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Tungsten as a chemically-stable electrode material on Ga-containing piezoelectric substrates langasite and catangasite for high-temperature saw devices
Thin films of tungsten on piezoelectric substrates La3Ga5SiO14 (LGS) and Ca3TaGa3Si2O14 (CTGS) have been investigated as a potential new electrode material for interdigital transducers for surface acoustic wave-based sensor devices operating at high temperatures up to 800 °C under vacuum conditions. Although LGS is considered to be suitable for high-temperature applications, it undergoes chemical and structural transformation upon vacuum annealing due to diffusion of gallium and oxygen. This can alter the device properties depending on the electrode nature, the annealing temperature, and the duration of the application. Our studies present evidence for the chemical stability of W on these substrates against the diffusion of Ga/O from the substrate into the film, even upon annealing up to 800 °C under vacuum conditions using Auger electron spectroscopy and energy-dispersive X-ray spectroscopy, along with local studies using transmission electron microscopy. Additionally, the use of CTGS as a more stable substrate for such applications is indicated.
Capability study of Ti, Cr, W, Ta and Pt as seed layers for electrodeposited platinum films on γ-Al2O3 for high temperature and harsh environment applications
High temperature surface acoustic wave sensors based on radio frequency identification technology require adequate antennas of high efficiency and thermal stability for the signal transmission. Platinum is well known and frequently used as a material of choice for high temperature and harsh environment applications because of the high melting point and its chemical stability. Therefore, one way to realize high temperature stable antennas is the combination of a Pt metallization on an Al 2 O 3 substrate. As a cost-effective technique, the Pt film is deposited via electrochemical deposition. For this growth procedure, a pre-deposited metallization on the Al 2 O 3 layer is required. This paper analyzes the influence of various seed layers (Ta, Ti, W, Cr, Pt) on the morphology, stability and electrical properties of the electrochemically-grown Pt thick film after heat treatments up to 1000 ∘ C in air. We find an oxidation of all adhesion layers except for Pt, for which the best electrical properties were measured. Although significant areas of the films delaminate from the substrate, individual anchor structures retain a stable connection between the Pt layer and the rough Al 2 O 3 substrate.
Study of TiAl thin films on piezoelectric CTGS substrates as an alternative metallization system for high-temperature SAW devices
Ti/Al multilayer films with a total thickness of 200 nm were deposited on the high-temperature (HT) stable piezoelectric Ca3TaGa3Si2O14 (CTGS) as well as on thermally oxidized Si (SiO2/Si) reference substrates. The Ti–Al films were characterized regarding their suitability as an alternative metallization for electrodes in HT surface acoustic wave devices. These films provide the advantage of significantly lower costs and in addition also a significantly lower density as compared to Pt, which allows a greater flexibility in device design. To realize a thermal stability of the films, AlNO cover as well as barrier layers at the interface to the substrate were applied. The samples were annealed for 10 h at up to 800 °C in high vacuum (HV) and at 600 °C in air and analyzed regarding the γ-TiAl phase formation, film morphology, and possible degradation. The Ti/Al films were prepared either by magnetron sputtering or by e-beam evaporation and the different behavior arising from the different deposition method was analyzed and discussed. For the evaporated Ti/Al films, AlNO barriers with a lower O content were used to evaluate the influence of the composition of the AlNO on the HT stability. The sputter-deposited Ti/Al films showed an improved γ-TiAl phase formation and HT stability (on SiO2/Si up to 800 °C in HV and 600 °C in air, on CTGS with a slight oxidation after annealing at 800 °C in HV) as compared to the evaporated samples, which were only stable up to 600 °C in HV and in air.
Durability of TiAl based surface acoustic wave devices for sensing at intermediate high temperatures
TiAl based surface acoustic wave (SAW) devices, which offer a promising cheap and easy to handle wireless sensor solution for intermediate high temperatures up to 600 °C, were prepared and investigated with respect to their durability. To obtain the devices, Ti/Al multilayers were deposited on high-temperature stable piezoelectric catangasite (CTGS) substrates and structured as electrodes via the lift-off technique. AlNO cover layers and barrier layers at the substrate site served as an oxidation protection. The devices were characterized regarding their electrical behavior by ex-situ measurements of their frequency characteristics after heat treatments up to 600 °C in air. In addition, long-term in situ measurements up to 570 °C were performed to analyze a possible drift of the resonant frequency in dependence on the temperature and time. Scanning electron microscopy of the surfaces of the devices and scanning transmission electron microscopy of cross sections of TiAl interdigital transducer electrode fingers and the contact pads were conducted to check the morphology of the electrode metallization and to reveal if degradation or oxidation processes occurred during the heat treatments. The results demonstrated a sufficient high-temperature stability of the TiAl based devices after a first conditioning of system. A linear dependence of the resonant frequency on the temperature of about −37 ppm/K was observed. In summary, the suitability of TiAl based SAW sensors for long-term application at intermediate temperatures was proven.
Evaluation of surface cleaning procedures for CTGS substrates for SAW technology with XPS
A highly efficient and reproducible cleaning procedure of piezoelectric substrates is essential in surface acoustic waves (SAW) technology to fabricate high-quality SAW devices, especially for new applications such SAW sensors wherein new materials for piezoelectric substrates and interdigital transducers are used. Therefore, the development and critical evaluation of cleaning procedures for each material system that is under consideration becomes crucial. Contaminants like particles or the presence of organic/inorganic material on the substrate can dramatically influence and alter the properties of the thin film substrate composite, such as wettability, film adhesion, film texture, and so on. In this article, focus is given to different cleaning processes like SC-1 and SC-2, UV-ozone treatment, as well as cleaning by first-contact polymer Opticlean, which are applied for removal of contaminants from the piezoelectric substrate Ca 3 TaGa 3 Si 2 O 14 . By means of X-ray photoelectron spectroscopy, the presence of the most critical contaminants such as carbon, sodium, and iron removed through different cleaning procedures were studied and significant differences were observed between the outcomes of these procedures. Based on these results, a two-step cleaning process, combining SC-1 at a reduced temperature at 30 ∘ C instead of 80 ∘ C and a subsequent UV-ozone cleaning directly prior to deposition of the metallization, is suggested to achieve the lowest residual contamination level.
The Influence of the Composition of Ru100−xAlx (x = 50, 55, 60, 67) Thin Films on Their Thermal Stability
RuAl thin films possess a high potential as a high temperature stable metallization for surface acoustic wave devices. During the annealing process of the Ru-Al films, Al2O3 is formed at the surface of the films even under high vacuum conditions, so that the composition of a deposited Ru50Al50 film is shifted to a Ru-rich alloy. To compensate for this effect, the Al content is systematically increased during the deposition of the Ru-Al films. Three Al-rich alloys—Ru45Al55, Ru40Al60 and Ru33Al67—were analyzed concerning their behavior after high temperature treatment under high vacuum and air conditions in comparison to the initial Ru50Al50 sample. Although the films’ cross sections show a more homogeneous structure in the case of the Al-rich films, the RuAl phase formation is reduced with increasing Al content.
Aluminum based high temperature thin film electrode system for wireless sensors
Self-sustained, wireless high-temperature stable sensors are developed, which are based on an aluminum alloy as the electrode metallization. Due to its cost-effectiveness accompanied by a high-temperature stability, this alloy substitutes and outperforms the commonly applied expensive Pt- and Ir-based metals. For the first time, a comprehensive structural, electrical and high-frequency characterization of these surface acoustic wave (SAW) sensors is shown. They are based on Catangasite (Ca3TaGa3Si2O14, CTGS) in combination with properly structured cover and barrier layers for the metallization. The frequency characteristics is determined up to 700 °C by ex situ and in situ methods. In addition, the morphology of the AlRu electrodes is analyzed after the thermal loadings and the temperature dependent sheet resistance is measured. The results reveal a reproducible and linear correlation between the applied temperature and the sheet resistance as well as the resonant frequency. In addition, hardly any degradation of the electrodes is detected after the thermal loadings. The observed high-temperature stability of the devices up to at least 700 °C demonstrates the large potential of the AlRu based SAW sensors as a cost-efficient alternative to expensive noble metal based sensors in industrial applications for the support of energy efficient operation.
Surface effects and challenges for application of piezoelectric langasite substrates in surface acoustic wave devices caused by high temperature annealing under high vacuum
Substrate materials that are high-temperature stable are essential for sensor devices which are applied at high temperatures. Although langasite is suggested as such a material, severe O and Ga diffusion into an O-affine deposited film was observed during annealing at high temperatures under vacuum conditions, leading to a damage of the metallization as well as a change of the properties of the substrate and finally to a failure of the device. Therefore, annealing of bare LGS (La 3 Ga 5 SiO 14 ) substrates at 800 ∘ C under high vacuum conditions is performed to analyze whether this pretreatment improves the suitability and stability of this material for high temperature applications in vacuum. To reveal the influence of the pretreatment on the subsequently deposited metallization, RuAl thin films are used as they are known to oxidize on LGS at high temperatures. A local study of the pretreated and metallized substrates using transmission electron microscopy reveals strong modification of the substrate surface. Micro cracks are visible. The composition of the substrate is strongly altered at those regions. Severe challenges for the application of LGS substrates under high-temperature vacuum conditions arise from these substrate damages, revealing that the pretreatment does not improve the applicability.
Stress and Microstructure Evolution in Mo Thin Films without or with Cover Layers during Thermal-Cycling
The intrinsic stress behavior and microstructure evolution of Molybdenum thin films were investigated to evaluate their applicability as a metallization in high temperature microelectronic devices. For this purpose, 100 nm thick Mo films were sputter-deposited without or with an AlN or SiO2 cover layer on thermally oxidized Si substrates. The samples were subjected to thermal cycling up to 900 °C in ultrahigh vacuum; meanwhile, the in-situ stress behavior was monitored by a laser based Multi-beam Optical Sensor (MOS) system. After preannealing at 900 °C for 24 h, the uncovered films showed a high residual stress at room temperature and a plastic behavior at high temperatures, while the covered Mo films showed an almost entirely elastic deformation during the thermal cycling between room temperature and 900 °C with hardly any plastic deformation, and a constant stress value during isothermal annealing without a notable creep. Furthermore, after thermal cycling, the Mo films without as well as with a cover layer showed low electrical resistivity (≤10 μΩ·cm).
Long-term high-temperature behavior of Ti–Al based electrodes for surface acoustic wave devices
The long-term high-temperature behavior of Ti–Al based electrodes for the application in surface acoustic wave (SAW) sensor devices was analyzed. The electrodes were obtained by e-beam evaporation of Ti/Al multilayers on the high-temperature stable piezoelectric Ca3TaGa3Si2O14 (CTGS) substrates and structuring via the lift-off process. AlNO (25 at.% Al; 60 at.% N and 15 at.% O) cover and barrier layers were applied as protection against oxidation from the surrounding atmosphere and to prohibit a chemical reaction with the substrate. The samples were annealed at temperatures up to 600 °C in air for a duration of up to 192 h. Scanning and transmission electron microscopy were used to evaluate the morphology and degradation of the electrodes as well as of the extended contact pads. The results revealed that the Ti–Al based electrodes remained unoxidized after annealing for 192 h at 400 and 500 °C and for 24 h at 600 °C. After the heat treatment for 192 h at 600 °C, a strong oxidation of the structured electrodes occurred, which was less pronounced within the pads. In summary, the investigation showed that Ti–Al based SAW devices are a cost efficient alternative for long-term applications up to at least 500 °C and short- and medium-term applications up to 600 °C.