改性酚醛环氧树脂F-51自修复微胶囊的制备

目的研制一种耐温性好、适用于防腐涂料的自修复微胶囊。方法通过活性稀释剂TMPEG改性具有较好耐温性的酚醛环氧树脂F-51,以原位聚合法,采用非离子表面活性剂复合乳化的方法制备脲醛树脂自修复微胶囊。运用光学显微镜(OM)和扫描电子显微镜(SEM)观察微胶囊的分布状况及轮廓形貌,激光粒度分析仪测定微胶囊的粒径值,引入Gauss拟合研究粒径分布。主要讨论乳化剂的选择、用量、原料比、搅拌转速等条件对微胶囊性能的影响,研究最佳合成工艺;利用OM和SEM观察单个微胶囊的形态,结合光衍射原理判断微胶囊芯壁构成;红外光谱仪(FT-IR)探讨其官能团组成,差示扫描量热仪(DSC)测定微胶囊芯材的反应活性,测试室温条件下微胶囊的贮存效果,并由同步热分析仪(TA)测量微胶囊的热失重情况。结果采用OP-10/JFC复合乳化剂,研制出聚脲甲醛包覆酚醛环氧树脂F-51自修复微胶囊,当用量为芯材质量分数的8.0%,原料比为0.8:1,搅拌速率为1600 r/min时,产率最高达82%,粒径分布相对集中,粒径平均值为107μm。OM中光衍射现象明显,在FT-IR特征曲线出现相应特征吸收峰,微胶囊研磨后可固化反应,室温下贮存100 d,失重率不到3.0%,且在250℃范围内可以保持完整囊-芯结构。结论成功制备了包覆修复剂的微胶囊,微胶囊具备反应活性,贮存稳定性及热稳定性良好,研究成果可为自修复防腐涂料的发展提供参考。     

含环氧树脂微胶囊自修复涂层的制备及其性能

目的制备含环氧树脂微胶囊的二元自修复涂层,并对其力学性能和自修复性能进行研究。方法将自制环氧树脂E-51/三聚氰胺-脲醛树脂微胶囊和潜伏型固化剂(2-甲基咪唑)按一定比例添加到环氧树脂基体中,制备二元自修复环氧树脂涂层。利用漆膜弹性试验机、漆膜冲击试验机和万能拉伸试验机对涂层的弯曲性能、耐冲击性能和拉伸性能进行测试。利用扫描电子显微镜(SEM)、光学显微镜(OM)对涂层的自修复性能进行考察。采用EIS对涂层的电化学性能进行测试。结果成功制备了含环氧树脂微胶囊二元自修复涂层,当涂层中微胶囊的质量分数为3%时,涂层的冲击强度和拉伸强度分别提高了10.6%和14.6%。当涂层中2-甲基咪唑和微胶囊质量分数分别为6%和5%时,涂层的自修复性能较佳。当微胶囊质量分数为9%时,涂层的电化学阻抗值可达1.2×105?。结论微胶囊的加入可有效提高涂层的冲击强度和拉伸强度。随着涂层中潜伏型固化剂含量的增大,涂层的自修复性能增强。当潜伏型固化剂含量达到一定值时,涂层的自修复性能随着微胶囊含量的增大而增强。随着微胶囊含量的增加,涂层的电化学阻抗值增大。     

Ni2Cr(BO3)O2涂层的制备及其红外发射性能

通过喷雾造粒和高温焙烧制备Ni_2Cr(BO_3)O_2粉末后利用等离子喷涂得到一种高红外发射涂层,并研究了该种涂层的红外发射性能。SEM观察涂层的表面、断面形貌,发现涂层与基体结合紧密、无脱落;XRD对焙烧后的粉末物相组成进行了表征,主要以Ni_2Cr(BO_3)O_2为主。对涂层红外波段发射率的测试表明,在0.76~2.5μm波段的发射率为0.896、2.5~14μm波段发射率为0.925,具有优异的红外发射性能。Ni_2Cr(BO_3)O_2晶胞内的畸变、非对称性以及电子转移跃迁是导致Ni_2Cr(BO_3)O_2这种材料具有高红外发射率的主要原因。Ni_2Cr(BO_3)O_2涂层能够经受37次"900℃~水冷"热震循环。该种涂层由于其高红外发射性能、优异的耐热震性能和热稳定性能而具有较高的实用价值。     

多壁异氰酸酯微胶囊的制备及其在自修复防腐涂层中的应用

目的制备多壁异氰酸酯微胶囊及该微胶囊包埋的聚氨酯(PU)自修复防腐涂层。方法在Pickering乳液中,通过界面聚合、原位聚合、自组装,一步生成由内至外依次为聚脲内膜、酚醛壳、聚甲基丙烯酸缩水甘油酯(PGMA)粒子层的多层囊壁包裹异佛尔酮二异氰酸酯(IPDI)芯材的IPDI微胶囊。通过索式提取实验获得了微胶囊的芯材含量,通过SEM、OM对微胶囊形貌及壳层结构进行观测,通过FTIR、DSC测试研究微胶囊的成分及芯材反应活性,通过EIS、加速腐蚀实验研究微胶囊包埋的PU涂层的自修复防腐性能。结果随着芯壳比的增加,微胶囊的芯材含量增大,当芯壳比为2.5∶1时,芯材含量最大,达70.22%。当芯壳比为1.5∶1时,微胶囊的球形度最好,平均粒径最小,为86.12μm,且分布均一。IPDI微胶囊具有一层聚脲内膜、酚醛壳及PGMA粒子层,IPDI芯材被成功包覆,且保持有效性。IPDI微胶囊的初始分解温度为235.8℃,对芯材起到较好的保护作用。包埋IPDI微胶囊的自修复涂层,划痕修复后的阻抗模量恢复至划痕前初始状态阻抗模量的同量级水平。盐水浸泡192h后,自修复涂层划痕处未见腐蚀产生。结论制备的IPDI微胶囊的芯材含量较高,球形度较好,分布均一。该一步法工艺有助于对活泼性芯材达到高效包覆,多囊壁结构有助于提高微胶囊的热稳定性和有效性。自修复涂层由于划痕处生成了固化膜,从而抑制了腐蚀的产生,具有较好的自修复防腐性能。     

六亚甲基二异氰酸酯微胶囊的制备及其在自修复涂料中的应用

目的 制备一种基于小尺寸六亚甲基二异氰酸酯(HDI)微胶囊的自修复防腐涂料,能够提高涂层的防腐性能并实现涂层划痕缺陷的在线修复。方法 通过调整界面聚合法合成HDI微胶囊过程中的乳化剂添加量、搅拌速率和体系pH值,降低微胶囊的平均粒径,并利用囊芯染色试验、红外光谱(FTIR)、热重试验(TG)对微胶囊的结构和热稳定性进行表征。以物理共混的方式将微胶囊掺入到环氧树脂基质中制备自修复防腐涂料,使用万能拉伸机、拉拔测试仪、电化学阻抗谱(EIS)研究微胶囊对涂层基础力学性能和耐腐蚀性能的影响。结合丝束电极(WBE)测试与划痕涂层浸泡腐蚀试验分析复合涂层的内在自修复机理。结果 确定了微胶囊制备过程的最佳乳化剂添加量为3%、搅拌速率为600 r/min、体系pH值为3.5,此时的微胶囊呈规则的球状结构,表面致密且具有一定的粗糙度,平均粒径尺寸降低为59μm,成型率达82%。FTIR和囊芯染色试验证明微胶囊由脲醛树脂囊壁和HDI囊芯组成,TG分析显示微胶囊初始分解温度为260℃。随着微胶囊含量的提高,自修复涂层的拉伸断裂强度和附着力有所下降。EIS测试结果表明,含0%、1%、5%和10%微胶囊的自修复...     

纳米Al_2O_3对等离子喷涂ZrC-ZrSi_2复合涂层结构与性能的影响

大气等离子喷涂ZrC-ZrSi_2陶瓷涂层的孔隙率高,提高等离子喷涂ZrC-ZrSi_2陶瓷涂层的致密度成为亟待解决的问题。在TC4钛合金表面采用大气等离子喷涂ZrC-ZrSi_2复合粉和ZrC-ZrSi_2-Al_2O_3复合粉分别制备两种复合涂层。研究纳米Al_2O_3对等离子喷涂ZrC-ZrSi_2复合涂层组织结构与性能的影响。结果表明,添加了Al_2O_3的ZrC-ZrSi_2复合涂层的组织结构更为致密,相较于ZrC-ZrSi_2复合涂层具有更优异的力学性能。熔点相对较低的Al_2O_3能够在喷涂焰流中先熔化,熔融态的Al_2O_3能够填充在ZrC-ZrSi_2复合涂层的孔洞处,提高复合涂层的致密度,改善涂层的力学性能。研究成果可为提高大气等离子喷涂制备含高熔点组分复合涂层的致密度提供指导。     

CaO-Bi2O3-MoO3-xNb2O5复合掺杂对高磁导率Mn-Zn铁氧体的微观结构和电磁性能的影响

采用高温固相反应制备了CaO-Bi_2O_3-MoO_3-XNb_2O_5(X=0.000%~0.075%,质量分数,步长:0.015%)复合掺杂的高磁导率Mn-Zn铁氧体材料,利用XRD、SEM、四探针电阻测试仪、阻抗分析仪、和软磁测试仪等分析测试手段对材料结构和性能进行表征,研究了复合掺杂剂中Nb_2O_5掺杂量对高磁导率Mn-Zn铁氧体材料的结构和电磁性能的影响。结果表明:当Nb_2O_5少量掺杂时,Nb_2O_5可以改善材料的微观结构,提高其密度、频率稳定性和品质因数,提高其电阻率,降低其体积功耗;当Nb_2O_5过量掺杂时,Nb_2O_5将恶化材料的微观结构,导致材料的电磁性能变差。当Nb2O5掺杂量为0.030%时材料的综合电磁性能最佳。     

Al_2O_3/MoS_2复合涂层的制备及摩擦磨损性能

以大气等离子喷涂工艺制备的Al_2O_3陶瓷涂层为模板,利用陶瓷涂层中存在的孔隙和微裂纹,采用水热反应在其内部原位合成具有润滑特性的MoS_2,制备出Al_2O_3/MoS_2的复合涂层。结果表明,通过水热反应在陶瓷涂层原有的微观缺陷中成功合成了MoS_2,合成的MoS_2固体粉末呈类球形状,并且这球状的粉末是由纳米片层状的MoS_2搭建组成的。摩擦试验结果表明,与纯Al_2O_3涂层相比,复合涂层中由于MoS_2润滑膜的形成,其摩擦因数和磨损率都显著降低,且载荷越大,复合涂层的摩擦性能越好。     

仿生自修复环氧树脂涂层制备及性能

采用一步原位聚合法制备了脲醛树脂包覆E-51/711微胶囊,观察微胶囊形貌呈球形,为单核结构,表面致密,粒径大小分布为25～375μm。模仿生物组织损伤自愈合原理,将微胶囊引入环氧树脂涂层结构中,设计了潜伏型微胶囊自修复环氧涂层。对不同微胶囊质量分数(5%,10%,15%,20%)的环氧自修复涂层的力学性能进行测试分析,结果表明:随着微胶囊的添加量增大,涂层的冲击强度、附着力级别和巴尔霍兹硬度不断降低,而适量添加微胶囊可提高涂层的附着力。对微胶囊环氧树脂涂料块体试样进行拉伸断裂测试试验,并对涂层进行预置划痕修复试验,结果表明:少量添加微胶囊对涂层起到了一定增韧作用,含微胶囊自修复体系的涂层在受到损伤时能够释放修复剂,填充修复损伤部位。     

石蜡/脲醛树脂相变微胶囊的制备及其热性能研究

采用原位聚合法制备了以脲醛树脂为壁材,包覆石蜡的相变微胶囊.利用扫描电子显微镜(SEM)和差示扫描量热仪(DSC)对微胶囊试样的表面形貌和热物理性能进行了研究,并讨论了芯壁比对微胶囊的形貌和热性能的影响.实验结果表明:当芯壁比为2∶1时,微胶囊的相变温度和相变潜热接近芯材石蜡.     

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.     

Sinterability and dielectric properties of Ba0.55Sr0.4Ca0.05TiO3-CaTiSiO5-Mg2TiO4 composite ceramics

The composite ceramics of Ba_0.55Sr_0.4Ca_0.05TiO₃-CaTiSiO₅-Mg₂TiO₄ (BSCT-CTS-MT) were prepared by the conventional solid-state route. The sintering performance, phase structures, morphologies, and dielectric properties of the composite ceramics were investigated. The BSCT-CTS-MT ceramics were sintered at 1100 °C and possessed dense microstructure. The dielectric constant was tailored from 1196 to 141 as the amount of Mg₂TiO₄ increased from 0 to 50 wt%. The dielectric constant and dielectric loss of 40 wt% Ba_0.55Sr_0.4Ca_0.05TiO₃-10 wt% CaTiSiO₅-50 wt% Mg₂TiO₄ was 141 and 0.0020, respectively, and the tunability was 8.64% under a DC electric field of 8.0 kV/cm. The Curie peaks were broadened and depressed after the addition of CaTiSiO₅. The optimistic dielectric properties made it a promising candidate for the application of tunable capacitors and phase shifters.     

Low temperature sintering and microwave dielectric properties of (Mg0.7Zn0.3)0.95Co0.05TiO3 ceramics with BaCu(B2O5) additions

The effects of BaCu(B₂O₅) additives on the sintering temperature and microwave dielectric properties of (Mg_0.7Zn_0.3)_0.95Co_0.05TiO₃ ceramics were investigated. The (Mg_0.7Zn_0.3)_0.95Co_0.05TiO₃ ceramics were not able to be sintered below 1000 °C. However, when BaCu(B₂O₅) were added, they were sintered below 1000 °C and had the good microwave dielectric properties. It was suggested that a liquid phase with the composition of BaCu(B₂O₅) was formed during the sintering and assisted the densification of the (Mg_0.7Zn_0.3)_0.95Co_0.05TiO₃ ceramics at low temperature. BaCu(B₂O₅) powders were produced and used to reduce the sintering temperature of the (Mg_0.7Zn_0.3)_0.95Co_0.05TiO₃ ceramics. Good microwave dielectric properties of Q × f = 35,000 GHz, ?_r = 18.5.0 and τ_f = −51 ppm/°C were obtained for the (Mg_0.7Zn_0.3)_0.95Co_0.05TiO₃ ceramics containing 7 wt.% mol% BaCu(B₂O₅) sintered at 950 °C for 4 h.     

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.     

Sol-gel synthesis of Bi3.25La0.75Ti3O12 nanotubes

Ferroelectric Bi_3.25La_0.75Ti₃O₁₂ (BLT) nanotubes were synthesized by sol-gel technique using nanochannel porous anodic aluminum oxide (AAO) templates, and were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM). BLT nanotubes with diameter of around 240 nm and the wall thickness of about 25 nm exhibited a single orthorhombic perovskite structure and highly preferential crystal growth along the [1 1 7] orientation, which have smooth wall morphologies and well-defined diameters corresponding to the diameter of the applied template. The formation mechanism of BLT nanotubes was discussed.     

FRICTION WELDING OF Zr55Al10Ni5Cu30 BULK METALLIC GLASS

采用摩擦焊对Zr₅₅Al₁₀Ni₅Cu₃₀块体金属玻璃进行了焊接, 当焊机主轴转速为4.0×10³---5.0×10³ r/min, 摩擦压力为80---100 MPa, 摩擦时间为0.2---0.4 s, 顶锻压力和保压时间分别为200 MPa和2 s时, 能够成功实施Zr₅₅Al₁₀Ni₅Cu₃₀金属玻璃的焊接. 用SEM, XRD和TEM观察分析未检测到晶化相, 焊缝处金属仍保持非晶状态. 金属玻璃的塑性在玻璃转变点T_g附近随温度变化很大, 在T_g以上具有良好的塑性变形能力, 这是实施摩擦焊焊接的重要基础.     

固相-水热法制备LiFePO4-Li3V2（PO4）3复合材料及其电化学性能（英文）

分别采用固相-水热法和球磨法制备磷酸亚铁锂-磷酸钒锂复合正极材料(LiFePO4-Li3V2(PO4)3)。电化学性能测试表明,LiFePO4-Li3V2(PO4)3复合正极材料的电化学性能远远高于 LiFePO4和 Li3V2(PO4)3单独作为正极材料的性能,并且以固相-水热法制备的复合材料性能优于以球磨法制得的复合材料。研究发现 LiFePO4-Li3V2(PO4)3复合材料有 4 个氧化还原峰,相当于 LiFePO4 和 Li3V2(PO4)3 氧化还原峰的叠加。采用固相-水热法制备的LiFePO4-Li3V2(PO4)3 复合材料形貌较为规则,且有新相物质产生,这是导致其电化学性能较好的原因。     

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。     

二维ZnO/ Bi3.9Zn0.4V1.7O10.5纳米异质结构的制备及其可见光催化活性

表面建造是提高半导体光催化活性的一种有效方法。本文利用Zn5(CO3)2(OH)6纳米片为基底沉积了BiVO4再通过煅烧成功制备了二维ZnO/Bi3.9Zn0.4V1.7O10.5复合纳米片。通过X射线衍射,透射电镜和元素映像技术表征了所制样品。结果显示随着锌与铋的原子比的上升,ZnO多孔片状的表面逐渐变成Bi3.9Zn0.4V1.7O10.5物质。但其比例高于1:0.02时,在片状Bi3.9Zn0.4V1.7O10.5的区域表面又生长出BiVO4纳米颗粒。漫反射光谱测试显示出ZnO/Bi3.9Zn0.4V1.7O10.5复合物随着锌与铋的原子比的上升其在400~600 nm可见光区的吸收逐渐增强。所制样品在可见光（波长大于420 nm）进行了光催化降解罗丹明B的测试,结果表明在所制样品中,锌与铋的原子比为1:0.0133的ZnO/Bi3.9Zn0.4V1.7O10.5纳米片虽然其可见光的吸收并没有明显增强但却表现出最佳的光催化活性。荧光与电化学测试得出了低含量BZVO的ZnO纳米片可见光催化活性的提高主要是因为表面ZnO/Bi3.9Zn0.4V1.7O10.5异质结构提高了光生载流子的分离与传送。这种二维材料的表面建造有利于光催化的进行。因此,此法可应用于其它二维纳米材料的建造以提高光催化活性。     

Synthesis and characterization of Y3Al5O12 and ZrO2-Y2O3 thermal barrier coatings by combustion spray pyrolysis

Y₃Al₅O₁₂ and ZrO₂-Y₂O₃ (8 mol% YSZ) coatings for potential application as thermal barrier coatings were prepared by combustion spray pyrolysis. Thermal cycling of as deposited coatings on stainless steel and FeCrAlY bond coat substrates was carried out at 1000 °C and 1200 °C to determine the thermal fatigue response. Structural and morphological studies on Y₃Al₅O₁₂ and 8 mol% YSZ coatings before and after thermal cycling have been carried out. It has been noted that the coatings on FeCrAlY substrates remain intact after 50 cycles between room temperature and 1200 °C, whereas the coatings on stainless steel show some minor damage such as peeling off near the periphery after 50 cycles at 1000 °C. Thermal diffusivity values of Y₃Al₅O₁₂ and 8 mol% YSZ films were measured by using photo thermal deflection spectroscopy and the values are lower than those of coatings produced by conventional techniques such as EBPVD and APS.