团聚粉末粒度对PS-PVD制备GYbZ热障涂层的性能影响

目的 探究不同粒度的微米级团聚粉末对等离子喷涂–物理气相沉(PS-PVD)制备GYbZ热障涂层性能的影响。方法 以微米团聚的(Gd_0.9Yb_0.1)₂Zr₂O₇(GYbZ)粉末为原料,通过PS-PVD工艺在镍基高温合金表面用3种不同粒径团聚粉末制备GYbZ热障涂层。采用扫描电子显微镜(SEM)和X射线衍射(XRD)分析GYbZ热障涂层的微观结构及相组成,采用电子万能试验机测试涂层的结合强度,采用自动水淬机对涂层的抗热震性能进行测试。结果 随着团聚粉末粒度的减小,团聚粉末的球形度会变低,且粉末的孔隙率逐渐变大,团聚粉末粒度越小,喷涂的气化率越高,涂层中未熔粒子越少,涂层羽–柱状结构越明显。D₅₀=13μm的团聚粉末在喷涂时,因粉末粒度过小,以及流动性较差,送粉过程中部分粉末未能顺利地通过喷嘴到达等离子焰流的中心,涂层的沉积率会略微降低。GYbZ团聚粉末衍射图呈现出Gd₂Zr₂O₇与Yb     

TiB2纳微米结构喂料的制备研究

采用喷雾干燥造粒技术和真空热处理工艺制备了TiB2纳微米结构喂料,用激光粒度仪、扫描电镜、X射线衍射等分析纳微米结构喂料的物理性能和物相组成.结果表明,团聚粉的颗粒形状、粒径分布、流动性等物理性能均满足热喷涂粉末的要求,真空热处理提高团聚粉的致密度;三阴极轴向送粉等离子喷涂TiB2纳微米结构喂料可制备较致密的TiB2复合涂层.     

纳米和微米ZrB_2-SiC粉末对涂层高温抗氧化性能的影响

选用纳米团聚粉末和常规微米商用ZrB_2-SiC粉末,利用超音速等离子喷涂在310S耐热不锈钢基体上制备高温抗氧化ZrB_2-SiC复合涂层。采用XRD、SEM、EDS分析涂层组织结构;拉伸法测定涂层结合强度;静态高温氧化法表征涂层抗高温氧化性能。优化了喷涂距离,研究纳米和微米ZrB_2-SiC粉末对涂层形貌、组织结构及性能的影响。结果表明:纳米团聚粉末(n-ZS)涂层表面孔隙和微裂纹较微米商用粉末(m-ZS)涂层大幅减少,涂层更为致密;n-ZS涂层结合强度达到44.6 MPa,较m-ZS涂层提升了约67%;经过1 100℃、50 h的高温氧化试验,n-ZS涂层增重明显低于m-ZS涂层,氧化倾向低,具有更好的高温抗氧化能力。     

以蔗糖为前驱体火焰喷涂原位TiC增强Ni基复合涂层的制备

以蔗糖为碳源,采用前驱体热分解技术制备Ni-Ti-C系反应热喷涂混合粉末,通过氧乙炔火焰喷涂技术合成并同时沉积原位TiC颗粒增强的Ni基合金复合涂层.利用XRD和SEM研究混合粉末和涂层的相成分和组织结构,分析TiC/Ni复合涂层的硬度和耐磨性.结果表明:反应火焰喷涂TiC/Ni复合涂层主要由TiC和Ni基体组成,并含少量的Ni3Ti和Ti3O5;涂层由复合强化片层相瓦叠加而成,复合强化片层中TiC颗粒均匀分布于Ni基体中,TiC颗粒呈球形,粒度达到亚微米级:涂层具有较高的硬度和耐磨性,复合强化片层显微硬度为FIV0.21433,涂层的耐磨性能远优于基板材料45号钢和对比涂层Ni60的耐磨性.     

Al2O3弥散强化316L不锈钢粉末的高速火焰喷涂

采用高能球磨工艺制备了Al2O3弥散强化316L不锈钢喷涂粉末,并进行高速火焰喷涂(HVOF)试验.研究了弥散强化粉末及其喷涂层的微观组织结构和硬度.采用销-盘磨损试验机测试了涂层的耐磨性能.结果表明,球磨加工后,Al2O3颗粒尺寸大多小于1 μm,由微米级、亚微米级及纳米级粒子组成并均匀分布在316L不锈钢基体粉末中.随着球磨时间的增加,粉末的显微硬度提高.喷涂后球磨粉末的微观组织结构基本不变,喷涂层的硬度比对应球磨粉末硬度低,其耐磨性明显优于单纯不锈钢粉末涂层.     

等离子喷涂纳米与微米YSZ热障涂层的孔隙结构比较

采用定量分析技术,分析了相同等离子喷涂工艺制备的微米及纳米YSZ热障涂层的孔隙结构,结果表明:纳米涂层的孔隙率低于微米涂层;两涂层的孔隙大小和形状分布规律相似,纳米涂层以直径在1～10μm之间的孔隙含量最多,而微米涂层则以直径大于10μm的孔隙比例最大;纳米YSZ涂层中等轴孔隙含量明显大于微米YSZ涂层.这些结果说明,粉末尺寸对等离子喷涂热障涂层的孔隙结构有着明显的影响.     

YSZ热障涂层表面MAX相Ti_2AlC防护层的料浆法制备

MAX相Ti_2AlC是一种很有潜力的热障涂层抗环境沉积物(CMAS)腐蚀防护层材料。采用料浆法在YSZ(Y_2O_3部分稳定ZrO_2)热障涂层表面制备Ti_2AlC防护层,研究粘结剂种类、粘结剂含量、涂覆方式、保温时间和烧结温度对涂层结合质量的影响。结果表明,与硅酸钠相比,乙基纤维素作为粘结剂更合适,当粘结剂含量为7%左右时,Ti_2AlC涂层表面完整,无明显缺陷;与刷涂方法相比,采用浸渍的涂覆方式得到的涂层致密性良好,界面处无明显缝隙;最佳的烧结温度和保温时间为1250℃,10 h。最终采用优化出的参数在YSZ热障涂层表面制备出了厚度～100μm的Ti_2AlC防护层,其与YSZ涂层之间的界面完整,结合良好,为MAX相Ti_2AlC用于CMAS防护层提供了指导。     

冷喷涂铁基非晶复合涂层的制备及摩擦性能研究

非晶合金拥有独特的短程有序、长程无序原子排列结构,具有高强度、高硬度及优异的耐腐蚀和耐磨损等性能,在防护涂层领域具有很强的应用潜力。以低温固态沉积为特点的冷喷涂层制备技术,可有效避免喷涂过程中非晶合金材料的氧化和晶化问题,但是冷喷涂技术严重依赖于粉末的塑性变形能力。为提高非晶合金颗粒在高速撞击下的沉积变形性能,本论文创新采用液氮-常温循环深冷处理工艺方法对Fe_87.4Cr_2.5Si_6.8B_2.4C_0.9非晶合金粉末进行预处理,通过调控冷喷涂工艺参数,成功在6061铝合金基体表面制备非晶涂层。同时研究了深冷处理工艺对非晶粉末沉积行为以及涂层微观组织的影响机理,通过摩擦磨损试验研究非晶合金涂层的摩擦磨损性能。结果表明：使用原始非晶粉末制备得到的涂层厚度仅为6μm,且非晶颗粒在基体表面不连续分布,只有粒径较小的非晶颗粒可发生有效的塑性变形,但是粉末沉积过程中晶化率较低;使用经过深冷预处理的非晶粉末制备的涂层平均厚度为67μm,且涂层内非晶合金颗粒分布均匀,粒径较大的非晶颗粒也可发生有效塑性变形,但是粉末沉积过程中晶化率较高。在摩擦磨损过程中6061铝合金基体的主要磨损机制为粘着磨损与疲劳磨损,非晶涂层的主要磨损机制为磨粒磨损,且使用原始非晶粉末和循环深冷处理粉末制备得到的非晶涂层的质量磨损量较低,分别为6061铝合金基体质量磨损量的15.7%、11.8%。     

亚微米WC添加对超音速火焰喷涂WC–Co涂层磨损性能影响

采用湿法球磨将亚微米WC（~300 nm）和WC–12Co粉末混合均匀并使亚微米WC均匀粘附于WC–12Co粉末的表面,采用超音速火焰喷涂方法（HVOF）在304不锈钢基体表面制备WC和WC–12Co的WC–Co复合涂层,研究亚微米WC的添加对涂层相组成、显微硬度、耐磨性能和表面形貌的影响。利用X射线衍射分析涂层相组成,压痕法测试涂层的显微硬度,通过往复式摩擦磨损实验测试磨损性能,扫描电子显微镜（SEM）对涂层磨损表面和断面进行微观形貌观察,并分析涂层的磨损过程和机制。结果表明,添加质量分数5%的亚微米WC颗粒显著提高了涂层的显微硬度（16.3%）;增强了涂层的耐磨性,磨损率从6.09×10-7 mm3/Nm减小到5.15×10-7 mm3/Nm（减小13.8%）;亚微米WC颗粒喷涂后在涂层中保持了WC相,并主要存在于WC–Co扁平粒子界面和孔隙。基于涂层中扁平粒子的结合特性与磨损失效特征,建立强化模型,分析亚微米WC颗粒对涂层扁平粒子界面的强化机制。     

喷涂用MoSi2粉末的制备及其在等离子弧中的熔化特性

采用喷雾干燥和真空烧结技术制备MoSi2团聚颗粒,以MoSi2团聚粉末为原料,通过大气等离子喷涂法制备二硅化钼涂层,借助XRD、扫描电镜及能谱对团聚体粉末在等离子焰流中的熔化特性和涂层的组织结构进行研究.结果表明:团聚粉末在1200℃真空热处理1 h后,粉末的流动性和松装密度分别提高55.6%和42.0%,适合等离子喷涂用.MoSi2颗粒经过高温等离子焰流后,粉末熔化充分,大多数团聚体粉末发生烧结过程,颗粒的平均粒度减小,形成较致密的球形颗粒.在喷涂过程中,部分四方相MoSi2(t)转变为六方相MoSi2(h)或氧化形成了少量的Mo<,5>Si3相,涂层中的富钼相呈"网状"组织结构.     

废旧锂离子电池中Li, Fe和V的回收及xLiFePO4-yLi3V2(PO4)3的制备

由于LiFePO_4和Li_3V_2(PO_4)_3材料的特征相近,制备方法类似,提供了一种从废旧LiFePO_4和Li_3V_2(PO_4)_3混合电池中回收Li、Fe和V,再制备xLiFePO_4-yLi_3V_2(PO_4)_3的方法。在空气气氛中600℃热处理1h后,去除粘结剂PVDF使活性物质与集流体分离。调节Li、Fe、V和P摩尔比,球磨、锻烧,配制不同比例的xLiFePO_4-yLi_3V_2(PO_4)_3(x:y=5:1,7:1,9:1)复合电极材料。表征了其形貌、结构和电化学性能,结果表明,回收制备的复合材料将同时具备LiFePO_4和Li_3V_2(PO_4)_3两种材料的电化学性能,能显著改善LiFePO_4的倍率性能。     

LaSrCuO4粉体微结构对Ag/LSCO电接触材料性能的影响

以硝酸镧、硝酸铜、硝酸锶等为原料,分别采用固相法、溶胶-凝胶法和共沉淀法合成了不规则颗粒状(LSCO_g)、介孔状(LSCOm)和片层状(LSCOl)的LaSrCuO_4(LSCO)粉体。采用高能球磨并结合初压-初烧-热压工艺制备出Ag/LSCO电接触材料。利用X射线衍射(XRD)、扫描电镜(SEM)、金属电导率仪、维氏硬度计和电寿命试验机等对粉体形貌及电接触材料的物理和电学性能进行了表征。结果表明:与Ag/LSCO_(m)、Ag/LSCO_l材料相比,Ag/LSCO_(g)电接触材料表现出更加优异的物理性能,其电阻率为2.37μΩ·cm,硬度为800MPa,密度为9.32g/cm~3;但电学性能差异较小,其在AC220V12A开断状态下的燃弧能量为400 mJ、燃弧时间为23 ms,关合状态下的燃弧能量为1500 mJ,燃弧时间为68ms。Ag/LSCO电接触材料的主要失效形式是液滴喷溅,微裂纹和孔洞。     

Effects of Mo and Al Additions on the Sulfidation Behavior of 310 Stainless Steel

The high-temperature sulfidation behavior of 310stainless steel (310SS) with Mo and Al additions (up to10 at.%) was studied over the temperature range700-900°C in pure-sulfur vapor over the range of 10^-3 to 10^-1 atm. Thecorrosion kinetics followed the parabolic rate law inall cases and the sulfidation rates increased withincreasing temperature and sulfur pressure. Thesulfidation rates decreased with increasing Mo and Al contents and it wasfound that the addition of 10 at.% Mo resulted in themost pronounced reduction among the alloys studied. Thescales formed on 310SS with Mo additions were complex, consisting of an outer layer of ironsulfide (with dissolved Cr), (Fe,Ni)₉S₈, andCr₂S₃/Cr₃S₄(with dissolved Fe), and an inner heterophasic layer ofFe_1-xS,Cr₂S₃/Cr₃S₄,NiCr₂S₄,Fe_1.25Mo₆S_7.7, FeMo₂S₄, andMoS₂. The scales formed on 310SS with Mo andAl additions had a similar mixture as above, except thatAl_0.55Mo₂S₄ was alsoobserved in the inner layer. The formation ofMoS₂ andAl_0.55Mo₂S₄ partly blocked the transport of cations throughthe inner scale, resulting in the reduction of thesulfidation rates compared to 310SS.     

Synthesis of lanthanum carbonate nanoparticles via sonochemical method for preparation of lanthanum hydroxide and lanthanum oxide nanoparticles

Lanthanum carbonate nanoparticles were synthesized from the reaction of lanthanum acetate and Na₂CO₃ under sonication via sonochemical method. Lanthanum hydroxide nanoparticles were prepared by facial hydrothermal processing from the resulted product at 110 °C for 24 h. The role of surfactant, calcination temperature and sonication time were investigated on the morphology and particle size of the products. Products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectrum (XPS), and Fourier transform infrared (FT-IR) spectra. La₂O₃ nanoparticles were obtained by calcinations of the nanoparticles of lanthanum carbonate at 600 °C.     

Effects of sulfur pressure on the sulfidation behavior of 310 stainless steel

High-temperature sulfidation behavior of 310 stainless steel was studied over the temperature range of 700–900°C above a pure sulfur pool with the sulfurvapor range of 10^–4–10^–1 atm. The corrosion kinetics followed the parabolic rate law in all cases. The corrosion rates increased with increasing temperature and sulfur pressure. The scales formed on 310 stainless steel were complex and multilayered. The outer scale consisted of iron sulfide (with dissolved Cr), (Fe, Ni)₉S₈ and chromium sulfides (Cr₂S₃ and Cr₃S₄ with dissolved Fe), while the inner layer was a heterophasic mixture of Cr₂S₃, Cr₃S₄, NiCr₂S₄, and Fe₁–_xS. Platinum markers were found to be located at the interface between the inner and outer scales, suggesting that the outer scale grew by the outward transport of cations (Fe, Ni, and Cr), and the inner scale grew by the inward transport of sulfur. The formation of Cr₂S₃, Cr₃S₄, and NiCr₂S₄ partly blocked the transport of iron through the inner scale, resulting in a reduction of the corrosion rates as compared with the results in the literature.     

The high-temperature corrosion behavior of Co-Nb alloys in mixed-gas atmospheres

The corrosion of Co-Nb alloys containing up to 30 wt.% Nb in H₂-H₂S-H₂O gas mixtures was studied over the temperature range of 600–800°C. The gas composition falls in the stability region of cobalt sulfide and Nb₂O₅ in the phase diagrams of the Co-O-S and Nb-O-S systems at all temperatures studied. Duplex scales, consisting of an outer layer of cobalt sulfide and a complex, heterophasic inner layer, were formed at all temperatures studied. In addition to cobalt sulfide and CoNb₃S₆, a small amount of NbO₂ was found in the inner layer. The reason for the formation of NbO₂ over that of Nb₂O₅ in the scale is that the outer sulfide scale lowers the oxygen activity within the scale into the NbO₂-stability region. Two-stage kinetics were observed for all alloys, including an initial irregular stage usually followed by a steady-state parabolic stage. The steady-state parabolic rate constants decreased with increasing amounts of Nb, except for Co-20Nb corroded at 700°C. Nearly identical kinetics were observed for Co-20Nb corroded at 600°C and 700°C. The presence of NbO₂ particles leads only to a limited decrease of the available cross-section area for the outward-diffusing metal ions. The activation energies for all alloys are similar and are in agreement with those obtained in a study of the sulfidation of the same alloys. The primary corrosion mechanism involves an outward Co transport.     

Effects of K2O-Li2O doping on surface and catalytic properties of Fe2O3/Cr2O3 system

The effects of K₂O and Li₂O-doping (0.5, 0.75 and 1.5 mol%) of Fe₂O₃/Cr₂O₃ system on its surface and the catalytic properties were investigated. Pure and differently doped solids were calcined in air at 400-600 °C. The formula of the un-doped calcined solid was 0.85Fe₂O₃:0.15Cr₂O₃. The techniques employed were TGA, DTA, XRD, N₂ adsorption at −196 °C and catalytic oxidation of CO oxidation by O₂ at 200-300 °C. The results revealed that DTA curves of pure mixed solids consisted of one endothermic peak and two exothermic peaks. Pure and doped mixed solids calcined at 400 °C are amorphous in nature and turned to α-Fe₂O₃ upon heating at 500 and 600 °C. K₂O and Li₂O doping conducted at 500 or 600 °C modified the degree of crystallinity and crystallite size of all phases present which consisted of a mixture of nanocrystalline α- and γ-Fe₂O₃ together with K₂FeO₄ and LiFe₅O₈ phases. However, the heavily Li₂O-doped sample consisted only of LiFe₅O₈ phase. The specific surface area of the system investigated decreased to an extent proportional to the amount of K₂O and Li₂O added. On the other hand, the catalytic activity was found to increase by increasing the amount of K₂O and Li₂O added. The maximum increase in the catalytic activity, expressed as the reaction rate constant (k) measured at 200 °C, attained 30.8% and 26.5% for K₂O and Li₂O doping, respectively. The doping process did not modify the activation energy of the catalyzed reaction but rather increased the concentration of the active sites without changing their energetic nature.     

Effect of Y2O3 additions on the plasticity of sintered Cr2O3

We have carried our constant strain-rate compression tests on polycrystalline Cr₂O₃ and Cr₂O₃ doped with 0.09 wt. % Y₂O₃ to establish whether there exists an effect of Y₂O₃ on the plasticity of Cr₂O₃. This study is motivated by previous work on the oxidation of alloys containing reactive-element additions. In that work, it has been observed that the addition of oxygen-active elements, such as Y to alloys that form Cr₂O₃ or Al₂O₃ oxide layers upon exposure at high temperature, strongly enhances the adhesion of the oxide layer to the base alloy as compared with alloys without reactive-element additions. We have found that at 1200°C (1) chromia exhibits limited plasticity at high temperatures, and (2) the presence of Y in the oxides does not enhance plasticity compared with addition-free oxides.     

The high-temperature corrosion behavior of Nb-Al alloys in a H2/H2S/H2O gas mixture

The corrosion behavior of pure Nb and three Nb Al alloys containing 12.5, 25, and 75 at.% Al was studied over the temperature range of 800–1000°C in a H₂/H₂S/H₂O gas mixture. Except for the Nb-12.5Al alloy consisting of a two phase structure of -Nb and Nb₃Al, other alloys studied were single phase. The corrosion kinetics followed the parabolic rate law in all cases, regardless of temperature and alloy composition. The parabolic rate constants increased with increasing temperature, but fluctuated with increasing Al content. The Nb-75Al alloy exhibited the best corrosion resistance among all alloys studied, whose corrosion rates are 1.6–2.2 orders of magnitude lower than those of pure-Nb (depending on temperature). An exclusive NbO₂ layer was formed on pure Nb, while heterophasic scales were observed on Nb-Al alloys whose compositions and amounts strongly depended on Al content and temperature. The scales formed on Nb-12.5Al consisted of mostly NbO₂ and minor amounts of Nb₂O₅, NbS2, and -Al₂O₃, while the scales formed on Nb-25Al consisted of mostly Nb₂O₅ and some -Al₂O₃. The scales formed on Nb-75Al consisted of mostly -Al₂O₃ and Nb₃S₄ atT 900°C, and mostly -Al₂O₃ , Nb₃S₄ and some AlNbO₄ at 1000°C. The formation of -Al₂O₃ and Nb₃S₄ resulted in a significant reduction of the corrosion rates.     

Improved capacity and rate capability of Ru-doped and carbon-coated Li4Ti5O12 anode material

Pure Li₄Ti₅O₁₂, modified Li₄Ti₅O₁₂/C, Li₄Ru_0.01Ti_4.99O₁₂ and Li₄Ru_0.01Ti_4.99O₁₂/C were successfully prepared by a modified solid-state method and its electrochemical properties were investigated. From the XRD patterns, the added sugar or doped Ru did not affect the spinel structure. The results of electrochemical properties revealed that Li₄Ru_0.01Ti_4.99O₁₂/C showed 120 and 110 mAh/g at 5 and 10 C rate after 100 charge/discharge cycles. Li₄Ru_0.01Ti_4.99O₁₂/C exhibited the best rate capability and the highest capacity at 5 and 10 C charge/discharge rate owing to the increase of electronic conductivity and the reduction of interface resistance between particles of Li₄Ti₅O₁₂.It is expected that the Li₄Ru_0.01Ti_4.99O₁₂/C will be a promising anode material to be used in high-rate lithium ion battery.