Non-evaporable Getter Research Articles

Pressure control of tritiated hydrogen isotopologues in hermetically sealed vessels by non-evaporable getters for sub-Doppler-resolution spectroscopy

Small molecules serve as valuable benchmarks for testing quantum chemical theories. Ultra-high-resolution spectroscopy currently offers the capability of measuring molecular hydrogen energy levels with a relative accuracy on the order of 10-10. Expanding such investigations to encompass different isotopologues of molecular hydrogen has emerged as a promising avenue for examining mass-dependent contributions to the full description of molecular structure in the framework of relativistic quantum electrodynamics. However, the delicate nature of handling radioactive tritium in a high-resolution spectroscopy environment poses significant technological challenges, thereby limiting the extension of these studies to include T2, DT and HT isotopologues. In this work, we present the experimental setup of the very sensitive, Doppler-free technique of Noise-Immune Cavity-Enhanced Optical Heterodyne Molecular Spectroscopy (NICE-OHMS), used to measure rovibrational transitions in the HT molecule. The NICE-OHMS measurements were performed in a closed cavity system without connection to an actively pumped vacuum system. For this reason, a new method for tritium storage and pressure regulation within 0.05–1Pa based on a temperature-controlled mini-getter system is employed using less activity than the tritium exemption limit (1GBq). Non-Evaporable Getters of the type SAES St171 were used for this purpose exploiting their property that hydrogen is released upon heating, while other gases remain being pumped. Prior to the NICE-OHMS experiment, the reversible sorption properties of the getter for hydrogen isotopes were investigated. We show measurements of the equilibrium (hydrogen) pressure for all three pure isotopes and for a H2:HT:T2 mixture (with H:T = 1:1) as a function of temperature for a system of defined volume and amount of gas. For the read-out of the temperature, a method using the resistance of the getter in combination with a pyrometric calibration has been implemented. We discuss the experiences from practical use of the tritium getter and show results obtained with the NICE-OHMS setup leading to frequency calibration of near-infrared transitions in HT at an accuracy, surpassing previous studies by nearly three orders of magnitude.

Laser scanning patterns induced surface properties variations of Ti-V-Hf-Zr non-evaporable getter film with 316L stainless steel substrates

The effects of laser treatment scanning patterns on the properties of Ti-V-Hf-Zr non-evaporable getter (NEG) film on 316L stainless steel (316L SS) substrates were analyzed. 316L SS substrates were laser-treated with different patterns, which resulted in spherical structure and protrusions on the surface of the substrates. Subsequently, Ti-V-Hf-Zr NEG films were deposited on ultrasonically cleaned laser-treated 316L SS by a direct current (DC) magnetron sputtering machine. Based on the XPS results of Ti-V-Hf-Zr, it has been revealed that the atomic proportions of film elements on the surface of samples #1-1∼#3–1 were about 2.2 (Ti):1.7 (Zr):0.9 (V):1.0 (Hf). In this paper, the Ar+-induced secondary electron yield (SEY) and surface resistivity of Ti-V-Hf-Zr NEG are discussed for the first time, and it has been observed that the laser treatment leads to an increase of the substrate surface roughness, which decreases the SEY and increases the surface resistivity.

Research on performance of porous scaffold-based getter activated by induction heating and its application in MEMS device

Non-evaporable getter (NEG) is widely used in vacuum packaging. However, there are two main contradictions. Firstly, the contradiction between bonding temperature of the device and activation temperature of the getter results in the getter being activated first and then packaged, and cannot be repeatedly activated, which seriously reduces the adsorption capacity and life of the getter. Secondly, the contradiction between the small package volume and the large adsorption capacity, how to integrate large adsorption capacity getter in a small space is a tricky problem. In view of the above contradictions, a porous scaffold-based getter activated by induction heating was proposed in this paper, results show that when nickel plating is used as the induction heating layer, the temperature can quickly rise to 700 °C within 10 s, and 1 μm Ti getter can be fully activated for 7 min. The good periodicity of the temperature curves proved that the nickel layer has good repeatable heating characteristics. In addition, the adsorption performance of the getter was tested and characterized at device level. The device level characterization of optical deflection method proves the effectiveness of induction heating to activate getter, which lays a foundation for the application of getter on MEMS devices.

Influence of the edge effect of the solenoid magnetic field on the discharge process of magnetron sputtering in long and narrow chambers

The fourth-generation light source or future particle accelerators have compact vacuum systems, resulting in a small flow conductance of the beam chamber. The development of NEG (Non-Evaporable Getters) films technology with distributed pumping is a good solution. This technology can obtain a pressure distribution with a small pressure gradient and an ultra-high vacuum of 10-8 Pa inside the vacuum chambers. In the magnetron sputtering process for NEG coating, the inhomogeneity of the magnetic field at the edge of the solenoid is a key parameter for affecting the stability of the magnetron sputtering discharge process. The influence mechanism of the edge magnetic field on the plasma discharge process and discharge uniformity was studied to optimize the coating parameters, which is very important. The Particle-In-Cell/Monte Carlo Collision (PIC/MCC) method was employed to simulate plasma discharge in a narrow vacuum chamber under various edge magnetic field conditions. The potential distribution, charged particle density distribution, and particle density distribution on the target were acquired for four sets of discharge parameters, followed by data processing and analysis. The electric field distribution during the discharge process is closely linked to the non-uniformity of the magnetic field at the solenoid's edge. The smaller Br (the radial component of the magnetic field) component of the magnetic field, the more uniform distribution of Ar+ on the target surface, and the smaller the difference along the length of the vacuum chamber. A smaller radial component (Br) of the magnetic field results in a more uniform distribution of Ar+ on the target surface and reduces variations in film thickness along the length of the vacuum chamber. This is attributed to the small distance between the inner wall of the vacuum chamber and the cathode target. The change in the edge magnetic field will result in the rapid migration of electrons to the inner wall of the vacuum chamber and insufficient collision with the discharge gas, making it challenging to sustain the discharge process. Moreover, fluctuations in the edge magnetic field of the solenoid induce gradient drift and curvature drift in charged particles, resulting in rapid electron loss and alterations in the density and potential distribution of charged particles at the ends of the vacuum chamber, ultimately leading to discharge instability. The research results show the importance of the edge magnetic field effect on the magnetron sputtering coating of the slender vacuum chambers, which provides an important reference for the segmented coating process of similar vacuum chambers in future accelerators.

Construction of SuperKEKB vacuum control system and its eight years operation experience

SuperKEKB has two main rings (MRs), namely low- and high-energy rings, with circumferences of 3 km; beam transport (BT) lines; and a positron damping ring (PDR). We upgraded the MRs and BT line vacuum control systems and designed a new PDR vacuum control system for upgrading KEKB to SuperKEKB.Here, we describe the basic configuration of the vacuum control system, which includes the interlock logic (gate valve open/closed control, non-evaporable getter pump activation, and beam abortion). We subsequently present the collimator driving system and the cooling water control system for the beam pipe of the final focusing superconducting quadrupole magnet as examples of special SuperKEKB vacuum control systems. Examples of problems in the SuperKEKB vacuum control system, including the discharge at the high-voltage connector of the ion pump, stoppage of the cooling water pump for the vacuum system, and failure of the collimator position measurement device are described.

Study on hydrogen absorption performance of the modified Zr/ZrVFe porous getters

Non-evaporable getter is used to remove active gases in sealed-off vacuum devices, especially H2 at room temperature. In this work, Zr/ZrVFe getters with different Zr content (0, 30 and 50 %) were fabricated using vacuum sintering method, then futher improvement of pumping properties had been explored with Ni overlayer as deposited on the surfaces of Zr/ZrVFe getter by magnetron sputtering technique. Subsequently, residual gas and pressure change during the activation process of Zr/ZrVFe getters were measured. It was found that when the activation temperature reached 350 °C, the desorption of impurity gases was basically completed, there was only H2 in the system. Moreover, the hydrogen absorption properties of the Zr/ZrVFe getters modified by Zr content and Ni overlayer were examined. Results indicated that the sintered ZrVFe getter with 0 % Zr content had a large number of cracks and occurred the phenomenon of falling powder, Zr30 %/ZrVFe getter had better hydrogen absorption properties in comparison with Zr50 %/ZrVFe getter owing to the larger porosity and specific surface area. Ni had the catalytic characteristics of decomposing molecular hydrogen into hydrogen atoms and Ni film was uniformly covered on the getter surface, the hydrogen absorption properties of Zr/ZrVFe getter with Ni overlayer were significantly improved.

Unveiling the secrets of non-evaporable getter films: Activation temperature, activation time, and achievable activation degree

Non-evaporable getter films play an important role in the creating and maintaining of high or ultra-high vacuum environments in advanced scientific disciplines. Prior to application, thermal activation in a vacuum environment is essential. Despite numerous attempts to reduce the film activation temperature, uncertainty remains as to whether extending the activation time at a relatively lower activation temperature will ensure a fully-activated state of the film. To address this issue, the microstructure and activation performance of the film has been investigated. Techniques, such as scanning electron microscopy, grazing incidence X-ray diffraction, energy dispersive spectroscopy, and in-situ X-ray photoelectron spectroscopy were employed. Experimental investigations show that a fully-activated state of the film cannot be achieved at around 150°C, regardless of the activation time. Further analysis shows that, at activation temperatures below about 200°C, the migration trend of oxygen atoms within TiZrV/TiZrHfV films exhibits asynchronous features. This process was accompanied by boundary effects of foreign atom migration channels. In addition, the achievable activation degree of the film shows a step characteristic. These results improve the understanding of the relationship between activation temperature, activation time, and the achievable activation degree of the film.

Design and implementation of intelligent control system for non-evaporable getter pumps

Abstract An intelligent control system for Non-Evaporable Getter (NEG) pumps was designed and developed. The main functions of the system include remote monitoring and remote control of key parameters of the NEG power supply, intelligent control of NEG working status according to NEG saturation status and vacuum chamber status, especially intelligent warning and protection of NEG from vacuum leaks and NEG supersaturation. The intelligent control system is proven stable and reliable, which provides a feasible logic architecture and control design for NEG pump application in future fusion devices.

Investigation on activation characterization, secondary electron yield, and surface resistance of novel quinary alloy Ti–Zr–V–Hf–Cu non-evaporable getters

The performance of next-generation particle accelerators has been adversely affected by the occurrence of electron multipacting and vacuum instabilities. Particularly, minimization of secondary electron emission (SEE) and reduction of surface resistance are two critical issues to prevent some of the phenomena such as beam instability, reduction of beam lifetime, and residual gas ionization, all of which occur as a result of these adverse effects in next-generation particle accelerators. For the first time, novel quinary alloy Ti–Zr–V–Hf–Cu non-evaporable getter (NEG) films were prepared on stainless steel substrates by using the direct current magnetron sputtering technique to reduce surface resistance and SEE yield with an efficient pumping performance. Based on the experimental findings, the surface resistance of the quinary Ti–Zr–V–Hf–Cu NEG films was established to be 6.6 × 10−7 Ω m for sample no. 1, 6.4 × 10−7 Ω m for sample no. 2, and 6.2 × 10−7 Ω m for sample no. 3. The δmax measurements recorded for Ti–Zr–V–Hf–Cu NEG films are 1.33 for sample no. 1, 1.34 for sample no. 2, and 1.35 for sample no. 3. Upon heating the Ti–Zr–V–Hf–Cu NEG film to 150 °C, the XPS spectra results indicated that there are significant changes in the chemical states of its constituent metals, Ti, Zr, V, Hf, and Cu, and these chemical state changes continued with heating at 180 °C. This implies that upon heating at 150 °C, the Ti–Zr–V–Hf–Cu NEG film becomes activated, showing that novel quinary NEG films can be effectively employed as getter pumps for generating ultra-high vacuum conditions.

Comparison of two vacuum system technologies for the synchrotron storage ring: case study of Iranian Light Source Facility

The current study compares two vacuum system designs for the Iranian Light Source Facility (ILSF) storage ring: conventional vacuum system design with stainless-steel vacuum chambers that are pumped by Non-Evaporable Getter (NEG) cartridges and ion pumps. In this design, all synchrotron radiation is absorbed by the local photon absorbers. In the second design, the water-cooled copper tubes that are coated with NEG materials are used as the vacuum chambers. This study will illustrate the advantages of using the NEG-coated vacuum chambers over the conventional design with the stainless-steel chambers. Since the two designs for ILSF are now completed, some of the details of this comparison might be interesting to other light sources, especially those that have plans to upgrade to a 4th generation.

Vacuum chambers for Swiss Light Source arcs

The vacuum chambers for diffraction limited storage ring differ from the previous storage rings generation in three main aspects: the cross-section dimension, which is divided by a factor of 2 or more to fit smaller magnet apertures; the material, which includes much more copper for heat dissipation and to limit resistive wakefields; the coating of the inner surface with a nonevaporable getter (NEG) to ensure good pumping level despite low conductance. This paper gives a detailed description of the vacuum chambers’ design used in the arc section of SLS 2.0, starting with conceptual design choices based among others on synchrotron radiation heat and wakefield considerations. The particular case of the main bending magnet vacuum chamber is explained in detail from design to manufacturing, including the development of an appropriate NEG coating procedure. Finally, the overall assembly of a 17 m long arc, its activation to reach pressure in the 10−11 mbar range followed by transport and installation into the magnets is presented. This validates the choice of activation for an arc vessel made out of copper, with wall thicknesses as small as 1 mm and with less than 0.5 mm clearance to magnet poles. Published by the American Physical Society 2024

In situ effective pumping speed measurements as a tool for non-evaporable getter activation and saturation monitoring

We have developed method of in situ effective pumping speed measurements based on injecting finite gas pulse into a vacuum volume and subsequent recording of pressure response using a Residual Gas Analyzer (RGA). The pressure burst caused by injected gas pulse falls exponentially in time and the exponential coefficient of such pressure decay is proportional to total effective pumping speed of all vacuum pumps acting on vacuum chamber volume. The effective pumping speed can be extracted from the dependence of injected gas species pressure vs time recorded by an RGA. Non-Evaporable Getters (NEGs) are widely used in multiple ultra and extremely high vacuum devices and applications during the last several decades. Areas of NEG applications were recently expanded into vacuum devices with relatively high-pressure levels (up to 10−7 Torr) by the invention of high capacity ZAO NEG which can be operated at elevated temperatures. The intrinsic property of all NEG-based vacuum pumps is the reduction of their pumping speed, called “NEG saturation”, after an extended period of operation. Typical time interval for such process can span from about a month and up to a few years depending on NEG type, vacuum level of NEG pump operation, and residual gas content. After that, the NEG pump will require a re-activation cycle to restore its pumping speed close to the initial value. For many applications it is difficult to realize what is the current pumping speed of NEG pump is and when the pump should be re-activated. A method for in situ effective pumping speed measurements developed in this study can be used as a tool for NEG-based pump activation and saturation monitoring. Application of such an approach to monitor pumping status of NEG pumps was utilized and will be continually used at Extended EBIS which was recently developed and commissioned for Relativistic Heavy Ion Collider (RHIC) and future Electron Ion Collider (EIC). The results obtained during commissioning are presented and discussed.

First results of non-evaporable getter pump studies for the application in the EAST tokamak

Enhanced particle exhaust is pivotal in optimizing fuel recycling and bolstering plasma performance within fusion reactors. Non-Evaporable Getter (NEG) pumps, renowned for their robust high-temperature tolerance, high pumping speeds and large adsorption capabilities, emerge as highly promising candidates for augmenting the particle exhaust efficiency of tokamaks. Rigorous evaluations have been undertaken to ascertain their pumping efficacy within a vacuum testing setup and the EAST tokamak environment. Experimental data have consistently demonstrated that NEG pumps maintain stable operation across a broad temperature range, from ambient conditions to 200 °C, with a notable direct correlation observed between the pumping speed and the ambient temperature. Their performance surpasses that of conventional cryopumps, especially at D2 gas pressures exceeding 0.1 Pa. Additionally, the application of nitrogen passivation has been validated as an effective method to modulate the pumping speed and to mitigate the risk of hydrogen embrittlement and oxygen and carbon contaminations. Despite exposure to the extreme operational demands, including 30 h of plasma exposure, and lithium processing, atmospheric conditions, and water leaks, the NEG pumps preserved approximately 70 % of their initial pumping capacity. These results underscore the compatibility of NEG pumps with the challenging environments of plasma operations, positioning them as a viable and promising solution for particle exhaust in the next-generation fusion reactors.

Effect of Adding Al on the Phase Structure and Gettering Performance of TiZrV Non-Evaporable Getter Materials.

Titanium zirconium vanadium (TiZrV) is a widely used non-evaporable getter (NEG) material with the characteristics of a low activation temperature and a large gas absorption capacity. At present, the research on TiZrV getters mainly focuses on the thin-film state, with little research on the bulk state. In this paper, a TiZrV getter was optimized by adding Al, and the phase structure, activation properties, and gettering performance were studied. With the addition of Al, the α-Zr phase and Ti2Zr phase changed into the Ti-Zr phase and Al-Zr, Al-Ti phase. The newly generated phase promoted the diffusion of hydrogen and oxygen atoms. The activation temperature decreased significantly, as shown in the in situ XPS results. The H2 and CO gettering performance of TiZrVAl samples was promoted to 2073 cm3·s-1 and 1912.8 cm3·s-1, increased by 40.7% and 40.3%. This paper provides valuable ideas for optimizing the properties of bulk TiZrV getters.

Terahertz scale microbunching instability driven by high resistivity nonevaporable getter coating resistive-wall impedance

Terahertz scale microbunching instability driven by high resistivity nonevaporable getter coating resistive-wall impedance

Characterization of a NEG cartridge under high pressure conditions

The development of advanced sintered pumping elements based on the ZAO® alloy, characterized by a high affinity towards hydrogen and its isotopes, make Non Evaporable Getter (NEG) pumps particularly appealing for applications in fusion research, which typically deal with large fluxes of these gaseous species. NEG getters show high pumping speeds and capacity, excellent reliability with ability to withstand a high number of loading and unloading cycles without showing any type of failure, ease of integration within a complex system (such as a fusion reactor) because of their high specific properties and the simplicity of the mechanism that regulates its operation. These properties make NEG technology particularly suitable for the development of compact, efficient and easily scalable solutions, which are also very safe, since the release of absorbed hydrogen is prevented in the case of power outage or subsystem failures, as it can occur only by providing an adequate amount of heat to the getter material. This paper reports the results of an experimental campaign conducted on a new type of NEG pump, aimed to obtaining an accurate characterization in response to different operating conditions. Hydrogen pumping speed was investigated in a range of pressures of particular interest for the activities of the Divertor Tokamak Test facility (between 0.1 and 10 Pa). The influence of nitrogen absorption and getter material operating temperature on the pumping performances of the NEG pump were also examined. Finally, numerical simulations have been performed to estimate the nominal pumping speed of the NEG pump, that is, the one acting at the absorbing surface, stripped of the effects of the conductance of the paths from the pump NEG to the pressure gauges.

Controlled adsorption of gas molecules by tuning porosity of titanium film

Within microelectromechanical system sensors, the establishment of a vacuum environment is a prerequisite for the control of specific residual gas molecules. At the wafer-level package stage, the interior of the sensor can be easily converted into a vacuum environment. However, after packaging, degassing occurs due to the accumulation of fumes with additional processing, resulting in a significant reduction in sensor reliability. To counteract this, non-evaporable getter (NEG) film is commonly packaged together with the sensor to absorb the outgassing gas molecules and maintain a vacuum environment within the sensor. Most NEG films require an activation process to migrate the adsorbed gas molecules from the surface to the bulk by thermal annealing. Recently, NEG films have been considered to reduce the activation temperature and time to avoid heat damage. Depositing an anti-oxidant layer on NEG film or alloying the NEG film with metallic materials through co-sputtering to create a distinct valence state during activation was found to prevent further oxidation of NEG film. However, these methods require expensive materials and fabrication equipment. In this study, we demonstrate that a much lower activation temperature (T = 350 °C) and time (t = 10 min) for Ti NEG film can be achieved by controlling the surface morphology depending on the deposition method and condition, without requiring further treatment such as the deposition of a capping layer or co-sputtering. Increasing the grain size of the Ti NEG film results in a larger surface area, which enables more efficient adsorption of gas molecules. Additionally, higher porosity in the film increases the diffusion of gas molecules, thus enhancing the overall gas adsorption capacity. Our experiments show that the Ti NEG film, which was deposited at 7.8 Å s−1 using a sputtering method, exhibited a grain size of 411 nm and a surface roughness of 59.185 nm. Furthermore, after an activation process at 350 °C for 10 min, the atomic ratio of the adsorbed gas molecules was 23.14%.

Preliminary evaluation of NEG materials in view of CMSB replacement in HCPB TER architecture

CMSB (Cryogenic Molecular Sieve Beds) operated at 77 K is used for tritium recovery in the reference design of HCPB (Helium Cooled Pebble Bed) TER (Tritium Extraction and Removal) system. However, this technology has two main drawbacks: large consumption of liquid nitrogen and the controlling of tritium stream sent to the Tritium Plant, during the regeneration of the CMSB, in such way to avoid large variations in the gas flow rate.This paper reports on a preliminary evaluation for CMSB replacement by non-evaporable getter materials for tritium recovery. The advantages of NEG technology are the high specific pumping speed and capacity and the ability to withstand a large number of absorption/desorption cycles. In addition, NEG do not release hydrogen unless power is supplied to heat them, addressing an important safety issue related to uncontrolled release in case of power outage or subsystem failures.

A new NEG coating setup with travelling thin solenoids for the SLS 2.0 complex vacuum chambers

The 288 m long Storage Ring of Swiss Light Source 2.0 (SLS 2.0) consists of several vacuum chambers with unique geometries. Complicated features, with many changes in the cross sections, are essential to provide the best impedance matching, and to allow synchrotron light extraction under the tight geometrical constraints. In order to speed up the commissioning time, it was decided to coat most of the vacuum chambers with non-evaporable getter (NEG) material. A new magnetron sputtering setup has been developed in Paul Scherrer Institut (PSI), where the plasma length, defined by thin solenoids, is relatively small. The solenoids are continuously travelling over the entire vacuum chambers more than hundred times per coating process with an average speed of 4 mm/s to assure the best possible thickness uniformity and to limit the cathode heat up. Flexibility provided by this solution allows to coat various vacuum vessels in one assembly. This paper will describe this NEG coating setup and show results on SLS 2.0 vacuum chambers.

Elettra 2.0: The Vacuum System Design for a New Generation Storage Ring

Next-generation synchrotron facilities currently under development and construction are promising and delivering great advances in terms of machine design and research physics. At the same time, they are pushing the limits of technological solutions for various subsystems: to achieve the desired ultra-low electron beam emittance required in the next generation machines, the magnetic lattice has to adopt a compact design with reduced magnet apertures and other constraints like high heat load from synchrotron radiation, dynamic pressure inside vacuum chambers and chamber wall impedance are presenting unique challenges for the vacuum and engineering teams. At Elettra-Sincrotrone Trieste (Italy), the Elettra 2.0 project aims to develop a new-generation storage ring. Taking into consideration the above-mentioned constraints, we decided to adopt a new design of a vacuum chamber, while utilizing novel pumping solutions to overcome hugely reduced conductance compared to the current machine. Large sputter ion pumps (SIP) will be in the majority replaced by distributed non-evaporable getter (NEG) coatings and small NEG cartridges and SIP pumps. For the synchrotron radiation handling, due to the tight space constraints imposed by the compact lattice, the photon absorption will be managed jointly with discrete and distributed solutions: photon absorbers have been carefully studied for combining compact form and high power density loads, while key sections of the new storage ring will be water-cooled. Throughout the whole development phase, we were using Monte-Carlo simulation codes like SynRad and MolFlow+ as effective tools supporting the design of new vacuum chambers and photon absorbers. The current state of development for the Elettra 2.0 vacuum system, the challenges we faced and the solutions we adopted are presented here.