Fretting properties of SUS304 stainless steel in a vacuum environment

In this paper the effect of the ambient pressure on the friction and wear of SUS304 stainless steel during fretting at room temperature is described.

The ambient pressure was varied from 10⁻³ to 10⁵ Pa. The experiment was carried out under the following conditions: normal load, 14 N; slip amplitudes, 35 and 110 μm; frequency, 8.3 Hz; number of fretting cycles, 6 × 10⁴.

The relationship between the frictional behaviour and the number of cycles is affected by the pressure. The coefficient of friction at steady state increases with a decrease in the pressure to below 10 Pa. From the point of view of the wear mechanism, the transition is determined as that from oxidative wear at the higher pressure to adhesive wear at the lower pressure. The transition pressure depends on the slip amplitude, i.e.it is 2.7 Pa at 35 μm and 10⁻¹ Pa at 110 μm. The wear volume is greater in the oxidative wear regime than in the adhesive wear regime. Oxide wear debris is removed easily from the interface in the former regime. In contrast, metallic wear debris is retained at the interface and adhesive transfer occurs from one surface to the opposing surface in the latter regime. The characteristic feature of the wear damage at 10⁻³ Pa and at 35 μm is the formation of a vertical crack at the boundary between the fretted and the unfretted areas.     

GCr15钢等离子体源离子注入表面改性

用等离子体源离子注入技术对GCr15钢进行了氮离子注入,对注入层的成分进行了俄歇剖面分析,对注入层的显微硬度和摩擦性能进行了测试,对摩擦磨损表面进行了扫描电镜分析,研究结果表明;注入层的硬度和耐磨性均获得了明显的提高。     

含芳香氨基酸三肽及其衍生物自由基离子的形成和解离机理研究

铜-配体(L)-三肽组成的三元复合物［Cu(L)M］²⁺,其中,L表示4′-氯-2,2′:6′,2″-三联吡啶(缩写为4Cl-tpy);M表示酪氨酰-甘氨酰-色氨酸(YGW)及其修饰型三肽(CH₃CO-YGW-OCH₃,缩写 Ac-YGW-OMe)。使用该复合物,通过碰撞诱导解离 (collision-induced dissociation, CID)产生两种自由基离子 (［YGW］^·+和［Ac-YGW-OMe］^·+)。采用串联质谱结合密度泛函理论 (density functional theory, DFT)得到气相稳定结构,并研究其气相解离行为。研究结果表明,［YGW］^·+和［Ac-YGW-OMe］^·+的气相解离行为截然不同,［YGW］^·+主要产生［M-CO₂-116］⁺和［M-CO₂］^·+碎片离子;而［Ac-YGW-OMe］^·+在气相中主要产生［M-CH₃OH］^·+碎片离子。推测这两种离子的气相裂解机理分别为：［YGW］^·+羧基上的质子重排到多肽骨架中羰基氧上,经历 C_α-C键的断裂产生［M-CO₂］^·+、断裂色氨酸侧链 C_β-C_γ键产生［M-CO₂-116］⁺离子;［Ac-YGW-OMe］^·+则先经历质子重排到酯基氧上,然后经过C-O酯键的断裂形成［M-CH₃OH］^·+离子。参与重排的质子可能有3个来源：Ac-YGW-OMe中甘氨酸的C_α-H、色氨酸的C_α-H 或C_β-H,该机理有待进一步验证。本研究将为其他类型多肽及衍生物的结构及气相反应机理研究提供参考。     

Tribology of silicon-thin-film-coated SiC ceramics and the effects of high energy ion irradiation

The sliding friction coefficients and specific wear of SiC ceramics coated with a silicon thin film (Si/SiC) with and without subsequent Ar⁺ irradiation against a diamond pin were measured with a pin-on-disk tester at room temperature in laboratory air of approximately 50% relative humidity without oil lubrication for 40 h. The friction coefficient of Ar⁺-irradiated Si/SiC was about 0.05 with a normal load of 9.8 N and remained almost unchanged during the 40 h test, while that of SiC increased from 0.04 to 0.12 during the test. The silicon deposition also reduced the specific wear of SiC to less than one tenth of that of the uncoated SiC. Effectively no wear was detected in Si/SiC irradiated to doses of over2×10¹⁶ions cm⁻².     

二硫-水自由基阳离子复合物中二中心三电子键的质谱研究

含硫二中心三电子（2c3e）键的研究一直是蛋白质中自由基传递领域的重要课题。本研究采用串联质谱和同位素标记方法研究不同位阻［RS-SR+H₂O］^+·的质谱碎裂模式,以探索位阻不同时这些自由基阳离子配合物内2c3e键的结构性质。结果表明,空间位阻低的［RS-SR+H₂O］^+·（R=甲基,乙基或丙基）碎裂时主要产生［RSH+H₂O］+·和［RSOH+H］⁺ 2种离子,而空间位阻高的［RS-SR+H₂O］^+·（R=异丙基或叔丁基）主要碎片离子是由母离子丢失H₂O而形成的［RS-SR］^+·。因此,在空间位阻低的［RS-SR+H₂O］^+·中2c3e键应以［S∴S］⁺的形式存在,而在空间位阻高的［RS-SR+H₂O］^+·中2c3e键应以［S∴O］+的形式存在。由此可见,结构环境的不同对自由基结构的性质有重要影响,这有助于理解与2c3e键有关的化学反应和生物体中自由基的传递过程机理。     

多肽衍生物中自由基介导的选择性C—C键断裂及异构体区分

选择性C—C键断裂反应是化学领域的前沿课题,尤其对于生物大分子,该研究具有重要意义。由于化合物中活性相似的C—C键普遍存在,选择性断裂其中1个C—C键是一大难点。本文以非天然氨基酸组成的多肽衍生物为研究对象,采用TEMPO自由基引发剂策略,将邻甲基苯甲酰(Bz)自由基引入多肽分子(M),在气相中成功制备出［Bz-M+H］^·+自由基离子。通过串联质谱实验发现,该离子相对于质子化多肽分子［M+H］⁺显示出更高的反应活性,具有更丰富的气相解离反应路径,其特征碎片离子［Bz·-a1］⁺和［(Bz-M+H)-HCOOEt］^·+可作为异构体区分和选择性C—C键断裂的灵敏探针,为质谱法区分多肽异构体和选择性C—C键断裂提供了思路和方法。     

65Mn钢表面激光熔覆温度场模拟及性能研究

为了探究不同激光熔覆工艺参数对温度场的影响,利用ANSYS软件对激光熔覆温度场进行模拟。在选定工艺参数下,通过激光熔覆技术在65Mn钢表面熔覆Ni60A合金粉,并与镍基焊条电弧焊试验进行对比。对两种熔覆层的显微组织、显微硬度及摩擦磨损性能进行观察和测试。结果表明：激光熔覆温度场的最高温度与激光功率、频率成正比,而与扫描速度成反比。在激光功率580 W,扫描速度100 mm/min,频率4 Hz,脉宽8 ms的工况下,温度场最高温度达到2 092.1℃。激光熔覆层主要由等轴晶、柱状晶组成,而电弧焊覆层组织的晶粒组织粗大,存有大量树枝晶。激光熔覆层晶粒更加致密,组织均匀,强度、塑韧性性能更好。在硬度与耐磨性方面,激光熔覆层硬度平均值为531.24 HV_0.2,电弧焊熔覆层硬度平均值为492.46HV_0.2,且激光熔覆对硬度的提高效果更加显著。激光熔覆层的磨损率为4.9×10^-4 mm³·N^-1·m^-1,是基体的3/5。磨损机理由严重的粘着磨损转变为轻微的磨粒磨...     

Research on the fretting wear behavior of silicon wafers before and after carbon ions implantation

Carbon ions with different doses of 2×10¹⁵ and 2×10¹⁶ ions/cm² were implanted into single crystal silicon wafers under an energy level of 80 keV. The nanohardness and elastic modulus of silicon wafers were studied on the nano-mechanical testing system. The fretting wear tests were performed on the UMT-2 Micro-tribometer to evaluate the fretting wear resistance of C⁺ implanted silicon wafer and to investigate its micro-tribological properties. The results demonstrate that the nanohardness and elastic modulus of silicon wafer with dose of 2×10¹⁵ ions/cm² decreased and those of 2×10¹⁶ ions/cm² changed little. Implanted silicon wafer with dose of 2×10¹⁶ ions/cm² had much lower coefficient of friction and wear volume under low loads, which suggests a significant effect of friction-reducing and anti-wear. The results also indicate that abrasive wear was the main wear mechanism for both virgin silicon and C⁺ implanted silicon with dose of 2×10¹⁵ ions/cm². However, adhesive wear played a significant role in the wear mechanism of the C⁺ implanted silicon with dose of 2×10¹⁶ ions/cm² under the low loads, while the abrasive wear dominated the wear mechanism under high loads.     

A comparison of the wear of cross-linked polyethylene against itself under reciprocating and multi-directional motion with different lubricants

A two-piece, silane cross-linked polyethylene (XLPE) finger prosthesis has been developed. To further the knowledge of the wear of XLPE against itself, a number of ‘pin-on-plate’ wear tests were undertaken, under different conditions of lubrication. These were distilled water, bovine serum and dry conditions. A second group of tests were then carried out, in which multi-directional motion was applied to the test pins. All tests had XLPE pins loaded at 40 N rubbing against XLPE plates. All the XLPE came from the same batch.

In all tests, pin wear was much less than plate wear. Under reciprocation only, the least wear was found when bovine serum was the lubricant (k=0.6×10⁻⁶ mm³/N m) and the maximum wear was when distilled water was the lubricant (k=5.8×10⁻⁶ mm³/N m). When multi-directional motion was applied to the test pins, increased wear occurred under lubrication with bovine serum (k=3.4×10⁻⁶ mm³/N m). Surprisingly, wear decreased when distilled water was used (k=0.7×10⁻⁶ mm³/N m), yet wear factors remained similar in the ‘dry’ test (k=0.7×10⁻⁶ mm³/N m). The dry tests had remarkably low wear.     

Mo离子注入提高TC4合金微动磨损抗力的研究

对TC4合金进行了Mo离子注入表面改性处理,利用摩擦磨损试验机进行了点接触微动磨损试验,借助读数显微镜和表面粗糙度仪测量出有关参数,计算出试样的微动磨损体积。结果表明,Mo离子注入使试样表面硬度提高,微动磨损体积明显降低。在微动磨损初期,Mo离子注入具有较好的减摩效果。Mo离子注入带来的表面强化效应是基体合金的微动磨损抗力得以提高的主要原因。     

Fretting wear behavior of nitrogen ion implanted titanium alloys in bovine serum lubrication

Nitrogen ion implantation was performed on biomedical titanium alloys by using of the PBII technology to improve the surface mechanical properties for the application of artificial joints. The titanium nitride phase was characterized with X-ray photoelectron spectroscopy (XPS). The nanohardness of the titanium alloys and implanted samples were measured by using of in-situ nano-mechanical testing system (TriboIndenter). Then, the fretting wear of nitrogen ion implanted titanium alloys was done on the universal multifunctional tester (UMT) with ball-on-flat fretting style in bovine serum lubrication. The fretting wear mechanism was investigated with scanning electron microscopy (SEM) and 3D surface profiler. The XPS analysis results indicate that nitrogen diffuses into the titanium alloy and forms a hard TiN layer on the Ti6Al4V alloys. The nanohardness increases from 6.40 to 7.7 GPa at the normal load of 2 mN, which reveals that nitrogen ion implantation is an effective way to enhance the surface hardness of Ti6Al4V. The coefficients of friction for Ti6Al4V alloy in bovine serum are obviously lower than that in dry friction, but the coefficients of friction for nitrogen ion implanted Ti6Al4V alloy in bovine serum are higher than that in dry friction. Fatigue wear controls the fretting failure mechanism of nitrogen ion implanted Ti6Al4V alloy fretting in bovine serum. The testing results in this paper prove that nitrogen ion implantation can effectively increase the fretting wear resistance for Ti6Al4V alloy in dry friction, and has a considerable improvement for Ti6Al4V alloy in bovine serum lubrication.     

SEM electron channelling patterns as a technique for the characterization of ion-implantation damage

Electron channelling patterns (ECPs) formed in back-scattered images in the scanning electron microscope (SEM) have been used occasionally to confirm surface amorphization during ion implantation. In order to place such observations on a more quantitative basis, the study reported here has explored the variation of ECP appearance with both specimen damage levels (and thus subsurface structures) and SEM accelerating voltage (i.e. sampled depth). Polished and annealed (0001) single crystal sapphire discs were implanted to various damage levels up to both subsurface and full surface amorphization. Damage levels were measured independently by Rutherford back-scattering (RBS). Selected-area ECPs were obtained in a Jeol-840 electron microscope operating over the range 5–40 kV in 5-kV steps. Progressive ECP degradation—in terms of high-order line disappearance—was observed with increasing dose, culminating in total pattern loss when full surface amorphization occurred. However, ECP information could still be obtained from the damaged near-surface material even when a subsurface amorphous layer was present, thus demonstrating the shallow retrieval depth of information from the ECP technique. Indeed, because the spatial distribution of damage from ion implantation is both calculable and measurable, these experiments have also allowed us, for the first time, to explore and demonstrate the shallow sample depths from which the majority of ECP contrast originates (< 150 nm in sapphire at an accelerating voltage of 35 kV), even when the beam penetration is considerable by comparison (～ 5 μm). Furthermore, the way in which this sampled depth varies with SEM accelerating voltage is both demonstrated and shown to be a powerful diagnostic technique for studying the distribution of near-surface structural damage.     

Microstructure and wear resistance of CP titanium laser alloyed with a mixture of reactive gases

Laser processing is a promising technique for alloying and synthesis of wear resistant layers. In this work, commercially pure titanium was laser alloyed with various proportions of nitrogen and carbon monoxide in order to produce a composite surface layer. The following gas mixtures were selected: 100% N₂, 67% N₂ + 33% CO, 50% N₂ + 50% CO, 33% N₂ + 67% CO and 100% CO. The microstructure, roughness and composition of coated specimens were characterized. The presence of Ti(C,N,O) in the surface layer was assessed by X-ray diffraction, X-ray photoelectron spectroscopy and Auger electron spectroscopy. The abrasive wear resistance of coatings was determined and related to their surface hardness. The abrasive wear resistance of the laser alloyed coating was substantially improved compared to untreated titanium and appears to be superior when composed of Ti(C,N,O) prepared from a mixture of gases.     

5,6,7,4′-四羟基黄酮和5,6,7,4′-四甲氧基黄酮高分辨电喷雾串联质谱裂解规律对比研究

以5,6,7,4′-四羟基黄酮和5,6,7,4′-四甲氧基黄酮为例,运用高分辨电喷雾串联质谱在正离子模式下(HR-ESI-MS/MS)获得的碎片离子,根据一、二级质谱离子的精确质荷比,分别推导出两种黄酮可能的裂解途径,并比较多甲氧基、多羟基黄酮质谱裂解规律的异同。结果表明:在正离子模式下,5,6,7,4′-四羟基黄酮和5,6,7,4′-四甲氧基黄酮的一级质谱均可获得稳定的准分子离子。5,6,7,4′-四羟基黄酮的二级质谱碎片离子由准分子离子[M+H]+经RDA裂解及进一步脱水和(或)脱一氧化碳中性分子产生,直接由准分子离子脱水及一氧化碳中性分子获得的碎片离子丰度比较低;5,6,7,4′-四甲氧基黄酮二级质谱碎片即可由准分子离子[M+H]+直接经RDA裂解,还可先脱去乙烷或甲烷中性分子再经RDA裂解(1,3断裂)获得。此外,该化合物还有大量的碎片离子是由准分子离子[M+H]+分别经脱水、甲烷、乙烷或进一步脱甲基、一氧化碳而获得。两个化合物质谱碎片的比较结果表明,多甲氧基黄酮的二级质谱碎片裂解机制更复杂,碎片信息更丰富。该方法可为黄酮类化合物成分的快速定性分析提供支持,也可为黄酮类化合物体内代谢产物的LC-MS/MS鉴定提供依据。     

The wear behaviour of high-chromium white cast irons as a function of silicon and Mischmetal content

The sliding wear behaviour of high-chromium white cast iron (16.8% Cr) has been examined as a function of silicon and Mischmetal alloy additions (1, 2, 3 and 5% Si and 0.1 and 0.3% Mischmetal). Such additions are known to modify the structure, but there is considerable controversy as to the exact effect. Silicon was found to refine the dendritic structure and increased the eutectic carbide volume fraction. However, for contents above 3%, transformation of the austenitic matrix to pearlite occurred in preference to martensite. Mischmetal additions reduced the austenite dendrite arm spacing, but did not have a significant effect on the carbide structure. The wear behaviour was investigated for each alloy in the as-cast (austenitic matrix) and hardened (martensitic) conditions using a block on ring configuration in pure sliding in the load range 42–238 N for a distance of 70 km against a hardened M2 steel counterface. For low loads (42 and 91 N), all the alloys showed a similar wear rate (3×10⁻⁴ to 4×10⁻⁴ mm³/m), associated with the formation of a thin (3 μm) oxide film of Fe₂O₃, the formation of very fine debris and a small depth of deformation below the worn surface (7 μm). For higher loads, wear was a strong function of microstructure, and was associated with a thicker film of the oxides Fe₂O₃ and Fe₃O₄ and greater depths of deformation. The iron with 2% silicon exhibited the best performance with a wear rate of 7×10⁻⁴ mm³/m and this was attributed to its finer structure and the formation of a thicker oxide film. In contrast, the iron with 5% silicon exhibited the worst performance, with a wear rate of 14×10⁻⁴ mm³/m, attributed to the pearlitic matrix. A linear relationship was observed between the depth of carbide fracture and the wear rate. The relationship between microstructure and wear mechanism is discussed.     

Investigation of the surface structure and elastic properties of calcium silicate hydrates at the nanoscale

This work is the first step towards the understanding of the structure of calcium silicate hydrate (C–S–H), the main constituent of cement paste, at the nanoscale. The first demonstration of atomic-resolution imaging of the (C–S–H) surface with an atomic force microscope (AFM) was performed.

C–S–H nanoparticles (60×30×5 nm³) were partially recrystallized by Ostwald ripening after long-term equilibrium in saturated calcium hydroxide solution of different concentration, leading to C–S–H of different calcium/silicon ratio (Ca/Si). The results of atomic resolution made possible the investigation of the C–S–H cell surface parameters. The surface layer structure depended on the calcium hydroxide concentration with which it equilibrated.

The change in structural properties perpendicular to the C–S–H layer was probed by modifying AFM for nanoindentation hardness measurements with a depth of indentation as low as 1 nm. The change in elastic modulus depending on the calcium/silicon ratio was evaluated and correlated in the change in structural parameters in this direction as estimated by X-ray diffraction.     

二次离子质谱仪中二次中性粒子空间分布研究

为提高二次离子质谱仪（secondary ion mass spectrometer, SIMS）的灵敏度,引入了飞秒激光电离一次离子轰击溅射产生的二次中性粒子。实验以纯银、纯铜为目标样品,利用自主研制的飞行时间质谱仪分析二次后电离的离子,研究二次中性粒子的后电离效率和空间分布。结果表明：飞秒激光电离技术可将仪器的灵敏度提高70倍以上;飞秒激光电离出的¹⁰⁷Ag⁺和¹⁰⁹Ag⁺的同位素丰度比值误差为0.8%;二次中性粒子的空间分布符合Maxwell-Boltzmann 模型。该结果可为在设计方法上提高SIMS仪器灵敏度提供依据。     

Preliminary considerations in the use of industrial sonic nozzles

Preliminary considerations applying to the necessary instrumentation for the use of sonic nozzles is reviewed. A way to make sonic nozzles for industry, together with a method to determine the discharge coefficient of a convergent nozzle operating in the sonic regime in conditions of ideal flow is suggested. The results obtained for the behaviour of the discharge coefficient of sonic nozzles, in the range from 4×10⁴ to 2×10⁵ are compared with the standard ISO 9300 (Standard ISO 9300. Measurement of gas flow by means critical flow Venturi nozzles, 1990) and the curve proposed by Ishibashi et al. (M. Ishibashi, M. Takamoto, N. Wanatabe, Y. Nakao. Precise calibration of critical nozzles of various shapes at the Reynolds number of 0.2–2, 5×10⁵. Proceedings of FLOMEKO 94).     

The acting wear mechanisms on metal-on-metal hip joint bearings: in vitro results

Metal-on-metal (MOM) hip joint bearings are currently under discussion as alternatives to metal-on-polymer (MOP) bearings. Some criteria under scrutiny are the wear resistance, the influence of wear particles on the surrounding tissue, as well as the frictional torque. In order to understand and control the wear behavior of such a bearing a close correlation between the microstructures of the alloys used and the acting wear mechanisms has to be found. Thus, commercially available CoCrMo-balls were tested against self mating concave pins in a physiological fluid at 37°C under reciprocating sliding wear (1 Hz). The compressive load was 750 N (body weight). For 2×10⁶ cycles tests were carried out continuously and with periodically occurring resting periods. On the basis of the observed wear appearances the acting wear mechanisms are defined and evaluated as to their contribution to the wear behavior. Due to the high local contact stresses surface fatigue prevails initially. Cr– and Mo–carbides are fractured and torn off the surfaces bringing about additional surface fatigue by indentations and initiating abrasion. The weight loss can be predominately attributed to these mechanically dominated wear mechanisms. In a parallel occurring tribochemical reaction layers are generated from denatured proteins. These adhere rigidly to the surfaces and cover parts of the contacting surfaces avoiding adhesion. Thus, the wear behavior is mainly influenced by the alternating balance between surface fatigue and abrasion on the one side and by tribochemical reactions on the other side.     

典型环亚胺类毒素大气压化学电离质谱分析

利用离子阱质谱技术分析了两种典型环亚胺类毒素（GYM和SPX1）在大气压化学电离（APCI）条件下的质谱裂解特征,并与电喷雾电离（ESI）质谱法进行了比较。GYM和SPX1在APCI一级质谱分析过程中易形成准分子离子［M+H］⁺峰（基峰）;在二级质谱分析过程中,母离子［M+H］⁺通过丢失H₂O中性碎片形成稳定的特征子离子峰;并结合三级质谱分析,推测了两种毒素的裂解途径。结果表明：大气压化学电离质谱法（APCI-MS）的灵敏度好于电喷雾质谱法（ESI-MS）;液相色谱-大气压化学电离质谱法（LC-APCI-MS²）分析4种不同基质样品中GYM和SPX1的专属性、重复性、稳定性和抗基质干扰能力均好于液相色谱 电喷雾质谱法（LC-ESI-MS²）。综上,APCI-MS法适于典型环亚胺类毒素的分析,本研究可为LC-APCI-MS定性、定量分析不同基质复杂样品中环亚胺类毒素提供参考和依据。