Understanding internal dissipation in resonant mechanical systems at the micro- and nanoscale is of great technological and fundamental interest. Resonant mechanical systems are central to many sensor technologies, and microscale resonators form the basis of a variety of scanning probe microscopies. Furthermore, coupled resonant mechanical systems are of great utility for the study of complex dynamics in systems ranging from biology to electronics to photonics. In this work, we report the detailed experimental study of internal dissipation in micro- and nanomechanical oscillators fabricated from amorphous and crystalline diamond materials, atomistic modeling of dissipation in amorphous, defect-free, and defect-containing crystalline silicon, and experimental work on the properties of one-dimensional and two-dimensional coupled mechanical oscillator arrays. We have identified that internal dissipation in most micro- and nanoscale oscillators is limited by defect relaxation processes, with large differences in the nature of the defects as the local order of the material ranges from amorphous to crystalline. Atomistic simulations also showed a dominant role of defect relaxation processes in controlling internal dissipation. Our studies of one-dimensional and two-dimensional coupled oscillator arrays revealed that it is possible to create mechanical systems that should be ideal for the study of non-linear dynamics and localization.
Many MEMS devices are based on polysilicon because of the current availability of surface micromachining technology. However, polysilicon is not the best choice for devices where extensive sliding and/or thermal fields are applied due to its chemical, mechanical and tribological properties. In this work, we investigated the mechanical properties of three new materials for MEMS/NEMS devices: silicon carbide (SiC) from Case Western Reserve University (CWRU), ultrananocrystalline diamond (UNCD) from Argonne National Laboratory (ANL), and hydrogen-free tetrahedral amorphous carbon (ta-C) from Sandia National Laboratories (SNL). Young's modulus, characteristic strength, fracture toughness, and theoretical strength were measured for these three materials using only one testing methodology - the Membrane Deflection Experiment (MDE) developed at Northwestern University. The measured values of Young's modulus were 430GPa, 960GPa, and 800GPa for SiC, UNCD, and ta-C, repectively. Fracture toughness measurments resulted in values of 3.2, 4.5, and 6.2 MPa×m 1/2, respectively. The strengths were found to follow a Weibull distribution but their scaling was found to be controlled by different specimen size parameters. Therefore, a cross comparison of the strengths is not fully meaningful. We instead propose to compare their theoretical strengths as determined by employing Novozhilov fracture criterion. The estimated theoretical strength for SiC is 10.6GPa at a characteristic length of 58nm, for UNCD is 18.6GPa at a characteristic length of 37nm, and for ta-C is 25.4GPa at a characteristic length of 38nm. The techniques used to obtained these results as well as microscopic fractographic analyses are summarized in the article. We also highlight the importance of characterizing mechanical properties of MEMS materials by means of only one simple and accurate experimental technique.
We have measured the temperature dependence of mechanical dissipation in tetrahedral amorphous carbon flexural and torsional resonators over the temperature range from 300 to 1023 K. The mechanical dissipation was found to be controlled by defects within the material, and the magnitude and temperature dependence of the dissipation were found to depend on whether flexural or torsional vibrational modes were excited. The defects that were active under flexural stresses have a relatively flat concentration from 0.4 to 0.7 eV with an ever increasing defect concentration up to 1.9 eV. Under shear stresses (torsion), the defect activation energies increase immediately beginning at 0.4 eV, with increasing defect concentration at higher energies.
Resist substrates used in the LIGA process must provide high initial bond strength between the substrate and resist, little degradation of the bond strength during x-ray exposure, acceptable undercut rates during development, and a surface enabling good electrodeposition of metals. Additionally, they should produce little fluorescence radiation and give small secondary doses in bright regions of the resist at the substrate interface. To develop a new substrate satisfying all these requirements, we have investigated secondary resist doses due to electrons and fluorescence, resist adhesion before exposure, loss of fine features during extended development, and the nucleation and adhesion of electrodeposits for various substrate materials. The result of these studies is a new anodized aluminum substrate and accompanying methods for resist bonding and electrodeposition. We demonstrate successful use of this substrate through all process steps and establish its capabilities via the fabrication of isolated resist features down to 6 {micro}m, feature aspect ratios up to 280 and electroformed nickel structures at heights of 190 to 1400 {micro}m. The minimum mask absorber thickness required for this new substrate ranges from 7 to 15 {micro}m depending on the resist thickness.
Nano-electromechanical oscillators (NEMOs), capacitively-coupled radio frequency (RF) MEMS switches incorporating dissipative dielectrics, new processing technologies for tetrahedral amorphous carbon (ta-C) films, and scientific understanding of dissipation mechanisms in small mechanical structures were developed in this project. NEMOs are defined as mechanical oscillators with critical dimensions of 50 nm or less and resonance frequencies approaching 1 GHz. Target applications for these devices include simple, inexpensive clocks in electrical circuits, passive RF electrical filters, or platforms for sensor arrays. Ta-C NEMO arrays were used to demonstrate a novel optomechanical structure that shows remarkable sensitivity to small displacements (better than 160 fm/Hz {sup 1/2}) and suitability as an extremely sensitive accelerometer. The RF MEMS capacitively-coupled switches used ta-C as a dissipative dielectric. The devices showed a unipolar switching response to a unipolar stimulus, indicating the absence of significant dielectric charging, which has historically been the major reliability issue with these switches. This technology is promising for the development of reliable, low-power RF switches. An excimer laser annealing process was developed that permits full in-plane stress relaxation in ta-C films in air under ambient conditions, permitting the application of stress-reduced ta-C films in areas where low thermal budget is required, e.g. MEMS integration with pre-existing CMOS electronics. Studies of mechanical dissipation in micro- and nano-scale ta-C mechanical oscillators at room temperature revealed that mechanical losses are limited by dissipation associated with mechanical relaxation in a broad spectrum of defects with activation energies for mechanical relaxation ranging from 0.35 eV to over 0.55 eV. This work has established a foundation for the creation of devices based on nanomechanical structures, and outstanding critical research areas that need to be addressed for the successful application of these technologies have been identified.
This report describes a new microsystems technology for the creation of microsensors and microelectromechanical systems (MEMS) using stress-free amorphous diamond (aD) films. Stress-free aD is a new material that has mechanical properties close to that of crystalline diamond, and the material is particularly promising for the development of high sensitivity microsensors and rugged and reliable MEMS. Some of the unique properties of aD include the ability to easily tailor film stress from compressive to slightly tensile, hardness and stiffness 80-90% that of crystalline diamond, very high wear resistance, a hydrophobic surface, extreme chemical inertness, chemical compatibility with silicon, controllable electrical conductivity from insulating to conducting, and biocompatibility. A variety of MEMS structures were fabricated from this material and evaluated. These structures included electrostatically-actuated comb drives, micro-tensile test structures, singly- and doubly-clamped beams, and friction and wear test structures. It was found that surface micromachined MEMS could be fabricated in this material easily and that the hydrophobic surface of the film enabled the release of structures without the need for special drying procedures or the use of applied hydrophobic coatings. Measurements using these structures revealed that aD has a Young's modulus of {approx}650 GPa, a tensile fracture strength of 8 GPa, and a fracture toughness of 8 MPa{center_dot}m {sup 1/2}. These results suggest that this material may be suitable in applications where stiction or wear is an issue. Flexural plate wave (FPW) microsensors were also fabricated from aD. These devices use membranes of aD as thin as {approx}100 nm. The performance of the aD FPW sensors was evaluated for the detection of volatile organic compounds using ethyl cellulose as the sensor coating. For comparable membrane thicknesses, the aD sensors showed better performance than silicon nitride based sensors. Greater than one order of magnitude increase in chemical sensitivity is expected through the use of ultra-thin aD membranes in the FPW sensor. The discoveries and development of the aD microsystems technology that were made in this project have led to new research projects in the areas of aD bioMEMS and aD radio frequency MEMS.
The strength and modulus of amorphous diamond, a new material for surface micromachined MEMS and sensors, was tested in uniaxial tension by pulling laterally with a flat tipped diamond in a nanoindenter. Several sample designs were attempted. Of those, only the single layer specimen with a 1 by 2 {micro}m gage cross section and a fixed end rigidly attached to the substrate was successful. Tensile load was calculated by resolving the measured lateral and normal forces into the applied tensile force and frictional losses. Displacement was corrected for machine compliance using the differential stiffness method. Post-mortem examination of the samples was performed to document the failure mode. The load-displacement data from those samples that failed in the gage section was converted to stress-strain curves using carefully measured gage cross section dimensions. Mean fracture strength was found to be 8.5 {+-} 1.4 GPa and the modulus was 831 {+-} 94 GPa. Tensile results are compared to hardness and modulus measurements made using a nanoindenter.
We have developed a new multilayer a-tC material that is thick stress-free, adherent, low friction, and with hardness and stiffness near that of diamond. The new a-tC material is deposited by J pulsed-laser deposition (PLD) at room temperature, and fully stress-relieved by a short thermal anneal at 600°C. A thick multilayer is built up by repeated deposition and annealing steps. We measured 88 GPa hardness, 1100 GPa Young's modulus, and 0.1 friction coefficient (under high load). Significantly, these results are all well within the range reported for crystalline diamond. In fact, this material, if considered separate from crystalline diamond, is the 2nd hardest material known to man. Stress-free a-tC also has important advantages over thin film diamond; namely, it is smooth, processed at lower temperature, and can be grown on a much broader range of substrates. This breakthrough will enable a host of applications that we are actively pursuing in MEMs, sensors, LIGA, etc.
The authors performed an X-ray diffraction study of tetrahedral-coordinated-amorphous carbon (a-tC) films prepared by pulsed laser deposition (PLD). Samples properties were analyzed as a function of laser energy and thickness. For all thicknesses and laser energies, films were made up of clusters with a basic unit size of 7 - 11 nm. Thicker films, as well as films prepared at higher laser densities exhibit larger clusters, in the tens of nanometers. The clusters are not readily observable by AFM, which may indicate the presence of a flat (graphitized) top film surface.
Carbon Nitride (CNx) films have been grown by ion-assisted pulsed-laser deposition (IAPLD). Graphite targets were laser ablated while bombarding the substrate with ions from a broad-beam Kaufman-type ion source. The ion voltage, current density, substrate temperature, and feed gas composition (N2 in Ar) have been varied. The resultant films were characterized by Raman, Fourier transform infrared (FTIR), and Rutherford back scattering (RBS) spectroscopy. Samples with ≈30% N/C ratio have been fabricated. The corresponding Raman and FTIR spectra indicate that nitrogen is incorporated into the samples by insertion into sp2- bonded structure. A low level of C≡N triple bonds is also found. As the ion current and voltage are increased with a pure Ar ion beam, Raman peaks associated with nanocrystalline graphite appear in the spectra. Adding low levels of nitrogen to the ion beam first reduces the Raman intensity in the vicinity of the graphite disorder peak without adding detectable amounts of nitrogen to the films (as measured by RBS). At higher nitrogen levels in the ion beam, significant amounts of nitrogen are incorporated into the samples, and the magnitude of the ″disorder″ peak increases. By increasing the temperature of the substrate during deposition, the broad peak due mainly to sp2-bonded C-N in the FTIR spectra is shifted to lower wavenumber. This could be interpreted as evidence of single-bonded C-N; however, it is more likely that the character of the sp2 bonding is changing.
We are studying carbon thin films by using a pulsed excimer laser to ablate pyrolytic graphite targets to form highly tetrahedral coordinated amorphous carbon (at-C) films. These films have been grown on room temperature p-type Si (100) substrates without the intentional incorporation of hydrogen. In order to understand and optimize the growth of at-C films, parametric studies of the growth parameters have been performed. We have also introduced various background gases (H2, N2 and Ar) and varied the background gas pressure during deposition. The residual compressive stress levels in the films have been measured and correlated to changes in the Raman spectra of the at-C band near 1565 cm-1. The residual compressive stress falls with gas pressure, indicating a decreasing atomic sp3-bonded carbon fraction. We find that reactive gases such as hydrogen and nitrogen significantly alter the Raman spectra at higher pressures. These effects are due to a combination of chemical incorporation of nitrogen and hydrogen into the film as well as collisional cooling of the ablation plume. In contrast, films grown in non-reactive Ar background gases show much less dramatic changes in the Raman spectra at similar pressures.
We are studying the boron nitride system using a pulsed excimer laser to ablate from hexagonal BN (cBN) targets to form cubic BN (cBN) films. We are depositing BN films on heated (25--800C) Si (100) surfaces and are using a broad-beam ion source operated with Ar and N{sub 2} source gases to produce BN films with a high percentage of sp{sup 3}-bonded cBN. In order to optimize growth and nucleation of cBN films, parametric studies of the growth parameters have been performed. The best films to date show >85% sp{sup 3}-bonded BN as determined from Fourier-transform infrared (FTIR) reflection spectroscopy. High resolution transmission electron microscopy (TEM) and selected area electron diffraction confirm the presence of cBN in these samples. The films are polycrystalline and show grain sizes up to 30--40 mn. We find from both the FTIR and TEM analyses that the cBN content in these films evolves with growth time. Initially, the films are deposited as hBN and the cBN nucleates on this hBN underlayer. Importantly, the position of the cBN IR phonon also changes with growth time. Initially this mode appears near 1130 cm{sup {minus}1} and the position decreases with growth time to a constant value of 1085 cm{sup {minus}1}. Since in bulk cBN this IR mode appears at 1065 cm{sup {minus}1}, a large compressive stress induced by the ion bombardment is suggested. In addition, we report on the variation in cBN percentage with temperature.