天然蛇纹石粉体润滑油添加剂的自修复性能及自修复层形成机理研究

采用RFT-III型往复摩擦磨损试验机(盘-块接触方式)考察了油酸表面修饰天然蛇纹石粉体润滑油添加剂对钢-钢摩擦副的自修复性能;采用显微硬度计测定了试块磨损表面硬度,采用扫描电镜、能谱仪、X射线光电子能谱仪分析了试块磨损表面和截面的形貌、组成、典型元素的化学状态,探讨了天然蛇纹石粉体的自修复机理.结果表明:油酸表面修饰天然蛇纹石粉体作为润滑油添加剂可显著减小钢-钢摩擦副的摩擦系数和磨损率.这是由于其可经由摩擦化学作用而在磨损表面生成具有良好减摩抗磨性能的自修复层所致.自修复层由不同粒径的纳米颗粒密堆积而成,主要成份为Fe₂O₃和非晶石墨,并含有少量Fe、有机物碎片、含硅有机化合物、SiO₂等.     

含纳米添加剂的润滑体系在摩擦过程中的接触电阻研究

采用UMT-2型微摩擦磨损试验机考察了4种纳米颗粒LaF3、Ag、SiO2 及Al2O3作为润滑油添加剂在摩擦过程中的接触电阻随时间变化的情况,并由此监测摩擦副表面的成膜状况;采用X射线光电子能谱仪分析4种纳米添加剂润滑下磨损表面典型元素的化学状态,并结合接触电阻测试结果分析纳米油润滑添加剂的润滑机理.结果表明:接触电阻测试能够适时监测添加剂在摩擦副表面的成膜过程,4种纳米润滑油添加剂在边界润滑条件下均能够在磨损表面沉积成膜,其在试验过程中的化学状态没有发生变化,但4种纳米润滑油添加剂在摩擦过程中的成膜性能不同,Ag和LaF3在摩擦过程中的沉积速率、沉积膜厚度及其在摩擦副表面的结合强度优于SiO2和Al2O3.     

羟基硅酸镁复合粉体润滑油添加剂对钢-钢摩擦副的抗磨自修复机理

以羟基硅酸镁复合矿物粉体作为润滑油添加剂,采用MM-200型环-块摩擦磨损试验机研究了45^#钢摩擦副的减摩抗磨性能;采用扫描电子显微镜观察了钢环磨损表面和润滑油所含添加剂颗粒的形貌,采用能谱仪分析了钢环磨损表面成份,采用表面形貌仪测定了钢环磨损表面粗糙度,进而探讨了复合矿物粉体添加剂的抗磨自修复机理.结果表明:羟基硅酸镁复合矿物粉体添加剂对钢-钢摩擦副具有良好的减摩抗磨作用.在基础油(46^#机油)润滑条件下,随着载荷的增加,磨损机制由轻微擦伤转变为严重擦伤和黏着磨损.在含添加剂的油润滑条件下,较低载荷下钢环磨损表面发生轻微擦伤,且擦伤程度比基础油润滑下的更轻;而在较高载荷条件下钢环磨损表面非常光滑,呈现轻微的黏着磨损迹象.其原因在于在较低载荷条件下,添加剂在摩擦过程中可发生团聚形成大小不一的球状团聚体,球状团聚体可起到微球轴承的作用,使钢-钢摩擦副由滑动接触状态转变为滚动接触状态,从而显著降低摩擦系数,提高抗磨性能.而在较高载荷下,羟基硅酸镁复合矿物粉体添加剂易在钢-钢摩擦副磨损表面形成自修复抗磨层,从而隔离金属表面的直接接触,起到良好的减摩抗磨作用.     

NiAl-TiO_2/Bi_2O_3纳米复合涂层制备及宽温域摩擦磨损性能

采用等离子喷涂(APS)技术制备NiAl-TiO_2/Bi_2O_3纳米复合涂层,通过高能球磨及喷雾造粒制备TiO_2/Bi_2O_3纳米复合喂料,考察纳米结构TiO_2/Bi_2O_3的不同配比对复合涂层显微结构、力学及摩擦磨损性能的影响.结果表明:复合涂层组织致密,各相分布均匀,采用TiO_2/Bi_2O_3纳米复合喂料使涂层呈现出典型的双态区域,涂层结合强度均高于40 MPa.单纯TiO_2纳米喂料制备的复合涂层中低温摩擦磨损性能较差,TiO_2/Bi_2O_3的复配改善了涂层中低温的塑性和摩擦学性能,并提高了涂层的高温润滑性能,其复合涂层磨损率均低于7×10-5 mm~3/(N·m),摩擦系数在800℃时可低至0.1左右,但过高的Bi_2O_3含量会导致涂层硬度降低,磨损率增加.高温摩擦促进了Bi_4Ti_3O_(12)、NiTiO_3等三元氧化物润滑相的生成,其与TiO_2、NiO在磨损表面形成光滑连续的摩擦层使涂层具有优异的高温摩擦学性能.     

油酸修饰纳米氟化钙的萃取法制备及其摩擦学性能

采用萃取法制备了油酸修饰的纳米CaF2,用X射线衍射(XRD)对纳米CaF2粉体样品进行物相分析,同时用透射电子显微镜(TEM)及傅立叶变换红外光谱仪(FT-IR)进行表面形貌和成分分析,并在四球摩擦磨损试验机上评价了CaF2在润滑脂中的摩擦学性能.结果表明,制备的纳米CaF2粒径在23 nm左右,油酸以化学吸附的方式吸附在CaF2纳米核表面;作为添加剂油酸修饰纳米CaF2在润滑脂中具有良好的抗磨性能和极压性能,在高载荷时具有良好的减摩性能.SEM,EDS和XPS分析表明在摩擦过程中形成了由CaF2、CaO、氧化铁和有机添加剂所组成的边界润滑膜,从而使OA-CaF2具有良好的摩擦学性能.     

碳酸钙纳米颗粒复合超分子凝胶润滑剂的摩擦学性能研究

采用碳酸钙纳米颗粒与全氟聚醚型超分子凝胶复合得到了一种新型的纳米颗粒复合超分子凝胶润滑剂. 超分子凝胶具有错综复杂的网络结构,有效地提高了碳酸钙纳米颗粒在全氟聚醚润滑油中的分散稳定性. 此外,碳酸钙纳米颗粒作为添加剂极大地提高了超分子凝胶的润滑性能,使其表现出较好的耐高温性能,以及较高的承载力. 采用差式扫描量热仪、热重分析仪和流变分析仪对该复合润滑剂的热力学性能进行表征,结果显示该复合润滑剂具有很好的热稳定性以及较好的力学性能. 最后,通过X射线光电子能谱(XPS)对其摩擦机理进行表征,结果表明碳酸钙纳米颗粒复合超分子凝胶润滑剂优异的摩擦学性能可归因于碳酸钙纳米颗粒在摩擦副表面形成了易剪切的薄膜,以及小尺寸的纳米粒子在摩擦过程中对摩擦表面进行的自修复效应.      

有机钼及其复合纳米润滑添加剂的摩擦磨损性能研究

采用X-P型销-盘摩擦磨损试验机和MRS-10J型四球摩擦磨损试验机考察了N68MD、N68ME、N68和SAE404种含有机钼及其复合纳米润滑添加剂的润滑油的摩擦磨损性能,分别采用扫描电子显微镜和电子衍射能量谱仪分析了摩擦副的磨损形貌及其磨损表面元素分布情况.结果表明:在N68MD润滑时,钢/钢摩擦副具有较低的摩擦系数和磨损量,并且具有良好的抗极压性能;在N68ME润滑时,钢/钢摩擦副除了表现出很小的摩擦系数和良好的抗极压性能以外,还表现出优异的自修复功能,这是由于有机钼与纳米铜协同作用的结果.     

油酸表面修饰PbO纳米微粒作为润滑油添加剂的摩擦学性能研究

利用四球摩擦磨损试验机考察了油酸修饰PbO纳米微粒作为润滑油添加剂的摩擦学行为,并用X射线光电子能谱仪（XPS）、扫描电子显微镜（SEM）和能量散射谱仪（EDS）等现代分析工具对钢球磨损表面进行了分析,摩擦磨损试验结果表明,油酸修饰PbO纳米微粒作为润滑油添加剂能够明显提高基础油的减摩抗磨能力,当添加质量分数为0.30%时,与基础油相比可以使摩擦系数和钢球磨厂主 直径降低30%左右。XPS、SEM及EDS分析结果表明,钢球表面在摩擦过程中形成了一层富含PbO的边界润滑膜,这使得油酸修饰PbO纳米微粒作为润滑油添加剂表现出良好的摩擦学性能。     

α-ZrP层状纳米片的修饰改性及其摩擦学性能

采用一步水热法制备了阳离子表面活性剂修饰改性的α-磷酸锆(α-ZrP)纳米片. 利用X-射线衍射仪、傅里叶变换红外光谱仪、拉曼光谱仪、场发射扫描电镜和透射电子显微镜对α-ZrP纳米片在表面活性剂修饰前后的组成、晶体结构以及微观形貌进行了表征分析和观察，并对改性前后的α-ZrP在合成基础油PAO-6中的分散稳定性进行了对比分析，利用SRV-Ⅳ型微动摩擦磨损试验机对含有改性α-ZrP纳米片的PAO-6润滑油的摩擦学性能进行了研究. 结果表明:表面改性的α-ZrP纳米片在PAO-6润滑油中具有良好的分散稳定性，其作为添加剂时可显著提高润滑油的极压性能和抗磨损性能.      

表面修饰SiO2纳米微粒对锂基脂抗磨性能影响的研究

合成了表面修饰SiO2纳米微粒,利用四球摩擦磨损试验机考察了SiO2纳米微粒作为锂基脂添加剂的摩擦磨损行为,用扫描电子显微镜、能量色散谱仪和X射线光电子能谱仪对钢球磨损表面进行了分析.结果表明:SiO2纳米微粒作为锂基脂添加剂具有良好的抗磨损性能,能够显著提高锂基脂的失效载荷.这是由于在摩擦过程中,SiO2纳米微粒富集在磨损表面并形成边界润滑膜,对磨损表面起到修复作用,从而使得锂基脂的抗磨和承载能力明显提高.     

WSe2纳米结构的合成及减摩性能研究

将W粉和Se粉按一定比例混合,直接密封在石英管中加热或高能球磨、压片,在Ar气氛中加热,得到了不同形貌的WSe2纳米结构.利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)和透射电子显微镜(TEM、HRTEM)分析了WSe2纳米结构的组成、微观形貌和组织形态;利用UMT-2摩擦试验机考察了WSe2作为HVI500液体基础油添加剂的摩擦磨损性能.研究结果表明:直接密封加热得到的产物为棒状WSe2纳米材料,最小棒直径为6 nm;球磨、压片后加热得到WSe2纳米颗粒,颗粒的平均尺寸在50 nm以下,二者都具有层状结构和良好的结晶性.添加质量分数5%的WSe2纳米材料作为基础油添加剂能够显著降低摩擦系数,减少磨损,增强了材料抗疲劳磨损能力.     

Effect of ion-beam assisted deposition on the film stresses of TiO2 and SiO2 and stress control

Based on Hartmann-Shack sensor technique, an online thin film stress measuring system was introduced to measure the film stresses of TiO₂ and SiO₂, and comparison was made between the film stresses prepared respectively by the conventional process and the ion-beam assisted deposition. The effect of ion-beam assisted deposition on the film stresses of TiO₂ and SiO₂ was investigated in details, and the stress control methodologies using on-line adjustment and film doping were put forward. The results show that the film stress value of TiO₂ prepared by ion-beam assisted deposition is 40 MPa lower than that prepared by conventional process, and the stress of TiO₂ film changes gradually from tensile stress into compressive stress with increasing ion energy; while the film stress of SiO₂ is a tensile stress under ion-beam assisted deposition because of the ion-beam sputtering effect, and the film refractive index decreases with increasing ion energy. A dynamic film stress control can be achieved through in-situ adjustment of the processing parameters based on the online film stress measuring technique, and the intrinsic stress of film can be effectively changed through film doping.     

Converting industrial waste contact masses into effective multicomponent copper-based catalysts for the Rochow process

In this work, we report a simple and inexpensive approach to synthesize effective multicomponent Cu–Cu₂O–CuO catalysts for the Rochow process from industrial waste contact masses (WCMs). WCMs from the organosilane industry were treated with acid followed by reduction with metallic iron powder. The obtained copper powder was then subjected to controlled oxidation in air at different temperatures, followed by ball milling. The orthogonal array approach was applied to optimize this process, and the stirring speed and pH were found to significantly affect the leaching ratio and copper yield, respectively. When used for the Rochow process, the optimized ternary Cu–Cu₂O–CuO catalyst greatly enhanced the dimethyldichlorosilane selectivity and Si conversion compared with Cu–Cu₂O–CuO catalysts prepared without ball milling, bare Cu catalysts, and Cu–Cu₂O–CuO catalysts with different compositions. This could be attributed to their small particle size and the strong synergistic effect among the multiple components in the catalyst with the optimized composition.     

Ti、TiN、TiO2改性层的纳米力学性能测试与分析

采用等离子表面合金化技术,分别在316L不锈钢表面制备出渗Ti改性层、渗TiN改性层和TiO2改性层薄膜.使用连续刚度法,从截面方向和表面方向对改性层进行纳米压痕实验,研究改性层的纳米力学性能.实验测得材料在压痕过程中的载荷—位移曲线以及硬度和模量随压入深度的连续变化值.结果表明,改性层纳米力学特性表现为各向异性;TiN改性层的力学性能表现良好.TiO2改性层由渗Ti改性层经氧化制成,二者的弹性模量和硬度在截面方向上变化规律相似,在表面方向上数值相近.     

表面特性对纯滑弹流油膜形状和摩擦力的影响的试验研究

针对界面滑移效应可能产生较低的摩擦力,采用具有不同表面浸润性的玻璃盘,进行了纯滑弹流润滑试验.在采用SiO2镀膜玻璃盘的球-盘接触高聚物纯滑润滑试验中,从弹流到动压润滑的摩擦系数曲线呈现不同于传统Stribeck曲线的两个拐点.两个拐点分别与凹陷出现及弹性变形消失相关联.在较低载荷下,不同盘表面产生相近的干涉图像和摩擦系数曲线,高聚物的非牛顿效应产生的表观滑移可能是入口凹陷及非典型摩擦系数曲线的主因;在较高载荷下,盘滑试验中铬盘产生的摩擦系数和油膜厚度均较SiO2盘低,具有较低表面能的铬盘产生的界面滑移被认为是产生较低摩擦系数的主因.     

TiO2-loaded activated carbon fiber: Hydrothermal synthesis,adsorption properties and photo catalytic activity under visible light irradiation

TiO₂-loaded activated carbon fibers (ACF) were prepared by a hydrothermal method. The samples were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectrometry and UV–vis diffuse reflectance spectra (DRS). SEM images showed that the TiO₂ nanoparticles were deposited on the surface of ACF, and the particle size and loading amount of TiO₂ were varied by changing the initial concentration of tetrabutyl titanate (TBOT). The results of an ash experiment showed that the loading amounts of TiO₂ were 18.4%, 43.3%, 52.5%, 75.1%, and 91.1% for initial concentrations of TBOT of 0.07, 014, 0.21, 0.28, and 0.35 mol/L, respectively. Physical interactions played an important role in the formation of TiO₂/ACF composite fibers that absorb UV and visible light. Compared with those of ACF, improved adsorption and photocatalytic activity toward Rhodamine B (RhB) were observed for TiO₂/ACF composite fiber. The Rhodamine B could be removed efficiently by TiO₂/ACF composite fibers, and the TiO₂ loading amount had a significant effect on the photocatalytic activity of TiO₂/ACF composite fibers.     

Influence of preparation route and slip casting conditions on titania and barium titanate ceramics

Titania (TiO₂) and barium titanate (BaTiO₃) were synthesized using three different dicarboxylates, which included oxalate, malate and tartarate. These powders were characterized by X-ray powder diffraction, scanning electron micrographs, BET specific surface area and particle size distribution. Their properties depended to a great extent on the nature of the precursor. The titania and barium titanate powders obtained from the tartarate precursor were found to be good for slip casting. Slips of these oxides with different solids contents were prepared at different pH values using both distilled water and ethanol as the dispersing agent and also with and without deflocculant. The rheological behaviors of the suspensions were then determined, and the slip, green and sedimentation bulk densities were measured. The minimum viscosities were observed at pH 8.2 for the TiO₂–water and pH 10.2 for the BaTiO₃–water system.     

High-frequency dielectric properties of BSTO ceramic prepared with hydrothermal synthesized SrTiO3 and BaTiO3 powders

BSTO dielectric ceramic was prepared from SrTi03 and BaTi03 powders synthesized by hydrothermal method, as well as from Bao.sSro.4TiO3 powder synthesized by conventional solid-state reaction. The former can be sintered at a relatively low temperature of 1120 ℃. Characterization by SEM showed that the grain shapes of both ceramics are cubical, though the grain size of the former is much smaller. Dielectric constants measured at 20℃ were shown to vary with frequency in the range from I kHz to 2 MHz and dc bias field, and further that the dielectric loss of the former to be less than 2 × 10^- 3 in the frequency range of 20 kHz to 1 MHz, much smaller than that of the latter sample. For the former, temperature dependence of dielectric constant is much flatter and there exists an extended phase transition diffusion covering a wide temperature range of Curie temperature To. The smaller grain size of the former depresses the dc bias electrical field dependence of dielectric constant. The tunability is 7% under a bias field of 0.6 kV/mm dc.     

Hydrodesulfurization catalyst prepared by urea-matrix combustion method

Co–Mo/γ-Al₂O₃–TiO₂ hydrodesulfurization (HDS) catalyst samples prepared by a urea matrix combustion (UMxC) method, were evaluated in a stainless tubular fixed-bed reactor, with thiophene, benzothiophene and dibenzothiophene in xylene as model feedstocks. The samples were pre-sulfurized using a cyclohexane solution of 3% CS₂ and then tested for the HDS reaction. The test results were compared with catalysts prepared by conventional methods involving sequential impregnation (SI) and co-impregnation (CI). The catalysts were characterized using X-ray diffraction (XRD), laser Raman spectroscopy (LRS), high resolution transmission electron microscopy (HRTEM) and N₂ physisorption, showing that the UMxC catalyst had higher pore volume and surface area than those prepared by the CI and SI methods. The UMxC method increased metal loading and avoided formation of inert phase, e.g., β-CoMoO₄, for the HDS reaction, suggesting that UMxC method is superior to the conventional impregnation techniques. TiO₂ promoter made particles on the catalyst surface closer and alleviated the interaction between molybdenum oxide and the support, and facilitated the formation of well-dispersed Co- and Mo-oxo species on catalyst surface, thus resulting in higher HDS catalytic activity than pure γ-Al₂O₃ support without modifiers. Consequently, the addition of TiO₂ obviously improved the HDS conversion of dibenzothiophene.     

硝酸铈爆轰制备球形纳米CeO2颗粒

以硝酸铈为原料,利用爆轰合成方法制备了CeO2纳米粒子。采用XRD和TEM对爆轰产物进行了检测和表征,并考察了尿素和亚硝酸钠对爆轰产物形貌的影响。3次实验结果表明,实验所得的CeO2晶体均为立方莹石结构,粒径分别为45、64、33 nm。比较发现:混合炸药中加入尿素后,颗粒外观呈球形;混合炸药加入亚硝酸钠后,颗粒直径较小。