粒尺寸趋于一致,为1μm左右,呈现出较致密的准球形堆积状态。随着热压温度的升高或热压时间的延长,复相陶瓷的相对密度、Vickers硬度和断裂韧性均有不同程度的提高,最大值分别为93.31%,975MPa和8.30MPa·m1/2。对显微硬度压痕裂纹进行扫描电镜观察和分析表明:材料断裂韧性的提高,是通过对裂纹的偏转和吸收、超细晶韧化和Fe3Al的补强和增韧等方式进行的。     

纳米SiC—Al2O3／TiC多相陶瓷复合材料显微结构的研究

考察了纳米SiC-Al2O3/TiC多相陶瓷复合材料的断裂方式,由于纳米SiC的加入,材料以穿晶断裂为主,通过透射电镜观察,研究了纳米陶瓷复合材料中纳米SiC的分布,证明所制备的材料主要为晶内型纳米复合陶瓷,在纳米SiC-Al2O3/TiC多相陶瓷复合材料中,少量纳米SiC位于基体晶粒间,大多数纳米SiC位于基体晶粒内,而且纳米SiC的加入细化了基体的晶粒,通过高分辨透射电镜观察,研究了纳米SiC－Al2O3/TiC多相陶瓷复合材料中,纳米SiC与基体间界面结合状态,发现在两颗粒间的晶界几乎没有玻璃相,证明纳米陶瓷复合材料中晶界得到了加强,有利于材料力学性能的提高,另外研究了裂纹在材料中的扩展行为,结果表明,纳米粒子对裂纹的扩展起到偏折和钉扎作用。     

纳米TiN改性Al2O3-TiC复合陶瓷的力学性能

通过添加粒径为50～80nm的TiN,改善了Al_2O_3-TiC复合陶瓷的力学性能。以15％(质量分数,下同)的TiN取代15％TiC,制备了纳来TiN改性Al_2O_3-TiC复合陶瓷。结果表明：70％Al_2O_3-15％TiC-15％TiN复合陶瓷的抗弯强度和断裂韧性分别为618 MPa和7.12 MPa·m~(1／2),比70％Al_2O_3-30％TiC的性能(567 MPa和4.96 MPa·m_(1／2))明显提高,特别是断裂韧性提高了64％。纳米TiN改性Al_2O_3-TiC复合陶瓷韧性的提高主要是由于材料致密度的提高和晶粒的细化所致,它的增韧方式为微裂纹、裂纹桥接和偏转。     

无压烧结Al2O3/ZrSiO4复相陶瓷的研究

以Al2O3颗粒为增强体,MgO-Y2O3为烧结助剂,采用无压烧结方法,在组分优化的基础上,制备的锆英石基复相陶瓷室温抗弯强度和断裂韧性分别可达371 MPa和3.4 MPa·m1/2;采用XRD、SEM分析样品的相组成和显微结构,结果显示:确定ZrSiO4为主要晶相,另外还有少量Al2O3和ZrO2的存在;确定复相陶瓷的强韧化是由Al2O3颗粒引发的裂纹偏转、微裂纹增韧和由ZrSiO4分解而来的ZrO2相变增韧共同作用而实现的,断裂方式主要为穿晶断裂.     

钇补强颗粒弥散陶瓷复合材料增韧机制的微观结构表征

在Al2O3/（W,Ti）C陶瓷复合材料中适量添加稀土元素钇能显著提高其断裂韧性。本文运用SEM与TEM技术,从微观结构的角度探讨了其增韧机制。表明,由于稀土钇的添加,使材料内部形成不同程度的强弱界面,它们与扩展中的裂纹相互作用,使得裂纹桥联、裂纹分支、裂纹偏转以及微裂纹增韧机制得到明显增加和加强,从而以多种增韧机制及其协同作用共同提高稀土补强Al2O3/（W,Ti）C陶瓷复合材料的断裂韧性。     

Al2O3 loss prediction model of selective laser melting Al2O3–Al composite

The element/phase loss is undesirable but existing during selective laser melting (SLM) of materials with volatile element/phase, which not only changes the material composition but also affects the molten pool flow. In the previous researches, the effect of remelting on the element/phase loss was neglected during the SLM process, instead, laser energy density was thought to be uppermost. In fact, the SLM process fabricates the parts in a manner of line by line and layer by layer, i.e., additive character, and the remelting in the overlap zone occurs during the SLM process. In this paper, three different Al₂O₃ loss prediction models of SLM Al₂O₃–Al composite by considering the additive character of SLM and the distribution of the Al₂O₃ associated with the different molten pool driving forces were developed. By comparing with the experimental results and predicted results, it is found that the Al₂O₃ is distributed on both sides of the molten pool under the combined action of the Marangoni flow and the evaporation recoil pressure. This kind of Al₂O₃ distribution enhances the effect of the remelting on the Al₂O₃ loss, i.e., the remelting brings a logarithmic increase in the Al₂O₃ loss rate. This determines the final Al₂O₃ loss rate of the SLMed 3D samples. During this study, although the Al₂O₃ loss rate of the single-track is only 33%, the loss rate of SLMed 3D samples increases significantly to 97% when the hatching space of 60 μm and scanning speed of 200 mm/s are utilized, i.e., almost no Al₂O₃ in the 3D sample. Thus, it is more important to reduce the remelting, i.e., overlap rate for reducing the element/phase loss. This study is a benefit for understanding and reducing the element/phase loss in SLM.     

Optical absorption and selective thermal emission in directionally solidified Al2O3-Er3Al5O12 and Al2O3-Er3Al5O12-ZrO2 eutectics

Al₂O₃-Er₃Al₅O₁₂ and Al₂O₃-Er₃Al₅O₁₂-ZrO₂ eutectic ceramic rods were directionally solidified using the laser floating zone technique at several growth rates. Binary eutectic microstructure consisted in a three-dimensional interpenetrated network of the eutectic phases whereas the ternary eutectic showed a geometrical microstructure at low growth rates and a nanofibrillar pattern at high rates. The microstructure size was strongly dependent on the growth rate, decreasing when the processing rate increased. The optical absorption was measured in the samples at room temperature and Judd–Ofelt analysis was used to model the optical absorption of the Er³⁺ ions. Thermal emission of the eutectic rods was studied at temperatures up to 1600 °C. An intense narrow emission band at 1.55 μm matching with the sensitive region of the GaSb photoconverter was obtained. The intensity of the selective emission band is larger for the binary eutectic than for the ternary compound and increases as the microstructural size decreases.     

Al2O歧化法制备微细Al2O3/Al复合粉体

真空条件下,以Al2O3和Al为原料,通过Al2O歧化法制备微细Al2O3/Al复合粉体.XRD和SEM分析表明:在反应温度为1200～1400℃时,随着温度的升高,粉体中氧化铝含量升高;冷凝温度约为550～750℃时,复合粉体中的氧化铝包括稳定晶型和不稳定晶型;冷凝温度约为1100～1300℃时,复合粉体中的氧化铝全部为稳定晶型;冷凝温度约为550～650℃时,复合粉体的平均粒径小于0.5μm;冷凝温度约为750℃时,铝熔化、微粒团聚;冷凝温度约为1100～1200℃时,铝形成铝珠,氧化铝为不规则状、平均粒径小于2μm;冷凝温度约为1300℃时,氧化铝为片状.因此,通过选取合适的反应温度、冷凝温度,可以控制Al2O3/Al复合粉体中氧化铝的含量、晶型和粒径.     

Combustion of Al–Al2O3 mixtures in air

An experimental study on the aluminum oxynitride and aluminum nitride formation by combustion of mixtures of micron-sized aluminum powder (average particle diameter a_s ∼9.0 μm) and alumina nanopowder (a_s ∼0.05 μm) of the fixed mass (∼10 g) and different mass ratios (Al/γ-Al₂O₃ = 0.1–19.0) in air is reported. The formation of aluminum oxynitride (Al₃O₃N) and aluminum nitride during the combustion of powdery aluminum-based mixtures in air is discussed in this study. The combustion synthesis of Al₃O₃N and AlN was carried out in self-sustaining way. XPS-FESEM, XRD and chemical analysis were executed on final products of synthesis. The combustion process was also recorded by a video-camera. It was found that powdery mixtures, ignited by local heating, burned in one- or two-stage self-propagating regime. The combustion regime is different for different initial mass ratios Al/γ-Al₂O₃ and mainly depends on the content of fuel (aluminum powder) in mixture.     

Fe3Al/Al2O3陶瓷复合梯度涂层抗热震性研究

通过800℃-压缩空气冷却热循环实验，对Fe3Al／A12O3梯度涂层的抗热震性和热震机制进行了研究。结果表明：涂层的主要热震损坏形式是随着循环次数的增加而产生的剥落。当裂纹在Al2O3中出现时，涂层将沿着基体一涂层界面迅速剥离，而对梯度涂层则具有相当的抗热震能力。实验证明：Fe3Al中间层和涂层成分的梯度变化缓解了热循环应力，提高了抗热震损坏能力，同时，有利于涂层结合强度的提高。     

Al2O3/Al2O3扩散连接机理的研究

采用热压方式进行氧化铝陶瓷材料的扩散连接，并深入探讨了其连接机理，结果表明：采用适当的连接工艺，可使此种材料产生塑性形变，接触面积增加，空洞收缩和闭合，扩散进行充分，1420℃，15MPa热压60min条件下，获得的最高强度为357MPa，超过母材强度平均连接强度为250MPa，是母材平均强度的85％。     

Fe3Al/Al2O3复合材料的凝胶注模成型工艺研究

机械合金化法制备Fe3Al粉,用凝胶注模成型的方法制备Fe3Al/Al2O3复合材料.结果表明,用凝胶注模成型工艺制备出了Fe3Al/Al2O3复合材料,分散剂MN可以显著提高浆料的固相含量,固相含量对浆料流变性有重要影响,10% Fe3Al/Al2O3坯体的微观结构最均匀.     

Ruby micro-piezospectroscopy in GdAlO3/Al2O3(/ZrO2), Er3Al5O12/Al2O3(/ZrO2) and Y3Al5O12/Al2O3(/ZrO2) binary and ternary directionally solidified eutectics

The fluorescence from (naturally present) Cr³⁺ impurities was used to measure the residual stress in the alumina phase of six melt-grown ceramic eutectic composites associating gadolinum aluminum perovskite (GAP), erbium aluminum garnet (EAG) or yttrium aluminum garnet (YAG) with α-alumina and cubic zirconia. Such measurements are reported for the first time in the GAP containing eutectics.In the usual hydrostatic assumption, we conclude to a residual compression in the range of ～70–400 MPa depending on the sample composition. The validity of the hydrostatic assumption is questioned when a microscope is used for the measurements.