Acoustic microscopy measurement of elastic constants and massdensity

A method is presented to determine the elastic constants and the mass density of isotropic and anisotropic solids and anisotropic thin films. The velocity and attenuation of leaky surface acoustic waves (SAWs) have been obtained for specified propagation directions from V(z) curves measured by line-focus acoustic microscopy (LFAM). The experimentally obtained velocities have been compared to velocities obtained from a measurement model for the V(z) curve which simulates the experiment. Since the measured and simulated V(z) curves have the same systemic errors, the material constants are free of such errors. For an isotropic solid, Young's modulus E, the shear modulus G and the mass density ρ have been determined from the leaky Rayleigh wave velocity and attenuation, measured by LFAM, and a longitudinal wave velocity measured by a pulse-echo transit-time technique. For a cubic-crystalline solid, the ratios of the elastic constants to the mass density (c₁₁ /ρ, c₁₂/ρ, c₄₄/ρ) have been determined from the directional variation of measured SAW velocities, using a preliminary estimate of ρ. The mass density ρ has subsequently been determined by additionally using the attenuation of leaky SAWs in crystal symmetry directions. For a cubic-crystalline thin film deposited on a substrate, the elastic constants and the mass density (c₁₁, c₁₂, c₄₄, ρ) of the film have been determined from the directional variation of the measured SAW velocities, and a comparison of the corresponding attenuation coefficient with the measured attenuation coefficient has been used to verify the results     

Elastic properties of proton exchanged lithium niobate

A method is demonstrated for determination of elastic constants of anisotropic layers on arbitrarily anisotropic and piezoelectric substrates only using the easily measured velocity of surface acoustic waves. By means of a detailed theoretical analysis it is shown that by use of the presented method, the elastic stiffness constants and propagation properties of any nonpiezoelectric isotropic, cubic, or even trigonal layer can be determined. The method is applied to proton-exchanged lithium niobate (PE:LiNbO(3)). Complete measurements of dispersion characteristics of Rayleigh waves on Y -cut PE:LiNbO(3) and calculated values of all elastic stiffness constants of the proton-exchanged film are reported.     

Inverse relationships for reflection diagnostics of uniaxially anisotropic nanoscale films on isotropic materials

The possibilities of determining the parameters of uniaxially anisotropic ultrathin nonabsorbing dielectric films on absorbing or transparent isotropic substrates by surface differential reflectance measurements are analyzed. The analysis is based on analytical reflection formulas obtained in the framework of a long-wavelength approximation. It is shown that, in the case of transparent substrates, it is always possible to determine the thickness of a uniaxially ultrathin film and its four parameters of anisotropy (optical constants n(o) and n(e) and angles θ and φ) simultaneously. However, for such films on absorbing substrates, it is possible to decouple the thickness and optical constants by differential reflectance measurements only if θ≠0. The accuracy of the obtained analytic formulas for determining the parameters of ultrathin films is estimated by computer simulations where the reflection problem was solved numerically on the basis of the rigorous electromagnetic theory for anisotropic layered systems.     

Experimental study of construction mechanism of V(z) curves obtained by line-focus-beam acoustic microscopy

The propagation characteristics, viz., phase velocity and attenuation, of leaky surface acoustic waves (LSAWs), excited on the water/sample boundary are obtained through analyzing the V(z) curves measured by line-focus-beam acoustic microscopy. However, different values of these characteristics are obtained, depending upon different ultrasonic devices and operating frequencies employed. The construction mechanism of V(z) curves was investigated experimentally by measuring the amplitude and phase for Teflon to provide an understanding of the device performance for velocity measurements. A V(z) curve measured for Teflon, on which no leaky waves are excited when water is the coupling medium, can be used for the characteristic device response, depending only upon the device parameters and the operating frequencies. From the investigation of the ultrasonic device and the frequency dependences of the characteristic device responses, the phase gradient was found to be directly related to values of measured LSAW velocities. From this result, apparent frequency dependences in LSAW velocity measurements are explained quantitatively for a specimen of gadolinium gallium garnet.     

Oscillations in V(z) curves of thin samples

The explanation of the oscillations appearing at large defocus in the V(z) curves of thin specimens is given for isotropic and cubic materials. Using a ray model it is shown that oscillations are generated by the interference of the normal ray with the shear ray reflected from the bottom surface along a symmetrical path to the lens. The model predicts that in isotropic materials oscillations arise at critical values of defocus, while in anisotropic solids the onset of the oscillations depends on the shape of the slowness surface. In particular, for cubic crystals cut along {001}, due to the convex shape of the slowness surface, oscillations in V(z) are predicted from the beginning of defocus. This finding has been experimentally confirmed in V(z) curves of thin GaAs(001) wafers. The dependence of the periodicity of the oscillations on the defocus and propagation direction has been confirmed by the ray model. An interpretation of the amplitude increase which is observed in the V(z) of GaAs samples at large defocus is given     

Numerical ellipsometry: Advanced analysis of thin absorbing films in the n-k plane

A major challenge for those utilizing ellipsometry is numerical processing of the measured data. The transcendental, multivalued equations arising from the physics of simple reflection are problematic for the least-squares numerical methods in common use. Previously we have applied Complex Analysis in the n-k plane and this has led to a growing array of numerical research methods which achieve computational accuracy at a chosen limit (~ 10^− 14) rather than achieving only a mean square value of a large number of measurements, more than 14 orders of magnitude less accurate in this case. The work presented here is the mathematics for film stacks of an arbitrary number of layers required to apply numerical methods for use with absorbing films deposited on transparent and on absorbing substrates. The approach finds intersections of projections of three “twisted curves” resulting from a single light incidence angle and light wavelength measurement for three film thicknesses at a time. The approach employed here determines the thickness and optical properties of chromium films (between 10 and 25 nm nominal thickness) deposited onto silicon substrates. A simple single film model matched the measurements to a first order only. Improved agreement is obtained by the addition of interface layers above and below the main chromium film.     

Influence of reflected waves from the back surface of thin solid-plate specimen on velocity measurements by line-focus-beam acoustic microscopy

We investigated the velocity measurements of leaky surface acoustic waves (LSAW) by line-focus-beam (LFB) acoustic microscopy of thin specimens for which the waves reflected from the back surface of the specimen (back reflection) must be included in the measurement model. The influence of back reflection resulted in a serious problem in measurement accuracy of the apparent changes of measured velocities. Using several samples of thin synthetic silica glasses, the determination of LSAW velocity affected by the reflected waves and the relationship between the specimen thickness and the apparent velocity change with a periodic frequency interval in the frequency dependence of measured LSAW velocities are discussed in detail. Three useful methods for eliminating that influence are proposed and demonstrated: first, separating the radio frequency (RF) pulsed wave signal from the specimen surface and the pulses reflected from the back surface by reducing the RF pulse width; second, scattering acoustic waves from the roughened back surface; and third, taking the moving average of measured frequency characteristics of LSAW velocities. It is shown that, among these methods, the moving average method is the most useful and effective as a general means to eliminate the influence and to determine intrinsic velocity values because this method needs no specimen process and no system change, and the same conventional V(z) curve measurement and analysis can be employed.     

Ellipsometry of thin films of copper phthalocyanine

Ellipsometric measurements have provided qualitative information on the optical properties of CuPC films deposited on a thin gold layer substrate. Detailed interpretation was complicated by variations in the density of the deposited layers and the surface roughness of the substrate. Films less than 100 nm thick can be satisfactory represented by a single homogeneous isotropic layer. Thicker films appear to be equivalent to an isotropic inner layer and an anisotropic outer layer, where the latter results from bulk deposition of CuPC with the molecules in a predominant orientation to the surface. Reasonable agreement has been obtained between film thicknesses measured by weighing and by ellipsometry, assuming a single homogeneous anisotropic film for thickness in excess of 150 nm.     

Effect of periodic surface roughness on V(z) curves for the line-focus acoustic microscope

A specimen with a periodic surface profile is considered to estimate the effect of surface roughness on the V(z) curve for the line-focus acoustic microscope. The Fourier optics approach is used to obtain the response of the lens and the Rayleigh-Fourier method is used to obtain the reflection coefficients for plane wave incidence from the fluid side on the periodic surface. An integral expression is obtained to calculate V(z) curves for periodic surface profiles. The V(z) curves are used to calculate the leaky Rayleigh wave velocities by applying the fast Fourier technique. Numerical results are presented to display the effect of sinusoidal surface roughness on the V(z) curves and the corresponding leaky Rayleigh wave velocities.     

Effect of diamond nucleation process on propagation losses of AlN/diamond SAW filter

In this work, the effect of a diamond nucleation process on freestanding aluminium nitride (AlN)/diamond surface acoustic wave (SAW) device performances was studied. Before diamond deposition, silicon (Si) substrates have been mechanically nucleated, using an ultrasonic vibration table with submicron diamond slurry, and bias-enhanced nucleated (BEN). Freestanding diamond layers obtained on mechanically scratched Si substrates exhibit a surface roughness of R(MS) = 13 nm, whereas very low surface roughness (as low as R(MS) < or = 1 nm) can be achieved on a freestanding BEN diamond layer. Propagation losses have been measured as a function of the operating frequency for the two nucleation techniques. Dispersion curves of phase velocities and electromechanical coupling coefficient (K2) were determined experimentally and by calculation as a function of normalized thickness AlN film (kh(AlN) = 2pi h(AlN)/lambda). Experimental results show that the propagation losses strongly depend on the nucleation technique, and that these losses are weakly increased with frequency when the BEN technique is used.     

Acoustic reflection from the boundary of anisotropic thermoviscoelastic solid with fluid

Vertical slownesses of waves at a boundary of an anisotropic thermoviscoelastic medium are calculated as roots of a polynomial equation of degree eight. Out of the corresponding eight waves, the four, which travel towards the boundary are identified as upgoing waves. Remaining four waves travel away from the boundary and are termed as downgoing waves. Reflection and refraction of plane harmonic acoustic waves are studied at a plane boundary between anisotropic thermoviscoelastic solid and a non-viscous fluid. At this fluid-solid interface, an incident acoustic wave through the fluid reflects back as an attenuated acoustic wave and refracts as four attenuating waves into the anisotropic base. Slowness vectors of all the waves in two media differ only in vertical components. Complex values of vertical slowness define inhomogeneous refracted waves with a fixed direction of attenuation, i.e. perpendicular to the interface. Energy partition is calculated at the interface to find energy shares of reflected and refracted waves. A part of incident energy dissipates due to interaction among the attenuated refracted waves. Numerical examples are considered to study the variations in energy shares with the direction of incident wave. For each incidence, the conservation of incident energy is verified in the presence of interaction energy. Energy partition at the interface seems to be changing very slightly with the azimuthal variations of the incident direction. Effects of anisotropy, elastic relaxation and thermal parameters on the variations in energy partition are discussed. The acoustic wave reflected from isothermal interface is much significant for incidence around some critical directions, which are analogous to the critical angles in a non-dissipative medium. The changes in thermal relaxation times and uniform temperature of the thermoviscoelastic medium do not show any significant effect on the reflected energy.     

Crystalline structure of germanium films on silicon substrates: I. Investigation of the perfection of germanium heteroepitaxial films on silicon by X-ray diffraction methods

The purpose of this paper is to describe an investigation of the structural perfection of heteroepitaxial Ge films on silicon by different X-ray diffraction methods. Quantitative information about the degree of structural perfection of the films has been obtained by X-ray intensity jumps measured near the K-edge absorption of germanium and by rocking curves. Structural damage in the films and substrates has been studied by X-ray topographical methods. The possibility of obtaining independent film and substrate topograms has been shown. Elastic strains arising during the film growth lead to film and substrate fragmentation. Films and substrates have the same configuration and sizes of fragments. A new X-ray method for the heteroepitaxial films thickness measurement has been proposed.     

High rectification ratios of Fe–porphyrin molecules on Au facets

We report room temperature measurements of current vs. voltage (I–V) from self-assembled Fe porphyrin [Fe(III) 5,15-di[4-(s-acetylthio)phenyl]-10,20-diphenyl porphine] molecular layers formed on annealed gold crystal facets on glass substrates. I–V curves were measured using an atomic force microscope with a conductive platinum tip. We observed a rectifier effect that shows asymmetric I–V curves from a monolayer of molecules. The majority rectification ratios at ±1 V obtained from hundreds of I–V lie in between 20 and 200, with the highest up to 9000. This is in contrast to the symmetric I–V curves measured from a few nm thick multilayer molecular islands. We contribute the observed rectification in ultrathin FeP molecular layers from asymmetric Schottky barriers that result from molecules in different bonding strengths to electrodes of gold and platinum.     

Preparation and characterisation of titanium dioxide films for catalytic applications generated by anodic spark deposition

The advanced plasma electrochemical process of anodic spark deposition (ASD) was used to generate photoactive titanium dioxide films on titanium metal substrates. A shift to easier-to-machine substrates was demonstrated by the deposition of a titanium film with physical vapour deposition onto different materials such as glass, silicon, and stainless steel prior to ASD. Obtained films were characterised by scanning electron microscopy, surface area measurement (Brunnauer-Emmett-Teller method, BET), X-ray diffraction, electron-probe microanalysis, and glow discharge spectroscopy. Additionally, film thickness was determined by eddy current measurements. Standard ASD conditions were defined as 180 V applied voltage over a 180 s hold time, a voltage ramp of 20 V/s, a duty cycle of 0.5 and a frequency of 1500 Hz. Most prominent characteristics of the titanium films produced under these standard conditions are a film thickness of ≤80 μm, a surface area of approximately 51 m²/g (BET) and an anatase content of approximately 30% and rutile content of approximately 70%. Furthermore, the film formation process is elucidated and the dependence of film thickness on deposition time and the dependence of the anatase and rutile content on the deposited mass are shown for varying ASD conditions.     

Ultra-thin atomic layer deposited TiN films: non-linear I-V behaviour and the importance of surface passivation

We report the electrical resistivity of atomic layer deposited TiN thin films in the thickness range 2.5-20 nm. The measurements were carried out using the circular transfer length method structures. For the films with thickness in the range of 10-20 nm, the measurements exhibited linear current-voltage (I-V) curves. The sheet resistance R(sh) was determined, and the resistivity was calculated. A value of 120 microohms-cm was obtained for a 20 nm TiN layer. With decreasing film thickness, the resistivity slightly increased and reached 135 microohms-cm for a 10 nm film. However, the measurements on 2.5-5.0 nm thick films revealed non-linear I-V characteristics, implying the dependence of the measured resistance, and therefore the resistivity, of the layers on applied voltage. The influence of the native oxidation due to the exposure of the films to air was taken into account. To fully eliminate this oxidation, a highly-resistive amorphous silicon layer was deposited directly after the ALD of TiN. The electrical measurements on the passivated 2.5- and 3.5 nm TiN layers then exhibited linear I-V characteristics. A resistivity of 400 and 310 microohms-cm was obtained for a 2.5- and 3.5 nm TiN film, respectively.     

Surface-dominated conduction in a 6 nm thick Bi2Se3 thin film

We report a direct observation of surface dominated conduction in an intrinsic Bi(2)Se(3) thin film with a thickness of six quintuple layers grown on lattice-matched CdS (0001) substrates by molecular beam epitaxy. Shubnikov-de Haas oscillations from the topological surface states suggest that the Fermi level falls inside the bulk band gap and is 53 ± 5 meV above the Dirac point, which is in agreement with 70 ± 20 meV obtained from scanning tunneling spectroscopies. Our results demonstrate a great potential of producing genuine topological insulator devices using Dirac Fermions of the surface states, when the film thickness is pushed to nanometer range.     

Measuring distribution of the ellipsoid of birefringence through the thickness of optical disk substrates

We have measured the birefringence of polycarbonate optical disk substrates, using ellipsometry. For a more comprehensive characterization, the probe beam was incident upon substrates in a wide range of polar angles and from different azimuths relative to track direction (?). Our measurements show that the ellipsoid of birefringence is tilted in the plane of radial (r) and normal (z) directions. The tilt angle varies through thickness, with a maximum value of approximately 10°. For beams passing through the substrate in the ?-z plane and at large incident angles, this tilt causes significant conversion (up to 100%) between p- and s-polarized components. Distributions of other parameters, such as the values of in-plane and vertical birefringence, are obtained simultaneously in the measurements.     

On the lower thickness boundary of sputtered TiNi films for shape memory application

In this paper, we study the effects of film thickness on phase transformation of constrained Ti_50.2Ni_49.8 films deposited onto silicon substrates. When the film is too thin, surface oxide and interfacial diffusion layers exert dominant constraining effect that renders high residual stress and low recovery capabilities in the film. The surface oxide and inter-diffusion layer restricts the phase transformation, alters stoichiometry of the remaining TiNi film, and reduces volume of the material available for phase transformation. As a result, a lower thickness boundary (about 100 nm) exists for TiNi films to remain “shape remembering”. Results indicate that a maximum recovery stress and actuation speed can be realized with a thickness of about 800 nm. Based on the curvature measurement results, the relationship between the relative stress and strain of the films (during phase transformation with change of temperature) can be derived.     

Shear-horizontal piezoelectric waves in an aluminum nitride film on a silicon substrate

The propagation of shear-horizontal waves in a piezoelectric film of aluminum nitride on a silicon substrate is studied. Three different electrode configurations are considered for thin film acoustic wave resonator application. A theoretical analysis is performed. The equations of linear piezoelectricity and anisotropic elasticity are used for the film and the substrate, respectively. Real and imaginary dispersion curves as well as electromechanical mode shapes are obtained. The effects of electrode configuration on the distribution of the electromechanical fields and the dispersion curves of long thickness-twist waves as well as energy trapping are examined.     

磷酸二氢钾晶体薄表面层生长动力学实时显微研究

利用光学显微镜实时观测磷酸二氢钾(KDP)晶体柱面及锥面薄表面层的生长过程,测得不同过饱和度下薄表面层前端不同倾角的非正常棱边推移速度。结果表明:倾角越小,非正常棱边推移速度越慢,薄表面生长终止于其前端的正常棱边处;随着过饱和度的增大,非正常棱边推移速度线性增加。计算得到柱面及锥面薄表面层前端非正常棱边推移动力学系数,由于Eslice(010) Eslice(101),因而柱面薄表面层的生长动力学系数大于锥面。建立了基于非奇异面上台阶生长机制下的薄表面层生长体扩散模型。应用该模型解释了薄表面层生长速度随其厚度及前端非正常棱边倾角的变化关系,并讨论了溶液流动对薄表面层生长的影响。结果发现薄表面层生长存在一个使其以恒定厚度向前推移的临界厚度。