TA32钛合金高温连续氧化行为研究

本文采用增重法研究了表面有/无喷涂高温润滑剂的TA32钛合金在热成形温度750℃~850℃范围内氧化10min-240h的氧化行为,通过SEM和EDS等微观分析方法对氧化层的表面形貌和成分、截面厚度和成分进行分析,并对氧化机理进行探讨。结果表明,750℃-850℃内的氧化行为均符合直线-抛物线规律,800℃～850℃内氧化速率迅速增加,氧化程度剧烈,温度是TA32钛合金氧化行为的重要影响因素之一。750℃时,氧化膜基本没有脱落,800℃时氧化膜部分脱落,温度升高到850℃时,氧化皮大块脱落。750℃-850℃内,随着保温时间的增加,氧化膜逐渐增厚,氧化物由颗粒状变为短棒状和针状,氧化皮逐渐由致密变得疏松多孔,抗氧化能力逐渐下降。TA32钛合金在750℃保温240h时,氧化层结构为：TiO₂和Al₂O₃/ TiO₂/ Al₂O₃/ TiO₂/基体;在800℃下氧化240h时,氧化层结构为：TiO₂和Al₂O₃/ Al₂O₃/ TiO₂/ Al₂O₃/ TiO₂/ Al₂O₃/ TiO₂/ Al₂O₃/ TiO₂/基体;在850℃下氧化240h时,表层氧化膜完全脱落。表面无喷涂试样和表面喷涂氮化硼的试样氧化规律一样,均符合直线-抛物线规律,但表面无喷涂试样的单位面积增重、氧化速率高于表面喷涂氮化硼的试样,氧化膜厚度也更厚,说明氮化硼有很好的抗氧化性能。表面喷涂氮化硼的TA32钛合金在750℃保温240h时,氧化层结构为：TiO₂和Al₂O₃/ TiO₂/ Al₂O₃/ TiO₂/Ti₃Al/基体。     

等离子喷涂制备MoSi<sub>2</sub>-CoNiCrAlY复合涂层的高温氧化行为

以高能球磨法制备的纳米MoSi<sub>2</sub>-CoNiCrAlY复合粉末为喷涂材料,利用等离子喷涂技术在GH4169合金表面沉积了MoSi<sub>2</sub>-CoNiCrAlY复合涂层,并研究了GH4169基材和复合涂层合金试样在900°C静态大气环境下的循环氧化行为。结果表明：复合涂层表现出较好的抗高温氧化性能,其氧化速率仅为1.23×10<sub>-7</sub> mg<sub>2</sub>.cm<sub>-4</sub>.s<sub>-1</sub>,这归因于MoSi<sub>2</sub>在氧化早期形成了SiO<sub>2</sub>相,可以自封氧化膜。氧化后期SiO<sub>2</sub>的脱落,Mo<sub>5</sub>Si<sub>3</sub>相的再次氧化生成MoO<sub>3</sub>和MoO<sub>2</sub>气相,以及MoSi<sub>2</sub>的内氧化直接气化,会降低涂层的抗氧化性能。     

超声辅助对共沉淀法制备富锂锰基正极材料Li[Li_0.144Ni_0.136Co_0.136Mn_0.544]O₂性能影响的研究

通过超声辅助共沉淀法成功制备了富锂锰基正极电极材料,研究了不同的超声时间对材料形貌、结构和电化学性能的影响。研究发现,超声辅助能够使材料颗粒更加均匀,结构更合理,有利于材料电化学性能的提升。当合成前躯体材料超声时间为8h时,复合材料的放电比容量最好,在0.1C的初始放电比容量为327.8 mAh g_-1,均高于未超声的复合材料的265.2 mAh g_-1,1C下循环50圈后放电容量为181.6 mAh g_-1,保持率为84.8%。通过循环伏安法测试和电化学交流阻抗测试,发现超声后的复合材料还原氧化峰电流更大,电荷转移阻抗更小,具有较好的倍率性能。     

LZO对热障涂层中粘结层氧化的抑制行为研究

为了阐明LZO对热障涂层(TBCs)中粘结层氧化的抑制作用,利用爆炸喷涂(D-gun)在310S基体上制备NiCoCrAlY粘结层,大气等离子(APS)制备单陶瓷8YSZ涂层和双陶瓷LZO/8YSZ涂层。采用SEM、EDS和XRD表征了不同结构TBCs喷涂态及高温氧化后的微观组织和相结构。结果表明：1100 ℃下等温氧化(100小时)后双陶瓷LZO/8YSZ与单陶瓷8YSZ热障涂层相对氧化增重分别为2.82 mg/cm₂和3.13 mg/cm₂,TGO生长速率常数K_p分别为5.79×10_-2μm₂/h和6.26×10_-2μm₂/h,厚度分布范围分别为3.75-5.25 μm和5-5.5 μm。相比单陶瓷TBCs,LZO/8YSZ双陶瓷TBCs中粘结层表现出氧化增重少、TGO生长速率低、粘结层中β相转变慢等明显特征。     

磷酸铁锂/石墨烯复合材料的低温微波水热法制备及性能

采用喷雾干燥结合低温微波水热法制备了石墨烯/LiFePO₄复合正极材料,利用SEM、XRD、DLS等对其微观形貌、结构、粒度分布进行了表征,并利用恒流充放电、CV、EIS等测试研究了复合正极材料的电化学性能和电极动力学过程。结果表明,与未包覆的样品相比,石墨烯包覆的LiFePO₄具有优异的倍率性能(5C放电比容量为125.4 mAh?g_-1)和循环稳定性(1C条件下100次充放电后容量保持率在95%左右)。包覆石墨烯后LiFePO₄正极材料的电荷迁移电阻减小,电化学可逆性增强,从而提高了材料的倍率性能。本文提供了一条提高磷酸铁锂正极材料电化学性能的简便途径,具有良好的应用前景。     

石墨烯掺杂和烧结温度对MgB<sub>2</sub>块体微观结构和超导性能的影响

我们采用未掺杂的粉末制备了MgB<sub>2</sub>块体作对比,研究了石墨烯掺杂对MgB<sub>2</sub>块材微观结构和超导性能的影响,研究了退火温度对石墨烯掺杂MgB<sub>2</sub>块材微观结构和超导性能的影响。对烧结后的样品采用XRD,SEM,SQUID进行了相组成,微观结构和超导性能等分析检测。研究发现石墨烯掺杂明显提高了MgB<sub>2</sub>超导材料的临界电流密度,在20 K和1 T磁场下,最大的临界电流密度达到1.8×10<sub>5</sub>A/cm<sub>2</sub>。     

TiAl合金表面阴极微弧沉积Al<sub>2</sub>O<sub>3</sub>陶瓷涂层的生长过程与相组成

目的：利用阴极微弧沉积技术在预处理后的TiAl合金表面制备了Al<sub>2</sub>O<sub>3</sub>陶瓷涂层,研究了涂层的生长过程和相组成。方法：采用电子扫描电镜(SEM、EDS)、电子透射电镜(TEM)、X射线衍射(XRD)等方法,对Al<sub>2</sub>O<sub>3</sub>涂层的生长过程中的微观形貌、组织成分以及晶体结构的演变进行了研究与分析。结果：TiAl合金表面阴极微弧沉积过程中,在阴极表面发生非晶态Al(OH)<sub>3</sub>的吸附、脱水烧结形成Al<sub>2</sub>O<sub>3</sub>陶瓷涂层的沉积。结论：Al<sub>2</sub>O<sub>3</sub>涂层生长分前期Ⅰ、中期Ⅱ和后期Ⅲ三个阶段,前期起弧阻挡层被击穿,涂层生长较慢、组织致密且与基体结合良好;反应中期涂层生长较快,Al(OH)<sub>3</sub>不断吸附和脱水烧结,涂层结晶度提高;反应后期涂层生长速度变缓,表层组织疏松、多孔,相组成为87.5 %的α–Al<sub>2</sub>O<sub>3</sub>和12.5 %的γ–Al<sub>2</sub>O<sub>3</sub>。     

Nd对Mg-13Gd-0.5Zr合金组织和力学性能的影响

采用X射线衍射仪、光学显微镜、扫描电镜、能谱仪和电子拉伸试验机等设备研究了Nd对Mg-13Gd-0.5Zr合金组织和力学性能的影响,结合错配度理论、位错密度的变化规律讨论了合金晶粒细化的机理,并从细晶强化和析出强化等方面阐述了合金强化机制。研究发现Mg-13Gd-0.5Zr合金的组成相主要有α-Mg、Mg₅Gd,Nd的加入在合金中形成了新相Mg₄₁Nd₅,并细化了合金晶粒。Nd的加入显著提高了Mg-13Gd-0.5Zr合金的室温和高温力学性能,当Nd的添加量为2%时,合金在室温和高温下的力学性能达到最大值279(室温)、319 MPa(250 ℃),合金力学性能的提高主要归因于Mg₅Gd和Mg₄₁Nd₅相的析出强化和细晶强化的双重效果。Mg-13Gd-2Nd-0.5Zr合金在不同温度下的断裂方式主要以脆性断裂为主,随着拉伸温度的升高并由脆性断裂向韧性断裂转变。     

Zn_²⁺掺杂对共沉淀法制备Ce:Gd₃Ga₃Al₂O₁₂陶瓷粉体闪烁性能的影响

本文利用化学共沉淀法制备Zn_²⁺共掺的Ce:GAGG陶瓷粉体。研究了Zn_²⁺共掺的Ce:GAGG陶瓷前驱粉体的TG/DTA和FTIR曲线；分析了不同煅烧温度对Ce:GAGG陶瓷粉体相、形貌和颗粒度分布的影响；系统研究了Zn_²⁺含量对Ce:GAGG陶瓷粉体光致发光,辐射发光,激发光谱和荧光寿命的影响。研究表明：前驱粉体在883℃的相组成为GdAlO₃相和GAGG相；前驱粉体在煅烧温度为900℃时,完全转化为GAGG相；当煅烧温度为1200℃时,GAGG颗粒尺寸控制在20nm~60nm,分布均匀；随着 Zn_²⁺含量的变化,光致发光和辐射发光强度也相应变化,特别的,当Zn_²⁺含量为0.4mol%时,光致发光和辐射发光强度达到最大值；随着Zn_²⁺掺杂含量的上升,荧光寿命出现下降的趋势。因此,Zn_²⁺含量对Ce:GAGG陶瓷粉体的辐射发光具有明显的影响,对降低荧光寿命具有积极的作用,对于提高GAGG闪烁材料的快速响应具有重要意义。     

瞬间液相(TLP)扩散连接GH4169/TC4接头微观结构及力学性能研究

为制备钛合金/镍基高温合金复合构件,拓展二者应用领域,本文以Ti/Ni复合箔片作为中间层,采用瞬间液相(TLP)扩散连接技术制备了TC4钛合金/GH4169高温合金接头,并对接头微观结构、力学性能和连接机理进行了研究和探讨。通过扫描电镜(SEM)、X射线衍射仪(XRD)、能谱分析仪(EDS)、万能实验机和显微硬度仪等对GH4169/TC4接头进行连接界面和断口形貌观察、成分表征、剪切性能和显微硬度测试,结果表明：在连接温度为960℃,保温时间30min,连接压力5MPa的工艺条件下,通过中间层与母材之间的元素扩散和化学反应,形成了“GH4169 / Ni(s,s)/ TiNi₃ / Ti₂Ni/ Ti / Ti₂Ni / Ni / TiNi/ TC4”的多层梯度结构接头,除了“Ni / TiNi+Ti₂Ni”界面处存在一定的孔洞和微裂纹,其余各连接界面连续致密,无明显缺陷。所制备GH4169/TC4接头各区域硬度起伏较大,其中,残余Ti层、Ni层区域硬度最低,有利于缓解接头内应力;GH4169侧界面区域硬度最高,主要是由于连接过程中形成的Ni(s,s)和TiNi₃硬度较高。结合接头剪切性能测试、断口形貌和物相分析,所制备GH4169/TC4接头剪切强度达124.6MPa,开裂发生在TC4附近的“Ni / TiNi+Ti₂Ni”界面区域,呈脆性断裂特征。     

碳纤维表面生长纳米碳管及其增强的炭/炭复合材料

采用化学气相沉积工艺在碳纤维表面生长了纳米碳管,将此种碳纤维作为增强材料,以中间相沥青为基体炭前驱体采用浸渍炭化工艺制备了炭/炭复合材料.观察了所得复合材料断口的微观形貌,测试了抗弯强度及热物理性能.结果表明,碳纤维表面的纳米碳管可以有效地提高纤维与基体的粘结力,复合材料的抗弯性能提高了50%,而对复合材料的导热性能影响较小.     

炭/炭复合材料热膨胀性能的研究

利用热膨胀仪测定了炭/炭复合材料从室温到1300℃的热膨胀系数,研究了热处理温度、炭纤维取向和环境温度对炭/炭复合材料热膨胀性能的影响。结果表明由于热解炭是以层状的方式围绕炭纤维生长,所以其热膨胀各向异性,垂直于纤维方向的热膨胀大于平行于纤维方向的热膨胀。随着热处理温度的升高,炭/炭复合材料中具有乱层石墨结构的晶体有序度增加,石墨化度增大,石墨片层间的范德华作用力增强,热膨胀系数减小。随着环境温度的升高热膨胀系数先增大后减小,在1200℃有最大值。     

炭/炭复合材料航空刹车副的湿态摩擦性能

对两种不同的炭/炭复合材料湿态下的摩擦磨损性能进行对比分析。结果表明:具有粗糙层热解炭的炭/炭刹车副由于其晶格结构较为完善,生长组织择优取向度和各向异性度均高于含有光滑层结构热解炭的炭/炭刹车副。前者的石墨化度及可石墨化能力均大于后者,由于前者的表面缺陷较少,所吸附的水分子较少,因而在湿态下刹车时,其刹车力矩将很快恢复到正常干态刹车时的力矩水平,对环境的适应能力大于光滑层结构的炭/炭刹车副。     

Microstructure of carbon fiber preform and distribution of pyrolytic carbon by chemical vapor infiltration

The carbon/carbon composites were made by chemical vapor infiltration(CVI) with needled felt preform. The distribution of the pyrolytic carbon in the carbon fiber preform was studied by polarized light microscope (PLM) and scanning electronic microscope(SEM). The experimental results indicate that the amount of pyrolytic carbon deposited on the surface of chopped carbon fiber is more than that on the surface of long carbon fiber. The reason is the different porosity between the layer of chopped carbon fiber and long carbon fiber. The carbon precursor gas which passes through the part of chopped carbon fibers decomposes and deposits on the surface of chopped carbon fiber. The pyrolytic carbon on the surface of long carbon fibers is produced by the carbon precursor gas diffusing from the chopped fiber and the Z-d fiber. Uniform pore distribution and porosity in preform are necessary for producing C/C composites with high properties.     

核壳结构镍碳纳米胶囊和碳纤维的制备

以脱油沥青（Deoiled Asphalt）为碳源、二茂铁为催化剂,采用化学气相沉积法（CVD）制备碳纤维（CFs）,其裂解后的残渣经真空热处理制得含镍碳纳米胶囊（CNCs）。用场发射扫描电镜（FESEM）、高分辨透射电镜（HRTEM）、X射线衍射仪（XRD）和拉曼光谱（Raman）对产物进行表征。结果表明：碳纤维纯度较高,属中空结构,直径主要分布在200～500 nm范围内;含镍碳纳米胶囊为准球形核壳结构,核为金属镍,壳为石墨化碳,大小在5～30 nm范围,晶化程度较高,结构较完善。     

Preparation and mechanical properties of carbon/carbon composites with high textured pyrolytic carbon matrix

Short carbon fiber felts with an initial porosity of 89.5% were deposited by isobaric, isothermal chemical vapor infiltration using natural gas as carbon source. The bulk density of the deposited carbon/carbon (C/C) composites was 1.89 g/cm³ after depositing for 150 h. The microstructure and mechanical properties of the C/C composites were studied by polarized light microscopy, X-ray diffraction, scanning electron microscopy and three-point bending test. The results reveal that high textured pyrolytic carbon is deposited as the matrix of the composites, whose crystalline thickness and graphitization degree highly increase after heat treatment. A distinct decrease of the flexural strength and modulus accompanied by the increase of the toughness of the C/C composites is found to be correlated with the structural changes in the composites during the heat treatment process.     

Double SiC coating on carbon/carbon composites against oxidation by a two-step method

To improve the oxidation resistance of C/C composites, a double SiC protective coating was prepared by a two-step technique. Firstly, the inner SiC layer was prepared by a pack cementation technique, and then an outer uniform and compact SiC coating was obtained by low pressure chemical vapor deposition. The microstructures and phase compositions of the coatings were characterized by SEM, EDS and XRD analyses. Oxidation behaviour of the SiC coated C/C composites was also investigated. It was found that the double SiC coating could protect C/C composites against oxidation at 1773 K in air for 178 h with a mass loss of 1.25%. The coated samples also underwent thermal shocks between 1773 K and room temperature 16 times. The mass loss of the coated C/C composites was only 2.74%. Double SiC layer structures were uniform and dense, and can suppress the generation of thermal stresses, facilitating an excellent anti-oxidation coating.     

Graphene-coated copper foam interlayer for brazing carbon/carbon composite and niobium

Problems such as poor structural integrity, inhomogeneous dispersion, and agglomeration of graphene in the brazing seam are typically encountered for graphene additives in a brazed joint interface. To resolve these problems, a plasma-enhanced chemical vapor deposition process was employed for in-situ preparation of a high-quality graphene-coated copper (Cu) foam composite interlayer prior to be applied for brazing carbon/carbon composite and niobium. The prepared graphene and the brazed joints were characterized via Raman spectroscopy, scanning electron microscopy, and high-resolution transmission electron microscopy. The results revealed that graphene was evenly distributed in the brazing seam with the help of the Cu foam, which was characterized by interconnected porosity. Simultaneously, the excellent chemical inertia of graphene inhibited the collapse of the Cu foam, based on which the thermal residual stress in the joint was effectively mitigated due to the synergistic reinforcement effect of the Cu foam (with good plastic deformation capacity) and graphene (with extremely low coefficient of linear expansion). This effect led to significant improvement in the average shear strength of the joint.     

预浸涂对航空刹车副用C/C复合材料抗氧化涂层性能的影响

采用在C/C复合材料基体表面预先浸涂浸渍剂 ,再涂刷涂层并进行涂层固化处理的工艺方法 ,可制备出抗氧化性能良好的涂层。预浸涂处理可使C/C复合材料的起始氧化温度提高近 2 0 0℃。单独预浸涂以硼酸或TEOS为主的浸渍剂后 ,试样抗氧化效果不明显 ,而预浸涂以磷酸或磷酸 硼酸混合液为主的浸渍剂效果较好 ,90 0℃ ,2h静态氧化质量损失率分别为 0 .4 0 %和 0 .33%。并对以硼酸 ,磷酸和TEOS及其混合液为主的浸渍剂的抗氧化机理进行了分析和探讨     

Equilibration of plain carbon and alloy steels with endothermic carburizing atmospheres: Part I. Activity of carbon in plain carbon steels

Experimental data on the activity of carbon in commercial plain carbon steel, AISI type 1010, common shim-stock material, at 871 °C, 927 °C, 1000 °C, and 1038 °C, equilibrated with common endothermic carburizing atmospheres, were found to be generally in agreement at relatively high carbon concentrations with previously published data on pure iron equilibrated with CO-CO₂ mixtures. However, noticeable differences were found at low carbon concentrations. The carbon contents of type 1010 steel were generally higher compared to those of previously published data regarding pure iron except at very high activities of carbon. The carbon contents of type 1010 steel foil specimens by weight gain were generally higher than or equal to those chemically analyzed; however, they corresponded with each other within 0.02 wt.% except at very low carbon potentials.