Ti-22Al-24Nb-0.5Mo粉末合金的制备及电子束焊接

采用预合金粉末热等静压工艺制备了Ti-22Al-24Nb-0.5Mo(原子分数,%)粉末合金,对Ti-22Al-24Nb-0.5Mo粉末合金环坯和板坯进行电子束焊接.采用OM,SEM,EPMA和X射线三维成像技术对焊接接头的微观组织进行表征,研究了焊后热处理对焊接接头显微硬度、拉伸性能和持久性能的影响.结果表明,热等静压温度显著影响Ti-22Al-24Nb-0.5Mo粉末合金的孔隙分布.在1030oC热等静压成型的粉末环坯经980oC,2 h,真空炉冷热处理后表现出较好的可焊性.焊接接头熔合区、热影响区和母材的化学成分均匀,虽然显微组织差异明显,但是显微硬度无明显区别.拉伸及持久性能测试试样皆断裂于熔合区.焊接接头熔合区存在大量的显微孔隙是焊接接头发生断裂的失效机制.焊后热处理可以减少焊缝处的显微孔隙数量,从而提高焊接接头塑性及高温持久寿命.     

Ti2AlNb异形粉末环件的轧制成形与性能研究

采用预合金粉末热等静压工艺制备了名义成分为Ti-22Al-24.5Nb-0.5Mo (原子分数,%)的Ti_2AlNb合金及大尺寸异形环坯(直径大于800 mm),采用热模拟压缩实验研究了Ti_2AlNb粉末合金的热变形行为,并对异形粉末环坯进行了轧制实验,分析了轧制前后的组织性能变化。结果表明,Ti_2AlNb粉末合金的热加工窗口宽且开裂倾向小,具有更均匀的化学成分和α_2相分布,但其应力抖动更加明显。优选1035～1045℃为Ti_2AlNb粉末异形环的变形温度区间,Ti2AlNb粉末异形环坯经两火轧制后,无损检测表明无任何裂纹产生。热变形促使Ti_2AlNb粉末合金的O板条细化和α_2相球化,热处理后,粉末制坯+环轧成形Ti_2AlNb合金为近两相(B2+O)组织,合金的室、高温拉伸塑性显著提高。     

焊接电流对Ti2AlNb/TC18焊接界面性能及元素扩散的影响

采用真空电子束焊接对Ti2AlNb和TC18合金进行连接,研究了不同焊接电流时焊接界面的性能及元素扩散情况。结果表明:焊接接头在室温和高温下均获得了较高的抗拉强度。采用同一电流焊接时,TC18侧热影响区的显微硬度值高于该合金基体却低于该侧焊缝区,而Ti2AlNb合金侧热影响区的显微硬度值均高于该侧焊缝区和Ti2AlNb合金基体;在28 mA的焊接电流下,焊接界面的整体显微硬度值均较高,这是因为焊接界面形成了含量较多且尺寸较小的α′马氏体和O相,对界面起到了强化作用。在不同的焊接电流下,合金元素均在焊缝和两侧母材交界处存在较大的浓度梯度,其原因是焊缝金属的快速凝固使得各合金元素没有足够的时间和能量进行充分扩散。     

异种钛合金TA15与Ti2AlNb激光焊接显微组织及力学性能研究

介绍了异种钛合金(TA15与Ti2AlNb)激光焊接工艺,分析了焊接接头的显微组织、显微硬度分布及室温、550℃高温时的拉伸性能。研究结果表明:焊缝区获得B2相、O相和α2相组成的混合组织,TA15侧热影响区主要为针状马氏体,Ti2AlNb侧热影响区组织主要为B2相和少量的α2相;TA15热影响区显微硬度值高于TA15母材,Ti2AlNb热影响区显微硬度值低于Ti2AlNb母材,在焊缝中心显微硬度值最低;室温时的拉伸断裂发生在焊缝处,断口特征为解理断裂,550℃高温时的拉伸断裂位置在TA15母材上,断口特征为韧窝。     

真空脱气对粉末冶金Ti2AlNb合金力学性能的影响

采用无坩埚感应熔炼超声气体雾化法制备了成分为Ti-22Al-24Nb-0.5Mo(原子分数，x/%)的预合金粉末，并对预合金粉末的化学成分、表面状态及流动性等进行了表征。通过包套热等静压工艺制备了粉末冶金Ti2AlNb合金，研究了真空脱气对粉末冶金Ti2AlNb合金力学性能的影响。结果表明，超声气体雾化法制备的Ti2AlNb合金粉末化学成分批次稳定性好；从粉末填充的工艺性能方面考虑，热等静压成形应选取粒度小于250 μm以下的全粒度分布预合金粉末；真空脱气处理可减少粉末冶金Ti2AlNb合金的孔隙缺陷，提升合金拉伸性能的稳定性和高温持久寿命。     

焊后热处理对异种合金摩擦焊件组织与性能的影响

用金相观察、SEM分析和拉伸试验等方法研究不同的焊后热处理制度对异种合金(Ti2AlNb/TC11)线性摩擦焊接件显微组织与力学性能的影响。结果表明:仅进行时效热处理时,随着保温时间的延长或热处理温度的提高,焊缝两侧热影响区条状α/O相析出量不断增加,焊接接头强度也相应得到提高;固溶及时效热处理后,TC11合金侧热影响区在晶界上析出大量粗条状α相,Ti2AlNb合金侧热影响区晶界主要由条状O相构成,焊接接头强度超出母材TC11合金的强度。     

板厚对Ti60钛合金电子束焊接头显微组织及力学性能的影响

研究了不同厚度Ti60钛合金板材电子束焊接接头的显微组织与力学性能。研究结果表明,不同厚度Ti60合金板材的焊接接头均由熔合区、热影响区和母材区组成,熔合区由粗大的柱状晶组成。板材厚度对柱状晶内部显微组织影响很小,不同厚度的板材熔合区柱状晶内的显微组织相似,均由细小的片层α相和少量β相组成,不同厚度的板材电子束焊接接头熔合区均具有较高的硬度和强度。700℃焊后热处理会使熔合区α相的边界处析出大量的硅化物。     

长期热暴露对304H耐热钢焊接接头组织和硬度的影响

使用Inconel 625合金焊丝对超(超)临界电站锅炉高温部件用304H奥氏体耐热钢进行焊接,对焊态焊接接头在650℃下进行5000 h的热暴露,研究了焊接接头组织和硬度随热暴露时间的演化规律。结果表明:焊后焊缝中Mo、Ti、Nb元素在枝晶间偏析,熔合线处未发生外延式生长,焊缝金属和热影响区(HAZ)的主要合金元素含量在熔合线处的浓度梯度明显。热影响区晶粒发生长大;经过3000 h热暴露后热影响区硬度达到母材的水平;随着热暴露时间的延长,母材和焊接接头均发生硬化,焊接接头微观组织无明显变化,组织稳定性较好。     

TiAl/Ti_2AlNb放电等离子扩散接头的组织性能研究

采用放电等离子扩散连接方法,对TiAl/Ti_2Al Nb合金进行了扩散连接,分析了焊接接头的显微组织和物相组成,并检测了焊接接头的拉伸强度和显微硬度。结果表明,放电等离子扩散焊可实现TiAl合金和Ti_2AlNb合金的无缺陷连接。焊接过程中Ti_2AlNb母材侧发生了O/α_2向B_2相转变,Ti_2AlNb热影响区由部分相变区、过渡区和完全相变区组成,TiAl母材侧显微形貌无明显变化,但有少量的α_2转变为α相;界面处组织由等轴的TiAl晶粒、(α+α_2)相和少Nb的B_2相构成;界面处显微硬度值最高;接头室温拉伸强度可达300 MPa。     

GH3539合金激光焊接接头组织及性能的研究

高温熔盐反应堆（MSR）利用熔融盐作为传热介质,其结构材料需要面对高温、熔盐腐蚀和中子辐照等极端环境,因此对于结构材料的性能要求极为严苛。GH3539合金作为新一代候选结构材料,在极端环境下具有显著的高温机械性能,为推动该合金的焊接应用,采用激光焊接技术对GH3539合金进行焊接,研究了合金激光焊接接头的显微组织、凝固模式及接头力学性能响应。结果表明：GH3539合金激光焊接接头具有较大的深宽比,焊接接头分为母材区、热影响区和熔合区三部分。母材区为奥氏体组织,基体中存在大量的富W碳化物以及少量的富Ti析出相。焊接接头未发现明显的焊接热影响区。熔合区中靠近熔合线的组织类型为平面晶组织,平面晶组织迅速转变为垂直于熔合线方向生长的柱状晶,且具有明显的方向性,柱状晶前沿在焊缝中线处接触,导致部分组织在焊缝中线处不规则,同时在焊缝中心处发现部分等轴晶。力学性能结果显示,熔合区硬度均值为273 HV,硬度值明显高于焊接接头的其他部分,接头中未见明显软化区域。在高温800℃时,焊接拉伸试样断裂发生在母材区域,断裂模式为明显的晶间断裂,屈服强度和最大抗拉强度分别为212.6 MPa和295.2 MPa...     

改进型镁扩散法制备高临界电流密度MgB2超导体性能研究

本文采用一种改进型镁扩散法成功制备出密度达到1.95g/cm₃的MgB₂超导块材。论文研究了不同的热处理条件对MgB₂块材的超导转变温度(T_c)和临界电流密度(J_c)性能的影响。采用最佳热处理条件制备的MgB₂超导体T_c和J_c分别达到了38.1K和0.53MA/cm₂(10K,自场)。为了改进镁扩散法MgB₂超导体中弱的高场磁通钉扎性能,本文还研究了nano-Pr₆O₁₁和C掺杂对MgB₂超导体的临界电流密度和不可逆场(H_irr)的影响。结果表明C掺杂的MgB₂超导体临界电流密度在10K,6T下达到了10₄A/cm₂,该结果比未掺杂MgB₂超导体在同样条件下性能提高了两个量级,甚至比固态反应法制备的nano-C掺杂MgB₂超导体性能更好。利用该方法制备的nano-Pr₆O₁₁掺杂的MgB₂超导体在10K,2T下也比未掺杂样品J_c提高达9.4倍。根据大量的实验结果和理论分析我们提出基于改进型镁扩散法和化学掺杂,包括纳米粒子和C掺杂,很有可能是一种制备高性能MgB₂超导体非常有效的途径。     

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。     

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.     

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.     

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.     

Preparation and characteristic of spherical Li3V2(PO4)3

Spherical Li₃V₂(PO₄)₃ was synthesized by using N₂H₄ as reducer. The products were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results show that single-phase, spherical and well-dispersed Li₃V₂(PO₄)₃ has been successfully synthesized in our experimental process. Electrochemical behaviors have been characterized by charge/discharge measurements. The initial discharge capacities of Li₃V₂(PO₄)₃ were 123 mAh g⁻¹ in the voltage range of 3.0–4.3 V and 132 mAh g⁻¹ in the voltage range of 3.0–4.8 V.     

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.     

Alloyed W–(Co,Ni,Fe)–C phases for reaction sintering of hardmetals

It has been shown that W–Co–C phases could dissolve a substantial amount of metals such as V, Cr and Ta, which are known to positively influence the microstructure of hardmetals with respect to uniform grain size distribution and fine grain size. This offers a tool to circumvent the conventional doping of hardmetals with individual carbides. In the present study we used double- and triple-alloyed κ-W₉Co₃C₄ (i.e. κ-(W,V,Cr)₉Co₃C₄ and κ-(W,V,Cr,Ta)₉Co₃C₄) and applied a variety of sintering experiments to obtain WC–Co, WC–(Ti,Ta,Nb)C–Co and WC–(Ti,Ta,Nb)(C,N)–Co hardmetals. We also prepared κ-W₉Fe₃C₄, alloyed κ-W₉Ni₃C₄, and κ-W₉(Fe/Ni)₃C₄, and used the latter for sintering.     

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.     

定-转子反应器制备LiFe1-xMxPO4 (M= Mn, Ni)粉体及其性能研究

采用具有高效传质和微观混合性能的定-转子反应器制备了LiFe_1-xMn_xPO₄ (x=0.0, 0.1, 0.2, 0.3)和LiFe_1-xNi_xPO₄ (x=0.00, 0.03, 0.05, 0.07)粉体,分别用作正极材料制成电池后,采用电池测试系统测定了电池的电化学性能随温度的变化规律。结果表明,粉体颗粒呈类球形,尺寸分布均匀,粒径范围为5~10 μm,Mn和Ni的掺杂没有改变粉体的晶体结构。以LiFe_0.8Mn_0.2PO₄和LiFe_0.95Ni_0.05PO₄两种组成的粉体性能最好,在倍率0.1 C下,所得电池的首次充放电比容量在室温和50 _oC时,分别为153.2和155.7 mAh/g,及156.4和160.4 mAh/g;100次充放电循环后电池的容量保持率分别为95.4和96.5%,及93.8和95.0%。借助具有过程强化作用的定-转子反应器制备的Mn和Ni掺杂LiFePO₄正极材料的电性能得到显著提高。原因是定-转子反应器一方面可以制备颗粒尺寸均匀的粉体,另一方面又可使掺杂的Mn和Ni在粉体颗粒中均匀分布,两者同时提高了电池中Li₊的扩散速率,进而提高了锂离子电池的电化学性能和高温电性能。