Comparative Study on the Outgassing Rate of Materials Using Different Methods

With so many material outgassing test methodologies, three of them were available at Academy of Opto-Electronics, which are the pressure rise method (PR), the throughput method and the switching between two pumping paths method (SPP). In order to compare the data derived via different methods and decide the proper concept to conduct a test, outgassing experiments of two pumping speeds with various periods were performed on one material using three methods, following the tool’s detection limit was demonstrated at first. The results reveal that a lower outgassing rate is achieved with longer evacuation time and a higher pumping speed. What’s more, a quite smaller value is obtained by the PR method against the other two, and the SPP method gets a little lower one as opposed to the throughput. Additionally, it is concluded that the PR method, with one simple chamber, is relatively more suitable for measuring high outgassing-amount materials, while the sample with lower one is more preferable to use the throughput or SPP method, which has a more complicated structure in contrast. However, different from the second approach, a little higher uncertainty may be acquired by the third method, in spite that it has the lowest detection limit.     

不同处理方法下铁氧体出气性能的研究

为减少加速器束流快引出元件铁氧体材料真空出气量,对铁氧体材料进行真空除气、镀膜以及烘烤工艺处理。采用旁路切换法(SPP)测量不同处理条件下的出气率。结果表明,铁氧体材料经真空除气后镀TiN膜,在测试罩中经烘烤,冷却后充氮气测得的出气率最低。     

Investigation of a set procedure for the stability of pressure control in the newly developed flow-control system at KRISS

Korea Research Institute of Standards and Science (KRISS) has assembled a new flow-control system (FCS-705) for the study of advanced applications and calibration of different types of vacuum gauges by comparison method. This report details the measurement of the outgassing rate of the main vacuum chamber by the pressure rate of rise method. Constant pressure was generated inside the vacuum chamber by employing a dynamic flow control method. Nitrogen gas flow data was recorded to demonstrate that constant pressure was controlled in the vacuum chamber. The measurements were performed in a sequence of increasing pressures.     

基于双通道方法对不锈钢高温出气性能的研究

采用双通道(SPP)方法对不锈钢材料在高温条件下真空出气性能进行研究。该方法能将传统动态法中真空测量元件对被测量材料出气速率的影响消除,提高测量精度;并通过SPP结构,在数据处理过程中只采用一只规管的真空度读数,避免规管的个体差异带来的计算误差。利用此方法测量了不锈钢材料的高温出气速率,并对比经过真空烘烤后充空气和充干燥氮气的出气性能差异。     

材料在真空环境下放气的测试技术研究

往真空材料放气率测试装置上对金属材料的放气特性进行了实验研究,实验采用的方法为静态升压法、固定流导法、双通道气路转换法。实验结果表明,测试装置的极限真空度为9．2×10^-9Pa,铜、铝合金2A12、304不锈钢三种材料半小时后的放气率分别为2．34×10^-8a·m^3·s^-1·cm^-2、1．83×10^-9Pa·m^3·s^-1·cm^-2、8．48×10^-11Pa·m^3·s^-1·cm^-2。利用四极质谱计测得装置的本底气体成分主要有H2、N2／CO、H2O和CO2,材料放出的气体成分主要有N2／CO、H2O。三种方法测试得到的铜金属材料的放气率随着温度的升高而小断增大。     

高真空条件下网状泡沫放气量的测试

利用航天工业行业标准及测试设备对一定真空度条件下的聚胺脂网状泡沫在常温及加温两种不同工况时的出气情况进行测试；对两者的放气量进行比较；对放气机理进行分析探讨。此工作对高真空连续卷绕网状泡沫镀镍设备的真空系统配置具有一定的指导意义。     

Gas dynamics modelling for particle accelerators

Design of an accelerator vacuum chamber requires an input from different scientific disciplines such as surface science, material science, gas dynamics, particle beam dynamics, and many others. Although vacuum scientists work on the boundary field between these disciplines, gas dynamics is the one that allows joining them to the vacuum science for particle accelerators. The vacuum requirements (usually UHV or XHV) in particle accelerators are defined by beam-gas interactions that should be negligible compared to other phenomena that limit the quality of the beam. At such low pressures the main source of gas in the vacuum chamber is a molecular desorption from materials used for the vacuum chamber and its components. The outgassing rates vary over a very wide range and depend on material, cleaning procedure, treatments, temperature, bombardment by particles and accumulated irradiation dose. The gas dynamics is used to design the research facilities to accurately measure and to study outgassing rates at different conditions. By applying these data to the accelerator vacuum design, one would have to consider that outgassing is often non-uniform and changes with time with different functions. The most time-efficient way of beam vacuum optimization is using a 1D diffusion model where all parameters are defined as a function of longitudinal coordinate (along the beam path). A full 3D modelling with TPMC codes provides much more accurate results, however, being time consuming work is not ideal for pumping and design optimization and is used for complex components and for finalized design.     

HL-2M装置真空室预抽气系统的研制

通过搭建HL-2M真空室整体预抽气系统,对真空室的设计、加工和安装工艺是否达到超高真空技术要求进行了试验检测.采用三套分子泵机组和一套低温泵机组作为主抽系统,对HL-2M真空室进行了预抽,72小时后真空室真空度达到3.7×10-5Pa,超过了预期的预抽真空度.在本底真空度为3.7×10-5Pa的条件下采用静态定容法测试...     

High-speed pumping to UHV

Development of a high-speed pumping system for ultra high vacuum (UHV) process dose not reduce only cost and waiting time for experiment and production, but also reduces CO₂ emission that is known as one of the serious causes in the global warming problem. Reduction of vapor water concentration in a purge gas line would be one of the most effective measures to reduce pumping time to UHV. We carried out control of water vapor in a nitrogen gas purge line in addition to surface treatments of chambers using buff polishing and electrolytic polishing, followed by measurement of outgassing rate of the chambers. Under the reasonable control of the water vapor, the pumping time to reach the pressure of 1 × 10⁻⁶ Pa was able to be shortened with two orders of the magnitude. And it was also found that the main residual gas in the chamber was hydrogen after pumping down with the low concentration of water vapor. The quality of residual gas was equivalent to the quality in a baked UHV system. The introduction of well controlled nitrogen gas to the vacuum system which was not baked out during its pumping has proved a pressure of 3 × 10⁻⁸ Pa for 24 h in the chamber without orifice.     

Static expansion vacuum standard with extended low pressure range

The main factor to affect lower limit of static expansion vacuum standard is outgassing of the inner surface. A new method has been demonstrated to extend the lower limit by using a non-evaporable getter pump (NEGP) to eliminate the outgassing influence. Because NEGP has no pumping speed for inert gases, it can maintain the ultra-high vacuum background without changing gas quantity in the calibration chamber when an inert gas is used as the test gas, which makes the standard pressure accurately calculable by Boyle’s law. By this method, the lower limit of static expansion vacuum standard has been extended to 10⁻⁷ Pa.     

Dynamic extension - A new principle for a vacuum primary standard for UHV-range (10-10 Pa) calibration of hot cathode ionisation gauges

The main obstacle in the construction of primary vacuum standards for very low pressures - ultra-high vacuum (UHV) - is outgassing from the walls of the apparatus. Thus, principles utilising a higher pumping rate in the calibration chamber, e.g., the pressure ratio technique, seem to be more useful for this range. However, a serious problem is inherent in this method, namely, that the gas in the calibration chamber is not in equilibrium and thus cannot be characterised by a single scalar pressure value, although such a value is then used to evaluate the measurement. This discrepancy can be overcome by using a hot cathode ionisation gauge as a transfer standard calibrated by the dynamic extension method.The dynamic extension method is explained and compared with the pressure ratio technique. The basic conditions for achieving acceptable uncertainty values are considered.     

绝热材料放气速率测试台研制

高真空条件下,绝热材料的放气速率会影响低温容器的真空性能,从而影响其绝热性能。根据GB/T31480-2015,搭建了绝热材料放气速率测试平台。通过本底放气速率的测定,验证了该测试平台的可靠性;利用静态法测试了某型号多层绝热材料的放气速率,给出了试验数据。本试验台将为绝热材料的应用及低温容器的设计提供数据支撑。     

固定流导法校准真空漏孔方法研究

固定流导法采用的是分压力测量技术,对质谱分析室的漏放气率的指标要求不高.通过实验得到四极质谱计的非线性引起的测量误差可达38%,在具体校准过程中能够很好调节稳压室中的气体压力,使通过小孔的气体流量与待校真空漏孔漏率非常接近,从而避免了四极质谱计的非线性影响.稳压室中的气体压力比较大,所以稳压室不需要特别严格的材料处理工艺,具体校准过程中也不需要彻底的烘烤出气就能得到纯净的单一气体.固定流导法校准真空漏孔的不确定度的评定值为2.6%,可以通过精确校准电容薄膜规和控制温度来进一步降低漏孔校准的不确定度.     

An UHV system to study gassing and outgassing of metals under friction

An UHV dynamic expansion system to study gassing and outgassing of metals under friction in vacuum has been developed. The vacuum chamber of the system has two main parts separated by a wall with a central orifice of nominal conductance of 5.27 l s⁻¹ for N₂ at 300 K. The main part of the system is equipped with a quadrupole mass-spectrometer, ion gauge and the gas line supply. The chamber closer to the pumping systems is also equipped with an ion gauge. The pumping of the system is performed by: (I) a turbomolecular and (II) a cryogenic pump, which can operate either independently or in parallel. The ultimate pressure of chambers 1 and 2 are respectively 5.2.10⁻¹¹ mbar and 1.10⁻⁹ mbar. The friction cell allocated in chamber 2 consists of a sample holder and a linear motion feedthrough with a steel ball indent allows the friction experiments. The sample holder lets to apply a load to the sample surface with a normal force in the range of 0,02 N to 0,85 N. Heating of the sample up to 500°C is provided by electron bombardment. The temperature of the sample as well as the electrical resistance between the indent and the sample surface can be measured. The results show that pressure increase caused by the deformation of the sealing bellow of the friction cell, i.e. without friction, is 1.7×10⁻¹¹ mbar (0.6% of the base pressure). The outgassing of the sample caused by friction depends on the normal force as well as on the sweep frequency. The behavior of the total pressure is characterised by an oscillating current supported on a continuous current, which is not possible to explain at present time.     

基于分子流传感元件的真空腔体漏率测量方法

本文介绍了一种基于分子流传感元件的真空腔体漏率测量方法,该方法通过分子流传感元件测量真空腔体整体漏率,采用的测量装置由气体流量测量系统、真空抽气系统、恒温系统等部分组成.在测量系统中,流经传感元件的气流处于分子流状态,通过测量传感元件两端的差压,计算质量流量,可以得到真空腔体的整体漏率.实验中对多个真空腔体漏率的测量结...     

Uncertainty analysis of the high vacuum part of the orifice-flow-type pressure standard

The orifice-flow-type pressure standard is commonly accepted as primary standard for vacuum gauge calibration in the high vacuum gas pressure range. It consists of two parts—a high vacuum part and a flowmeter. Practical questions arising at design of the standard have to be answered based on the standard uncertainty analysis.The analysis of the uncertainty sources in the high vacuum part except deviations from the Maxwellian distribution is given in the paper. Uncertainty of a precise flowmeter is taken from references for comparison. It follows from the analysis that uncertainties caused by some sources at routinely achievable parameters are negligibly small and further improvement brings no benefit. The crucial quantities influencing the total uncertainty are the temperature of the chamber and the flowmeter, the outgassing rate from the inner surfaces, the ultimate pressure of the pump and the additional (detrimental) pumping speed. The pumping speed of the main pump has to be “sufficiently higher” than the orifice conductance.     

Wasserstoff in Hochvakuumsystemen mit Turbomolekularpumpen bei verschiedenen Vorpumpen

The combination of diaphragm pumps with wide‐range turbomolecular pumps constitutes a small but powerful oil‐free high vacuum pumping system. Turbomolecular pumps show gas dependent compression ratios, the lowest for hydrogen. Thus, the high vacuum can be governed by the hydrogen partial pressure. In the present investigation the residual gas composition of a turbomolecular pump and different backing pumps shows no improvement if diaphragm pumps with low ultimate pressure are replaced by rotary vane or Roots pumps. In this case the ultimate pressure in the high vacuum chamber is basically determined by the ratio of outgassing to pumping speed and not by the product of compression ratio and backing pressure. However, the hydrogen partial pressure increased if the ultimate pressure of the diaphragm pump was raised. At a backing pressure of 0.5 mbar the high vacuum reached a stable value not improvable by reduction in backing pressure.     

真空钎焊系统内材料出气对压升率的影响研究

随着微电子封装向小型化、高密度化、高可靠性的方向发展,各行业对钎焊技术提出了高钎透率、高钎焊接头质量、材料具备高净化度等需求.高真空钎焊技术也随之日益普及、加速发展.该技术通过保障真空室的洁净度及焊接真空度,进而保障元器件的焊接质量及寿命.高真空钎焊技术要求真空钎焊炉具备高真空度、低压升率.高温下材料出气是高真空状态下...     

Measuring volume ratios of vacuum vessels using non-evaporable getters

Several methods have been used in vacuum metrology for volume determination. Volume ratios can be determined by different gas expansion methods, which were primarily developed for the precise determination of expansion ratios in static expansion systems. Measurements of the volume ratios using the gas expansion methods below 10⁻² Pa are influenced by outgassing from chamber walls. To reduce outgassing in the expansion chambers during measurements at low pressures, we have installed non-evaporable getter (NEG) pumps, which pump hydrogen and other active gases but have a negligible pumping speed for inert gases. The volume ratio of two chambers of an experimental static expansion system has thus been measured using the inert gases argon, helium and krypton. The obtained results were compared with the measurements without the use of an NEG pump. Measurements of the pressure ratios were performed with a spinning rotor gauge (SRG).     

Das Saugvermögen von Pumpen: Untersuchung verschiedener Meßverfahren im Grobvakuumbereich

The term pumping speed of a vacuum pump denotes the volume flow rate of gas removed by the pump. In a measurement of the pumping speed it has to be taken into account that the volume of a quantity of gas depends on pressure and temperature. The present article presents a critical investigation of two different procedures for measuring the pumping speed in the rough vacuum regime: In the first procedure, gas flows continuously through the test dome and the pump under investigation. The pumping speed is obtained from the stationary values of throughput and pressure in the test dome. This procedure is well established, technical details are described in various standards. In the second procedure, a large vessel with known volume is evacuated by the pump, and the pumping speed is derived from the pressure decrease with time. In order to avoid disturbances by thermal effects, the vessel may be pumped only during short time intervals with intermediate waiting for thermal equilibrium. The second procedure offers instrumental advantages and its practices are described in a new DIN standard. The physical basis and technical aspects of both procedures including disturbing thermal and other effects are investigated. If applied correctly at inlet pressures in the rough vacuum range, both procedures are expected to yield the same values of the pumping speed. Comparative measurements at a diaphragm pump confirm this expected behaviour within the experimental uncertainty of about 3% (2σ).