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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.
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.
Functionalization of Ti-40Nb implant material with strontium by reactive sputtering
Background: Surface functionalization of orthopedic implants with pharmaceutically active agents is a modern approach to enhance osseointegration in systemically altered bone. A local release of strontium, a verified bone building therapeutic agent, at the fracture site would diminish side effects, which could occur otherwise by oral administration. Strontium surface functionalization of specially designed titanium-niobium (Ti-40Nb) implant alloy would provide an advanced implant system that is mechanically adapted to altered bone with the ability to stimulate bone formation. Methods: Strontium-containing coatings were prepared by reactive sputtering of strontium chloride (SrCl2) in a self-constructed capacitively coupled radio frequency (RF) plasma reactor. Film morphology, structure and composition were investigated by scanning electron microscopy (SEM), time of flight secondary ion mass spectrometry (ToF-SIMS) and X-ray photoelectron spectroscopy (XPS). High-resolution transmission electron microscopy (HR-TEM) was used for the investigation of thickness and growth direction of the product layer. TEM lamellae were prepared using the focused ion beam (FIB) technique. Bioactivity of the surface coatings was tested by cultivation of primary human osteoblasts and subsequent analysis of cell morphology, viability, proliferation and differentiation. The results are correlated with the amount of strontium that is released from the coating in biomedical buffer solution, quantified by inductively coupled plasma mass spectrometry (ICP-MS). Results: Dense coatings, consisting of SrOxCly, of more than 100 nm thickness and columnar structure, were prepared. TEM images of cross sections clearly show an incoherent but well-structured interface between coating and substrate without any cracks. Sr2+ is released from the SrOxCly coating into physiological solution as proven by ICP-MS analysis. Cell culture studies showed excellent biocompatibility of the functionalized alloy. Conclusions: Ti-40Nb alloy, a potential orthopedic implant material for osteoporosis patients, could be successfully plasma coated with a dense SrOxCly film. The material performed well in in vitro tests. Nevertheless, the Sr2+ release must be optimized in future work to meet the requirements of an effective drug delivery system.
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.