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Microstructural Comparisons of Ultra-Thin Cu Films Deposited by Ion-Beam and dc-Magnetron Sputtering
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Microstructure Morphology of Bicontinuous Nanocomposites Thin-Films During Physical Vapor Deposition (PVD).
Abstract not provided.
Interpreting Neutron Reflectivity Profiles of Diblock Copolymer Nanocomposite Thin Films Using Hybrid Particle-Field Simulations
Mixtures of block copolymers and nanoparticles (block copolymer nanocomposites) are known to microphase separate into a plethora of microstructures, depending on the composition, length scale and nature of interactions among its different constituents. Theoretical and experimental works on this class of nanocomposites have already high-lighted intricate relations among chemical details of the polymers, nanoparticles, and various microstructures. Confining these nanocomposites in thin films yields an even larger array of structures, which are not normally observed in the bulk. In contrast to the bulk, exploring various microstructures in thin films by the experimental route remains a challenging task. Here in this work, we construct a model for the thin films of lamellar forming diblock copolymers containing spherical nanoparticles based on a hybrid particle-field approach. The model is benchmarked by comparison with the depth profiles obtained from the neutron reflectivity experiments for symmetric poly(deuterated styrene-b-n butyl methacrylate) copolymers blended with spherical magnetite nanoparticles covered with hydrogenated poly(styrene) corona. We show that the model based on a hybrid particle-field approach provides details of the underlying microphase separation in the presence of the nanoparticles through a direct comparison to the neutron reflectivity data. This work benchmarks the application of the hybrid particle-field model to extract the interaction parameters for exploring different microstructures in thin films containing block copolymers and nanocomposites.
Modulation of microstructure and optical properties of Mo-doped ZnO thin films by substrate temperature
Highlights: • Mo-doped ZnO films are obtained by sputtering at various substrate temperatures. • High-quality MZO thin films with good crystalline have been obtained at 200 °C. • Deposition temperature affects the amount of defects in the crystalline structure - Abstract: Mo-doped ZnO(MZO) films were deposited on Si (1 1 1) substrates by radio frequency sputtering at different substrate temperatures of 200, 300 and 400 °C. The effect of the substrate temperature on the structural and optical properties of the MZO films has been investigated. X-ray diffraction results reveal that all the films are polycrystalline with a hexagonal wurtzite structure with a preferential orientation according to the direction (0 0 2) plane. The crystallinity and surface morphologies of the films are strongly dependent on the growth temperature, which in turn exerts a great effect on microstructural and optical properties of the MZO films. The optical absorption measurements show high ultraviolet (UV) absorbance property of MZO with sharp and intense absorption band in this region and the optical band gap (E{sub g}) are 3.18, 3.22, 3.25 and 3.21 eV for the films deposited at room temperature, 200, 300 and 400 °C. The photoluminescence (PL) intensity of a strong broad violet–blue emission from MZO nanostructures with increasing deposited temperature was also observed. X-ray photoelectron spectroscopy (XPS) was employed to investigate the surface chemical composition of growth products.
Heterogeneous Morphologies and Hardness of Co-Sputtered Thin Films of Concentrated Cu-Mo-W Alloys
Heterogeneous microstructures in Cu-Mo-W alloy thin films formed by magnetron co-sputtering immiscible elements with concentrated compositions are characterized using scanning transmission electron microscopy (STEM) and nanoindentation. In this work, we modified the phase separated structure of a Cu-Mo immiscible system by adding W, which impedes surface diffusion during film growth. The heterogeneous microstructures in the Cu-Mo-W ternary system exhibited bicontinuous matrices and agglomerates composed of Mo(W)-rich phase. This is unique, as these are the slower-diffusing species, contrasting past reports of binary Cu-Mo thin films that exhibited Cu-rich agglomerates. The bicontinuous matrices comprised of Cu-rich and Mo(W)-rich phases exhibited bilayer thicknesses of less than 5 nm. The hardness of these thin films measured using nanoindentation is reported and compared to similar multilayers and nanocomposites in binary systems.
Microstructural, optical and electrical properties of CdS thin films grown by spray pyrolysis technique as a function of substrate temperature
In this research, nanocrystalline cadmium sulfide thin films were produced by the spray pyrolysis technique on glass substrates. The effects of substrate temperature in the range 400–550 °C on the structural, morphological, optical, and electrical properties of the thin films were investigated. The thin films have been characterized by investigating their X-ray diffraction, field emission scanning electron microscope (FE-SEM), and optical absorption (UV–Vis) measurements. X-ray analysis revealed that thin films were a polycrystalline structure with the hexagonal phase in all cases and by increasing in substrate temperature, crystallite size decreases, and dislocation density increases. The FE-SEM images showed that the surface of the thin films is uniform, homogeneous and without cracks. The average sizes of the grains are at the range of 210–235 nm. The obtained values for optical band gap have been in the range of 2.18–2.41 eV, where the value of optical band gap for the thin films decreases by increasing substrate temperature. The Urbach energies of the thin films increase as the substrate temperature is increased. When substrate temperature increased from 400 to 550 °C, electrical resistivity increased from 531 to 2817 Ω cm, carrier concentration decreased from 15.96 × 10{sup 14} to 3.71 × 10{sup 14} cm{sup −3}, Hall mobility decreased from 7.37 to 5.98 cm{sup 2}/V s. Hall effect analysis indicated that the thin films exhibited n-type conductivity.
Atomic-scale microstructure underneath nanoindentation in Al-Cr-N ceramic films
In this work, Al-Cr-N ceramic films deformed by nanoindentation were peeled off from silicon substrates and their atomic-scale microstructures underneath the indenter were investigated by high resolution transmission electron microscope (HR-TEM). Dislocations were formed underneath the indenter and they accumulated along nano-grain boundaries. The accumulative dislocations triggered the crack initiation along grain boundaries, and further resulted in the crack propagation. Dislocations were also observed in nano-grains on the lateral contact area. A model was proposed to describe the variation of microstructures under nanoindentation.
The annealing effects on the micro-structure and properties of RuMoC films as seedless barrier for advanced Cu metallization
100 nm thick RuMoC films and 5 nm thick RuMoC films with Cu capping have been deposited on Si(111) by magnetron co-sputtering with Ru and MoC confocal targets. The samples were subsequently annealed at temperatures ranging from 450 to 650 °C in vacuum at a pressure of 3 × 10{sup −4} Pa to study the annealing effects on the microstructures and properties of RuMoC films for advanced seedless Cu metallization applications. The sheet resistances, residual oxygen contents, and microstructures of the RuMoC films have close correlation with the doping contents of Mo and C, which can be easily controlled by the deposition power ratio of MoC versus Ru targets (DPR). When DPR was 0.5, amorphous RuMoC film (marked as RuMoC II) with low sheet resistances and residual oxygen contents was obtained. The fundamental relationship between the annealing temperatures with the microstructures and properties of the RuMoC films was investigated, and a critical temperature point was revealed at about 550 °C where the components and microstructures of the RuMoC II films changed obviously. Results indicated that below 550 °C, the RuMoC II films remained amorphous due to the well-preserved C-Ru and C-Mo bonds. However, above 550 °C, the microstructures of RuMoC II films transformed from amorphous to nano-composite structure due to the breakage of Ru-C bonds, while the supersaturated solid solution MoC segregated out along the grain boundaries of Ru, thus hindering the diffusion of Cu and O atoms. This is the main mechanism of the excellent thermal stability of the RuMoC films after annealing at high temperatures. The results indicated great prospects of amorphous RuMoC films in advanced seedless Cu metallization applications.
Thermal Conductivity and Phonon Scattering Processes of ALD Grown PbTe–PbSe Thermoelectric Thin Films
Abstract This work studies the thermal conductivity and phonon scattering processes in a series of n‐type lead telluride‐lead selenide (PbTe–PbSe) nanostructured thin films grown by atomic layer deposition (ALD). The ALD growth of the PbTe–PbSe samples in this work results in nonepitaxial films grown directly on native oxide/Si substrates, where the Volmer–Weber mode of growth promotes grains with a preferred columnar orientation. The ALD growth of these lead‐rich PbTe, PbSe, and PbTe–PbSe thin films results in secondary oxide phases, along with an increase microstructural quality with increased film thickness. The compositional variation and resulting point and planar defects in the PbTe–PbSe nanostructures give rise to additional phonon scattering events that reduce the thermal conductivity below that of the corresponding ALD‐grown control PbTe and PbSe films. Temperature‐dependent thermal conductivity measurements show that the phonon scattering in these ALD‐grown PbTe–PbSe nanostructured materials, along with ALD‐grown PbTe and PbSe thin films, are driven by extrinsic defect scattering processes as opposed to phonon–phonon scattering processes intrinsic to the PbTe or PbSe phonon spectra. The implication of this work is that polycrystalline, nanostructured ALD composites of thermoelectric PbTe–PbSe films are effective in reducing the phonon thermal conductivity, and represent a pathway for further improvement of the figure of merit ( ZT ), enhancing their thermoelectric application potential.
Microstructural dependence of defect formation in iron-oxide thin films
In this report passivating iron-oxide films are grown atop iron films simulating the corrosion process in a nuclear reactor environment. Two oxide films grown via physical vapor deposition at 600 °C and room temperature exhibited dense-epitactic and columnar-polycrystalline, microstructures respectively. A third oxide film grown in open air at 600 °C exhibited an eqiuaxed, porous morphology. Cubic maghemite and magnetite phases in each oxide film were identified via grazing incidence X-ray diffraction. Positron annihilation spectroscopy was used to characterize point defects and measure their depth and size distributions in each oxide layer and showed a range of average positron lifetimes from 0.23 ns in the high temperature, vapor deposited film, 0.35 ns in the room temperature-grown film, and 0.31 ns in the thermally grown oxide. These data indicate that the film morphology, which varies greatly in these films, leads to very different defect content. Finally, four-dimensional scanning transmission electron microscopy was used to measure the internal stress of each film and was correlated to the strain state presented in the X-ray diffraction spectra. The defect formation in each film is reasoned through using a thin film growth model.
Reactions of Atomic Oxygen (O(3P)) with Polybutadienes and Related Polymers
Thin films of the following polymers were exposed at ambient temperature to ground-state oxygen atoms (O(3P)), generated by a radio-frequency glow discharge in O2: cis- and trans-1,4-polybutadienes (CB and TB), amorphous 1,2-polybutadiene (VB), polybutadienes with different 1,4/1,2 contents, trans polypentenamer (TP), cis and trans polyoctenamers (CO and TO), and ethylene-propylene rubber (EPM). Transmission infrared spectra of CB and TB films revealed extensive surface recession, or etching, unaccompanied by any microstructural changes within the films, demonstrating that the reactions were confined to the surface layers. Contrary to the report by Rabek, Lucki, and Ranby (1979), there was no O(3P)-induced cis-trans isomerization in CB or TB. From weight-loss measurements, etch rates for polybutadienes were found to be markedly dependent on vinyl content, decreasing by two orders of magnitude from CB (2% 1,2) to structures with 30 to 40% 1,2 double bonds, thereafter increasing by half an order of magnitude to VB (97% 1,2). Relative etch rates for EMP and the polyalkenamers were in the order: EMP is greater than CO (or TO) is greater than TP is greater than CB. The sole non-elastomer examined, TB, had an etch rate about six times that of CB, ascribable to a morphology difference. Cis/trans content had a negligible effect on the etch rate of the polyalkenamers. Mechanisms involving crosslinking through units are proposed for the unexpected protection imparted to polybutadienes by the 1,2 double bonds.
Reducing leakage current and enhancing polarization in multiferroic 3D super-nanocomposites by microstructure engineering
Abstract Multiferroic materials have generated great interest due to their potential as functional device materials. Nanocomposites have been increasingly used to design and generate new functionalities by pairing dissimilar ferroic materials, though the combination often introduces new complexity and challenges unforeseeable in single-phase counterparts. The recently developed approaches to fabricate 3D super-nanocomposites (3D‐sNC) open new avenues to control and enhance functional properties. In this work, we develop a new 3D‐sNC with CoFe 2 O 4 (CFO) short nanopillar arrays embedded in BaTiO 3 (BTO) film matrix via microstructure engineering by alternatively depositing BTO:CFO vertically-aligned nanocomposite layers and single-phase BTO layers. This microstructure engineering method allows encapsulating the relative conducting CFO phase by the insulating BTO phase, which suppress the leakage current and enhance the polarization. Our results demonstrate that microstructure engineering in 3D‐sNC offers a new bottom–up method of fabricating advanced nanostructures with a wide range of possible configurations for applications where the functional properties need to be systematically modified.
Process monitoring during AlN{sub x}O{sub y} deposition by reactive magnetron sputtering and correlation with the film's properties
In this work, AlN{sub x}O{sub y} thin films were deposited by reactive magnetron sputtering, using an aluminum target and an Ar/(N{sub 2}+O{sub 2}) atmosphere. The direct current magnetron discharge parameters during the deposition process were investigated by optical emission spectroscopy and a plasma floating probe was used. The discharge voltage, the electron temperature, the ion flux, and the optical emission lines were recorded for different reactive gas flows, near the target and close to the substrate. This information was correlated with the structural features of the deposits as a first step in the development of a system to control the structure and properties of the films during reactive magnetron sputtering. As the target becomes poisoned, the discharge voltage suffers an important variation, due to the modification of the secondary electron emission coefficient of the target, which is also supported by the evolution of the electron temperature and ion flux to the target. The sputtering yield of the target was also affected, leading to a reduction of the amount of Al atoms arriving to the substrate, according to optical emission spectroscopy results for Al emission line intensity. This behavior, together with the increase of nonmetallic elements in the films, allowed obtaining different microstructures, over a wide range of compositions, which induced different electrical and optical responses of films.
Effect of processing parameters on microstructure of MoS{sub 2} ultra-thin films synthesized by chemical vapor deposition method
MoS{sub 2} ultra-thin layers are synthesized using a chemical vapor deposition method based on the sulfurization of molybdenum trioxide (MoO{sub 3}). The ultra-thin layers are characterized by X-ray diffraction (XRD), photoluminescence (PL) spectroscopy and atomic force microscope (AFM). Based on our experimental results, all the processing parameters, such as the tilt angle of substrate, applied voltage, heating time and the weight of source materials have effect on the microstructures of the layers. In this paper, the effects of such processing parameters on the crystal structures and morphologies of the as-grown layers are studied. It is found that the film obtained with the tilt angle of 0.06° is more uniform. A larger applied voltage is preferred to the growth of MoS{sub 2} thin films at a certain heating time. In order to obtain the ultra-thin layers of MoS{sub 2}, the weight of 0.003 g of source materials is preferred. Under our optimal experimental conditions, the surface of the film is smooth and composed of many uniformly distributed and aggregated particles, and the ultra-thin MoS{sub 2} atomic layers (1∼10 layers) covers an area of more than 2 mm×2 mm.
Reactive sputtering of δ-ZrH{sub 2} thin films by high power impulse magnetron sputtering and direct current magnetron sputtering
Reactive sputtering by high power impulse magnetron sputtering (HiPIMS) and direct current magnetron sputtering (DCMS) of a Zr target in Ar/H{sub 2} plasmas was employed to deposit Zr-H films on Si(100) substrates, and with H content up to 61 at. % and O contents typically below 0.2 at. % as determined by elastic recoil detection analysis. X-ray photoelectron spectroscopy reveals a chemical shift of ∼0.7 eV to higher binding energies for the Zr-H films compared to pure Zr films, consistent with a charge transfer from Zr to H in a zirconium hydride. X-ray diffraction shows that the films are single-phase δ-ZrH{sub 2} (CaF{sub 2} type structure) at H content >∼55 at. % and pole figure measurements give a 111 preferred orientation for these films. Scanning electron microscopy cross-section images show a glasslike microstructure for the HiPIMS films, while the DCMS films are columnar. Nanoindentation yield hardness values of 5.5–7 GPa for the δ-ZrH{sub 2} films that is slightly harder than the ∼5 GPa determined for Zr films and with coefficients of friction in the range of 0.12–0.18 to compare with the range of 0.4–0.6 obtained for Zr films. Wear resistance testing show that phase-pure δ-ZrH{sub 2} films deposited by HiPIMS exhibit up to 50 times lower wear rate compared to those containing a secondary Zr phase. Four-point probe measurements give resistivity values in the range of ∼100–120 μΩ cm for the δ-ZrH{sub 2} films, which is slightly higher compared to Zr films with values in the range 70–80 μΩ cm.
Thin Film Multilayer Conductor/Ferroelectric Tunable Microwave Components for Communication Applications
High Temperature Superconductor/Ferroelectric (HTS/FE ) thin film multilayered structures deposited onto dielectric substrates are currently being investigated for use in low loss, tunable microwave components for satellite and ground based communications. The main goal for this technology is to achieve maximum tunability while keeping the microwave losses as low as possible, so as to avoid performance degradation when replacing conventional technology (e.g., filters and oscillators) with HTS/FE components. Therefore, for HTS/FE components to be successfully integrated into current working systems, full optimization of the material and electrical properties of the ferroelectric films, without degrading those of the HTS film; is required. Hence, aspects such as the appropriate type of ferroelectric and optimization of the deposition conditions (e.g., deposition temperature) should be carefully considered. The tunability range as well as the microwave losses of the desired varactor (i.e., tunable component) are also dependent on the geometry chosen (e.g., parallel plate capacitor, interdigital capacitor, coplanar waveguide, etc.). In addition, the performance of the circuit is dependent on the location of the varactor in the circuit and the biasing circuitry. In this paper, we will present our results on the study of the SrTiO3/YBa2Cu3O(7-delta)/LaAl03 (STO/YBCO/LAO) and the Ba(x)Sr(1-x)TiO3/YBa2Cu3O(7-delta)/LaAl03(BSTO/YBCO/ILAO) HTS/FE multilayered structures. We have observed that the amount of variation of the dielectric constant upon the application of a dc electric field is closely related to the microstructure of the film. The largest tuning of the STO/YBCO/LAO structure corresponded to single-phased, epitaxial STO films deposited at 800 C and with a thickness of 500 nm. Higher temperatures resulted in interfacial degradation and poor film quality, while lower deposition temperatures resulted in films with lower dielectric constants, lower tunabilities, and higher losses. For STO/LAO multilayer structures having STO film of similar quality we have observed that interdigital capacitor configurations allow for higher tunabilities and lower losses than parallel plate configurations, but required higher dc voltage. Results on the use of these geometries in working microwave components such as filters and stabilizing resonators for local oscillators (LO) will be discussed.
A Semiconducting Two‐Dimensional Polymer as an Organic Electrochemical Transistor Active Layer
Abstract Organic electrochemical transistors (OECTs) are devices with broad potential in bioelectronic sensing, circuits, and neuromorphic hardware. Their unique properties arise from the use of organic mixed ionic/electronic conductors (OMIECs) as the active channel. Typical OMIECs are linear polymers, where defined and controlled microstructure/morphology, and reliable characterization of transport and charging can be elusive. Semiconducting two‐dimensional polymers (2DPs) present a new avenue in OMIEC materials development, enabling electronic transport along with precise control of well‐defined channels ideal for ion transport/intercalation. To this end, a recently reported 2DP, TIIP, is synthesized and patterned at 10 µm resolution as the channel of a transistor. The TIIP films demonstrate textured microstructure and show semiconducting properties with accessible oxidation states. Operating in an aqueous electrolyte, the 2DP‐OECT exhibits a device‐scale hole mobility of 0.05 cm 2 V –1 s –1 and a µ C * figure of merit of 1.75 F cm –1 V –1 s –1 . 2DP OMIECs thus offer new synthetic degrees of freedom to control OECT performance and may enable additional opportunities such as ion selectivity or improved stability through reduced morphological modulation during device operation.