Thermal Desorption Spectrometer with MS

带 MS 的热解吸光谱仪

• 批准号: 508420290
• 金额: --
• 依托单位: Universität des Saarlandes
• 依托单位国家: 德国
• 项目类别: Major Research Instrumentation
• 财政年份: 2022
• 资助国家: 德国
• 起止时间: 2021-12-31 至 无数据
• 项目状态: 未结题
• 来源: https://gepris.dfg.de/gepris/projekt/508420290?language=en
• 关键词: Thermal; Desorption; Spectrometer; MS

Hydrogen embrittlement of high-strength steels has been a known challenge for component design and fatigue strength of systems for more than 150 years. There are numerous examples of how hydrogen embrittlement has led to enormous damage and thus to high costs. As hydrogen will become more and more present in technical systems in the coming years due to the energy transition and a resource-efficient use of materials requires increasingly high-performance materials, the issue of hydrogen embrittlement will become essential. Particularly in the case of metallic materials, strength-increasing and thus more sustainable alloying concepts are making the materials increasingly susceptible to hydrogen degradation. The instrument is a multi-analyzer system for the determination of hydrogen (H), oxygen (O), nitrogen (N) and argon (Ar) concentrations especially in metallic samples. Concentrations down to the sub-ppm range can be resolved. In carrier gas melt extraction, samples weighing a few grams (depending on density) are melted in a temperature-controlled manner at temperatures up to 3500°C and the contents of the gases to be analyzed (O,N,H,Ar) released from the material sample into the carrier gas stream are determined. At the same time, hot carrier gas extraction can be carried out by means of an auxiliary infrared furnace at temperatures up to 1100°C. Compared to melt extraction, a significantly larger sample can be subjected to both a stepped and a continuous temperature profile with the aim of improving the measurement resolution. The gas concentration released as a function of temperature can then be used to infer the trapping energy of the gas to be analyzed or of the gas atoms in the metal lattice, the energy with which hydrogen is localized at lattice defects and which a hydrogen atom must overcome to leave the defect. This method is also known as "Thermal Desorption Spectroscopy" (TDS). When the TDS system is combined with a quadrupole mass spectrometer (MS) due to the highest measurement resolution required for diffusible hydrogen (dH) detection, the method is referred to as TDMS. TDMS is mandatory to measure the trapping energies of hydrogen at lattice defects in the metal atom lattice in a defect-specific manner. Neither TDS, TDMS or hot/melt extraction are accessible despite years of intensive hydrogen research at Saarland University (UdS) or in the scientific and industrial environment.

150多年来，高强度钢的氢脆一直是系统部件设计和疲劳强度的已知挑战。有许多例子表明氢脆如何导致巨大的损害，从而导致高成本。由于能源转型，未来几年氢将越来越多地出现在技术系统中，并且资源有效利用材料需要越来越高的性能材料，因此氢脆问题将变得至关重要。特别是在金属材料的情况下，增加强度和因此更可持续的合金化概念使材料越来越容易受到氢降解的影响。该仪器是一个多分析仪系统，用于测定氢（H），氧（O），氮（N）和氩（Ar）浓度，特别是在金属样品中。可以分辨低至亚ppm范围的浓度。在载气熔融萃取中，重量为几克（取决于密度）的样品以温度控制的方式在高达3500°C的温度下熔融，并确定从材料样品释放到载气流中的待分析气体（O，N，H，Ar）的含量。同时，可通过辅助红外炉在高达1100°C的温度下进行热载气提取。与熔融萃取相比，可以对大得多的样品进行阶梯式和连续式温度分布，以提高测量分辨率。然后，作为温度的函数释放的气体浓度可用于推断待分析气体或金属晶格中的气体原子的俘获能量，氢在晶格缺陷处局部化的能量以及氢原子必须克服以离开缺陷的能量。这种方法也被称为“热解吸光谱”（TDS）。当TDS系统与四极质谱仪（MS）结合时，由于扩散氢（dH）检测所需的最高测量分辨率，该方法被称为TDMS。TDMS是强制性的，以缺陷特定的方式测量氢在金属原子晶格中的晶格缺陷处的捕获能。尽管萨尔兰大学（UdS）或科学和工业环境多年来对氢进行了深入研究，但TDS、TDMS或热/熔体萃取都无法实现。