真空计量标准的研制与应用

兰州物理研究所研制了一系列真空标准装置,可用于真空规、方向规、分压力质谱计、真空漏孔和正压漏孔的校准.其静态膨胀法真空标准装置、动态流量法真空标准装置及超高/极高真空校准装置是用于真空规校准的三套基础标准,覆盖的校准范围为(10-10～105)Pa;程控式真空规校准装置适用于工业部门,其校准范围为(10-4～105)Pa;为实现质谱计的校准,研制了一台具有三路相同独立进样系统的分压力质谱计校准装置,标准分压力通过磁悬浮转子规以两种不同的方法进行测量,该校准装置可实现(10-7～10-1)Pa范围内的分压力校准;为实现真空漏孔的校准,研制了恒压式气体微流量标准装置和固定流导法气体微流量标准装置.恒压式气体微流量标准装置的校准范围为(10-8>～10-2)Pa·m3/s,同定流导法气体微流量标准装置的校准范围为(10-10～10-5)Pa·m3/s,漏孔漏率的校准通过比较被校漏孔和标准气体微流量计在一台四极质谱计上引起示漏气体离子流的大小计算得到;为实现正压漏孔的校准,研制了一台正压漏孔校准装置,采用定容法和定量气体动态比较法对正压漏孔进行校准,校准范围为(5 × 10-5～10-1)Pa·m3/s;研制了一台定向流真空校准装置,实现对方向规的校准和非平衡态分子流的研究,装置的校准范围为(10-7～10-1)Pa.     

温度对正压漏孔校准装置本底漏率影响的研究

在实验室条件下,由于温度变化引起正压漏孔校准装置本底漏率变化是影响正压漏孔校准下限的主要因素,因此正压漏孔校准装置采用水浴恒温技术,采取主动恒温与被动恒温相结合的方式进行恒温,以减小因温度变化对本底漏率的影响。通过实验研究,采取恒温措施后,本底漏率降低到1.36×10-9Pa×m3/s,正压漏孔的测量下限可以扩展到2.667×10-8Pa×m3/s,延伸了正压漏孔标准的下限。     

正压漏孔校准装置的研制

作者对正压漏孔校准方法作了研究,为了对不同示漏气体的正压漏孔进行精确校准,建立了一套改进型的PΔV/t漏孔校准装置,并对该装置进行了不确定度的分析.该装置校准范围1×10-4 Pa m3/s～1×10-7 Pa m3/s,在漏率2×10-6 Pa m3/s时系统总误差小于4.0%.     

比较法校准氦真空参考漏孔漏率及合成不确定度评定

直接比对法是氦质谱检漏仪在稳定工作和引入气体相同条件下,将参考漏孔流出的氦气和标准漏孔提供的已知流量的氦气分别引入校准室中,用氦质谱检漏仪分别测量氦气产生的离子流,通过比较两次离子流的测量值计算出参考漏孔漏率的一种校准方法。这种校准范围为1×10-7Pa.m3/s~1×10-10Pa.m3/s。对同一参考漏孔,采用同样的校准测量,可以采用高斯分布统计的方法获得校准不确定度,其他不确定度分量由氦质谱检漏仪组成的校准装置决定,其合成相对不确定度可达到10%。     

比对法漏率校准装置

比对法漏率校准装置是计量气体漏率的一种装置 ,可绝对法和相对法对真空漏孔进行校准。绝对法的校准范围为 10 - 4～ 10 - 9Pa· m3/s;相对合成标淮不确定度为小于 10 %。相对比对法的校准范围为 10 - 6～10 - 1 0 Pa· m3/s,相对合成标准不确定度为小于 2 5 %。     

现场真空漏孔校准装置的设计

为了减小现场环境与校准环境的差异对真空漏孔校准的影响,通过理论研究,设计了现场真空漏孔校准装置,可实现对真空漏孔的现场校准。考虑到现场真空漏孔校准装置需便于携带及搬运,装置的设计采用了分体式结构。现场真空漏孔校准装置由抽气系统、校准室系统、真空漏孔连接系统、流量输出系统、充气系统、定容室与压力测量系统及烘烤系统等7个部分组成,复合了定容法及固定流导法两种校准方法,预计真空漏孔校准范围为5＆#215;10-10～5＆#215;10-5 Pa？m3/s,合成标准不确定度为10％。     

真空漏率校准装置的研制和应用

真空漏率校准装置可以对(10~5~10~(-4))Pa范围内的各种真空计和(10~(-7)~10~(-9))Pa·m~3/s的真空漏孔进行校准。该装置的特点是结构简单、量程宽、易操作和工作效率高。     

不同气体和压力对真空漏孔漏率的影响

针对目前大多数标准漏孔的漏率都是在He和入口压力为100 kPa下的漏率,采用定容变压法校准了铭牌漏率为2.3×10~(-6)Pa·m~3/s的标准真空漏孔在使用H_2、He、D_2三种气体时,在不同入口压力下的漏率。预先对系统进行了加热除气后计算了系统本底漏率大小,并探讨了本底漏率对校准漏孔漏率的影响。结合粘滞流-分子流理论研究了不同气体和漏孔入口压力对漏孔漏率的影响。     

定容法正压漏孔校准装置

研制出定容法正压漏孔校准装置。采用满量程分别为133 Pa(差压式)、1.33×105Pa(绝压式)的两台高精度电容薄膜真空计测量压力变化,通过全金属密封结构减小定容室漏放气对测量结果的影响;采用高精度半导体双级恒温系统获得了296±0.02 K的恒温效果,减小温度对漏孔漏率的影响;通过三个不同的标准体积作为定容室,拓宽装置的校准范围。研究结果证实,研制的校准装置仅采用定容法实现了3×10-1~4×10-8Pa·m3/s的校准范围,合成标准不确定度为1.2%~3.2%。     

一种下限为10~(-10)Pa·m~3/s的正压漏孔校准装置

为了解决漏率小于10~(-8)Pa·m~3/s正压漏孔(示漏气体为He气)的校准问题,研制出下限可达10~(-10)Pa·m~3/s的校准装置。提出基于累积比较的正压漏孔校准方法,通过向漏孔入口充入100 kPa高纯度N_2气模拟大气压环境,将漏孔泄漏后的示漏气体引入累积室经过一段时间的累积来提高浓度,采用膨胀衰减压力和分子流进样将混合气体引入质谱分析室,提出对质谱分析室中示漏气体进行累积模式的测量方法,通过四极质谱计作为比较器分别测量漏孔泄漏形成的混合气及配置的标准混合气体在累积模式下离子流的变化率得到漏孔漏率,解决了无法测量微小示漏气体离子流信号的技术瓶颈;采用全金属密封结构和特殊的工艺处理解决了累积室中延伸下限由于本底示漏气体的影响因素,采用体积小于1 mL的取样室通过直接取样和膨胀衰减压力取样获得与漏孔累积后形成同等数量的标准混合气体,解决了微小漏率正压漏孔校准所用标准混合气体获得。为此基于累积比较法的正压漏孔校准方法实现了10~(-8)～10~(-10)Pa·m~3/s的校准范围,合成标准不确定度不超过7. 5%。     

The Research of Anti-Wear Properties of Organomolybdenum Compounds in the Engine Oils

A four-ball tester was used to evaluate the anti-wear performance of three kinds of organomolybdemun compounds in the engine oils, i. e., molybdenum dialkyldithiophosphate (MoDDP), molybdenum dialkyldithiocarbamate ( MoDTC), and sulphur and phosphorus freeorganomolybdeum (Molybdate). The results indicate that a low concentration of MoDDP doesn' t improve the anti-wear properties of the commercial engine oils, but a high concentration of MoDDP can obviously improve the anti-wear properties and the load-carrying capacity of the engine oils. MoDTC doesn' t improve the antiwear properties of the engine oils, but worsens the anti-wear properties of the oils. Signifi can timprove ment of frictional and wear characteristics is obtained with Molybdate added in the commercial engine oils and the formulated oils.     

Certification Becomes Important for the I Quality; and Safety Supervision of the Chinese Liquor Sector

The end of 2007, over 200 unit products of more than 80 Chinese firms have passed the quality grade certification for liquor products. These products involve distilled spirits, beer, wine, yellow wine, fruit syrup wine and others, and cover over 80% of the national top-branded liquor products.……     

Deposition and Coating Properties on CVD Tungsten

Surface characterization and microstructure studies are performed on chemical vapor deposited (CVD) tungsten coating. There is about 2 μm thickness diffusion layer of tungsten in the molybdenum substrate. The thermal shock test shows tungsten coating has good adhesion with molybdenum substrate, but the elements of oxygen and carbon in the tungsten coating have the bad affection to the adhesion. The result of high-temperature diffusion experiment is the diffusion rate from molybdenum substrate to tungsten coating is faster.     

Analysis of marine hydrobiont lipid extracts as possible cryoprotective agents

We studied a combined effect of the cryoprotectants both of lipid and carbohydrate origin at the presence of DMSO or without it on cell viability and the RNA synthesis in the embryonic mollusc and echinoderm cell cultures obtained at different developmental stages. Cryoprotective properties of exogenous lipids correlated with their thermotropic behavior. Lipid extracts from marine hydrobiontes, which thermal transitions are characterized by relatively small part of calorimetric thermogram area lying at temperatures above 0 °C (6–18%), were found to possess a considerable cryoprotective activity. The results are discussed in relation to the prediction of the cryoprotective activity of lipid extracts for marine animal cells. In addition, it was found that marine invertebrate cells can be cryopreserved without DMSO at the presence of trehalose and lipid extracts of some marine hydrobiontes.     

Low-Temperature Properties of Silver

Pure silver is used extensively in the preparation of high-temperature superconductor wires, tapes, films, and other configurations in which the silver not only shields the superconducting material from the surrounding materials, but also provides a degree of flexibility and strain relief, as well as stabilization and low-resistance electrical contact. Silver is relatively expensive, but at this stage of superconductor development, its unique combination of properties seems to offer the only reasonable means of achieving usable lengths of conductor. In this role, the low-temperature physical (electrical, thermal, magnetic, optical) and mechanical properties of the silver all become important. Here we present a collection of properties data extracted from the cryogenic literature and, to the extent possible, selected for reliability.     

Early ironwork in Biscay: Survey,excavation, experimentation and materials characterization. An integral study of the mountainside ironworks (ferrerías de monte or “haizeolak”)

ABSTRACT

The production of iron in Biscay (Basque Country, Spain) has been a hallmark of this territory of the North of the Iberian Peninsula throughout its history. The Archaeology team of the Basque Country Mining Museum has spent 13 years, so far, studying the origins of this activity through the evidences left at the old pre-hydraulic iron production workshops known as mountainside ironworks (ferrerías de monte) or haizeolak. It has catalogued 170 archaeometallurgical sites of this type in Biscay, and the archeological excavation of some of them has led to the knowledge of the different stages of the production process that took place in these workshops. The team has also experimentally reproduced the work carried out in a mountainside ironworks from the High Middle Ages, and it has currently started the characterization process of this type of activity through the study of the collected materials.     

Mechanism Study on the Wear of CrAlTiN Coated High-Speed Steel Twist Drills Under Dry Cutting Conditions

As demands about environment protection are growing up, dry cutting technology is getting more and more concerns from all over the world. Main works performed here are study on dry cutting performances and wear mechanisms of M2high-speed steel (HSS) twist drills with CrAlTiN multicomponent coatings, which was deposited using magnetron sputter ion plating system, in drilling 45 and 30CrMnSiA steel, and their comparisons to those in drilling the same steel but using monolayer CrN and commercial TiN coated drills. Drilling performances of drills are evaluated mainly through the measurements of width on outer corner flank land and the cutting forces. Results show that performances of CrAlTiN coated drills are better than those of monolayer CrN and TiN coated drills. In drilling 45 and 30CrMnSiA steel, the average tool life of the CrAlTiN coated drills are 17.2 and 11.8 times higher than those of the uncoated drills. Observing wear of the drill with scanning electronic microscope, results show that there is no crack or spallation of the CrAlTiN coatings in wear zones. Main mechanism of the wear here is adhesion.     

Study on Bond Ability of Arc-Spraying Coatings with Different Surface Pretreatment on Cast-Iron

Arc spraying coatings are widely used in various applications, but uncommon in cast iron substrate. Different surface pretreatment technology is tested on substrates of gray cast iron. Surface roughness and residual stress were measured by TR200 and X-ray diffraction analyzer. Influence of different surface pretreatment methods ( dry blasting and fusebond) on roughness and residual stress was analyzed. The arc-sprayed coatings of wire 3Cr13 (φ2mm) on gray cast iron substrate is studied. The microstructure and interface of bonding layer were observed by SEM. The bond strength was taken by tensile test. Results show that bond strength with grit blasting is higher than fuse-bond; it is feasible to make wire 3Cr13 coating with arc spraying on cast iron substrate roughened by grit blasting.     

Structural Characteristics of TiO2 Ceramic Coating by Micro-Plasma Oxidation

TiO2 ceramic coatings with thickness of 20 μm were formed on the surface of pure titanium by micro-plasma oxidation. Their micro-structures were investigated by by using X-ray diffraction and their surface images were detected by using scan electronic microscope. There were three kinds of TiO2 coatings, pure anatase type TiO2 phase, mixed phases consisted of rutile type TiO2 phase and anatase type TiO2 phase, pure rutile type TiO2 phase. The coating surface with the pure anatase type TiO2 phase is rough, while the coating surface with the pure rutile type TiO2phase is smooth. The upper coating surface with the mixed type TiO2 phases is anatase type TiO2 structure and the subsurface of the TiO2 coating is rutile type TiO2structure.     

Evaluation of fatigue life of steel using steel grain size

The insightful discussion of the relationship between the construction of metallographic and fatigue life and proposition of mathematical relationships describing this relationship was conducted in the paper. This paper presents a method for estimating the fatigue life, based on the construction of the microstructural material taking into account the grain size and the participation of ferrite and pearlite phase.