Electrostatic force microscopy study on the domain switching properties of the Pb(Zr0.2Ti0.8)O3 thin films with different crystallographic orientations for the probe-based data storage

The domain switching properties of the ferroelectric Pb(Zr(0.2)Ti(0.8))O(3) (PZT) thin films with two types of crystallographic orientations were investigated by electrostatic force microscopy (EFM). The crystallographic orientations of the PZT thin films were random on the (111)Pt/MgO(100) and c-axis preferred on the (100)Pt/MgO(100), respectively. When dc bias was applied to the films for writing in micro-scale area, electrostatic force images showed that the domain switching was hard in the PZT thin films with random orientation, while the pattern could clearly be written in the PZT films with c-axis orientation. The differences in the domain switching properties of each PZT thin film were investigated in the crystallographic orientations point of view, and the domain switching dynamics were also measured by investigating the nano-sized dot switching behavior with respect to the width of the applied voltage pulse.     

Grain boundary enrichment in the FePt polymorphic A1 to L10 phase transformation

A series of Fe_54±1Pt_46±1 thin films have been sputter-deposited and annealed at various times and temperatures to facilitate the A1 to L1₀ polymorphic phase transformation. The annealing times span one minute to tens of minutes over temperatures of 300–800 °C. The films were characterized by X-ray and electron diffraction and atom probe tomography. This time–temperature regime provides ‘snap-shots’ into the compositional segregation evolution at the grain boundaries during the polymorphic phase transformation. The as-deposited A1 phase showed a preferential segregation of Pt to the grain boundaries. The reduction of Pt enrichment at the boundaries was observed for all L1₀ ordered films.     

Structural properties of 0.65Pb(Mg1/3Nb2/3)O3–0.35PbTiO3 relaxor ferroelectric thin films on SrRuO3 conducting oxides

Coating of 0.65Pb(Mg_1/3Nb_2/3)O₃–0.35PbTiO₃ (PMN–PT) relaxor ferroelectrics by a sol–gel method is followed by growth of epitaxial SrRuO₃ (SRO) metallic oxide electrodes on SrTiO₃ (STO) single-crystal substrate by pulsed laser deposition. High-quality PMN–PT films on SRO with preferred growth orientation were successfully fabricated by controlling the operation parameters. Structural properties of relaxor ferroelectric PMN–PT thin films on SRO/STO substrates have been studied by X-ray diffraction (XRD), transmission electron microscopy (TEM) and atomic force microscopy (AFM). In-plane and out-of-plane alignments of the heterostructure are confirmed and the structural twinning of the materials are also revealed.     

High load AFM friction and wear experiments on V2O5 thin films

High load friction and wear experiments by means of atomic force microscopy were carried out at the surface of highly (0 0 1) oriented vanadium oxide V₂O₅ thin films deposited on silicon by reactive magnetron sputtering. Microscopic friction coefficient was estimated for wide range of loads. The nature of surface wear due to multiple, high load scanning is presented and discussed.     

Structural analyses of Nd-doped CeO2 thin films deposited by pulsed laser deposition

CeO₂ thin films doped with neodymium oxides for application to gas sensors have been elaborated by the pulsed laser deposition technique. The films were deposited on orientated Si (100) substrates with variable deposition times (t = 90, 180 and 360 s) and molar fractions of Nd₂O₃ (0, 6.5, 15, 21.5 and 27 at.%). The resulting Nd–CeO₂ thin films were characterized by means of X‐ray diffraction analysis, scanning electron microscopy and transmission electron microscopy equipped with EDS (Energy Dispersive Spectrometer) microanalysis. From X‐ray diffraction analyses, it is clearly established that the texture is modified by Nd additions. The preferred (111) orientations of the CeO₂ crystals change into the (200) orientation. The morphology of the CeO₂ grains changes from triangles, for pure CeO₂ thin films, to spherical grains for Nd‐doped films. In addition, cell parameter analyses from X‐ray diffraction data show that a partial chemical substitution of Ce by Nd should occur in the face‐centred cubic lattice of ceria: this should give rise to Ce_1‐xNd_xO_2?z phases with oxygen non‐stoichiometry.     

Thermal sensors based on p-Pb0.925Yb0.075Te:Te and n-Pb0.925Yb0.075Se0.2Te0.8 thin films grown using thermal evaporation method

We utilize p-Pb_0.925Yb_0.075Te:Te and n-Pb_0.925Yb_0.075Se_0.2Te_0.8 ingots in a standard solid-state microwave synthesis route to fabricate thermally evaporated thin films. The nanostructure and composition of the films were studied through X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and energy dispersive X-ray spectroscopy (EDX). The Seebeck coefficient and electrical conductivity were measured at a temperature range of 298–523 K. The micro-thermoelectric devices were composed of 20 pairs and 10 pairs of p-Pb_0.925Yb_0.075Te:Te and n-Pb_0.925Yb_0.075Se_0.2Te_0.8 thin films on glass substrates, respectively. The dimensions of the thin films thermoelectric generators which comprised of 10-pair were 12 mm × 10 mm, whereas, 20-pair were 23 mm × 20 mm, respectively of legs connected through aluminum electrodes. The serial 20-pair p–n thermocouples generated a maximum output open-circuit voltage of 275.3 mV and a maximum output power of 54.37 nW at a temperature difference of ΔT = 162 K; the values are 109.4 mV and 16.68 nW at ΔT = 162 K for the 10-pair thermocouples, respectively.     

Characterization and mechanical/tribological properties of nano Au-TiO2 composite thin films prepared by a sol-gel process

Nano Au-TiO₂ composite thin films on Si(1 0 0) and glass substrates were successfully prepared with a facile sol-gel process followed by sintering. The morphology and mircostructure of the films were investigated via X-ray diffractometry (XRD), X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), and scanning electron microscopy (SEM). The Au particles, of diameter 14-22 nm depending on the sintering temperatures used, were found to be well dispersed in the TiO₂ matrix, with a small amount of the particles escaped from the film. The surfaces of the films were uniform, compact and crack-free. Hardness and elastic modulus of the films were measured by using the nanoindentation technique. Friction and wear properties were investigated by using a one-way reciprocating tribometer. It was found that the highest hardness and elastic modulus values were obtained for the films prepared with 500 °C sintering temperature. The films displayed superior antiwear and friction reduction performances in sliding against an AISI 52100 steel ball. With 5.0 mol% Au, the friction coefficient was only 0.09-0.10 and the wear life was more than 2000 sliding cycles. The friction coefficient and wear life decreased with increasing sliding speed and load. The failure mechanism of the Au-TiO₂ films was identified to be light scuffing and abrasion. Those films can be potentially applied as ultra-thin lubricating coatings.     

厚度效应对Pb(Zr0.53Ti0.47)O3薄膜微结构、铁电、介电性能的影响

用改进的溶胶-凝胶法在Pt(111)/Ti/SiO₂/Si(100)衬底上制备了不同厚度的高度(111)取向的Pb(Zr_0.53Ti_0.47)O₃薄膜.运用X射线衍射(XRD)和原子力显微镜(AFM)分析了薄膜的微结构,原子力显微镜表明厚度为0.3μm和0.56μm的PZT薄膜的晶粒尺寸和表面粗糙度分别为0.2～0.3μm、2～3μm和0.92nm、34nm.0.3μm和0.56μm PZT薄膜的剩余极化(Pr)和矫顽场(Ec)分别为32.2μC/²、79.9kV/cm, 27.7μC/cm²、54.4kV/cm;在频率100KHz时,薄膜的介电常数和介电损耗分别为539、0.066,821、0.029.     

Molecular dynamics study of optimal packing structure of OTS self-assembled monolayers on SiO2 surfaces

Optimal packing structure of Octadecyltrichlorosilane (OTS) self-assembled monolayer (SAM) adsorbed on a SiO₂ (1 0 0) surface with a Si substrate was studied performing molecular dynamics (MD) computational simulations. Molecular substitution, substitution pattern and molecular orientation of the OTS molecules on the SiO₂ (1 0 0) are the main factors studied in order to determine the optimal packing structure taking into account energetic balance. We have used the optimal packing structure to study other properties usually used to characterize SAMs as molecular and system tilt angles, film thickness and gauche defects. These properties and monolayer stability were studied performing MD simulations in a temperature range from 100 to 600 K and we found that results obtained agree with those from experimental measurements. We found that OTS films are stable up to 500 K. The optimal structure obtained could be used in further MD simulations studies in order to determine tribological properties of OTS–SiO₂ systems.     

Dynamics of space and polarization charges of ferroelectric thin films measured by atomic force microscopy

Retention behavior and local hysteresis characteristics in Pb(Zr(0.52)Ti(0.48))O(3) (PZT) thin films on Pt electrodes have been investigated by electrostatic force microscopy (EFM). A sol-gel method is used to synthesize PZT thin films and drying conditions are carefully explored over a wide range of temperature. Decay and retention mechanisms of single-poled and reverse-poled regions of the ferroelectric thin films are explained by space charge redistribution. Trapping behavior of space charges is dependent on the nature of interface between ferroelectric thin films and bottom electrodes. Local measurement of polarization-electric field curves by EFM shows inhomogeneous space charge entrapment.     

Characterization of nanoscale recording mark on Ge2Sb2Te5 film

We have fabricated nanoscale recording marks on Ge₂Sb₂Te₅ (GST) films with conductive atomic force microscope (AFM). GST films were deposited on glass or polyimide film with thickness of 150–200 nm by the rf–sputtering method. Through current–voltage (I–V) spectroscopy, good cantilevers for fabrication and characterization of nanoscale marks on GST were selected. A fresh and highly conductive tip showed voltage-switching characteristic in the I–V curve, where the threshold voltage was 1.6 V. Nanoscale dot and wire arrays of crystalline phases were successfully obtained by varying sample bias voltage from −10 to 10 V. With highly conductive tips, nanowires having full-width at half-maximum of 20 nm could be fabricated, whereas nanowires could not be fabricated with bias voltage below −2 V. The width of the nanoscale mark was increased by repetition of AFM lithography even with same applied voltage and lithography speed. For a thicker nanowire, the width measured in current-image (C-image) was observed to be 2 times of that measured in topography-image (T-image). This result supports that current sensing provides an image of phase-changed GST area with higher resolution than topography sensing.     

A study on friction and wear characteristics of nanometer Al2O3 /PEEK composites under the dry sliding condition

The friction and wear properties of the polyetheretherketone (PEEK) based composites filled with 5 mass% nanometer or micron Al₂O₃ with or without 10 mass% polytetrafluroethylene (PTFE) against the medium carbon steel (AISI 1045 steel) ring under the dry sliding condition at Amsler wear tester were examined. A constant sliding velocity of 0.42 m s⁻¹ and a load of 196 N were used in all experiments. The average diameter 250 μm PEEK powders, the 15 or 90 nm Al₂O₃ nano-particles or 500 nm Al₂O₃ particles and/or the PTFE fine powders of diameter 50 μm were mechanically mixed in alcohol, and then the block composite specimens were prepared by the heat compression moulding. The homogeneously dispersion of the Al₂O₃ nano-particles in PEEK matrix of the prepared composites was analyzed by the atomic force microscopy (AFM). The wear testing results showed that nanometer and micron Al₂O₃ reduced the wear coefficient of PEEK composites without PTFE effectively, but not reduced the friction coefficient. The filling of 10 mass% PTFE into pure PEEK resulted in a decrease of the friction coefficient and the wear coefficient of the filled composite simultaneously. However, when 10 mass% PTFE was filled into Al₂O₃/ PEEK composites, the friction coefficient was decreased and the wear coefficient increased. The worn scars on the tested composite specimen surfaces and steel ring surfaces were observed by scanning electron microscopy (SEM). A thin, uniform, and tenacious transferred film on the surface of the steel rings against the PEEK composites filled with 5 mass% 15 nm Al₂O₃ particles but without PTFE was formed. The components of the transferred films were detected by energy dispersive spectrometry (EDS). The results indicated that the nanometer Al₂O₃ as the filler, together with PEEK matrix, transferred to the counterpart ring surface during the sliding friction and wear. Therefore, the ability of Al₂O₃ to improve the wear resistant behaviors is closely related to the ability to improve the characteristics of the transfer film.     

Morphological properties of sputtered MoS2 films

As the lubricating properties of MoS₂ are due to the sliding of lamellae, the crystallographic orientation and structural properties of these lamellae are important for the tribological behaviour. Thus an analysis of the growth morphology of sputtered MoS₂ films was carried out. It is shown that morphological properties can be influenced by the parameters of the deposition process; in particular, it is possible to prepare coatings in which the lamellae are oriented parallel to each other.     

A study of the initial growth of PtxCo(1−x) thin films on Si3N4

Pt _x Co_{(1− x )} thin films where x  =0.24 have been deposited onto Si₃N₄ windows and studied using transmission electron microscopy. The films are used in ultrahigh-density recording studies and it was found that the surface of the substrate had a strong influence on the microstructure, crystallography and magnetic properties of the film. An investigation of the early growth of the film was made by studying films of different thickness between 100 and 300 Å. It was found that the grains were hexagonal in structure with a strong c -axis orientation perpendicular to the surface.     

Atomic-scale anisotropy of nanoscratch behavior of single crystal iron

In this paper a parallel molecular dynamics (MD) model has been developed to investigate the nanoscratch process of single crystal iron. The simulations were performed for two cases with different crystallographic orientations and scratch directions. In Case I the scratch plane is (1 0 0) and the scratch direction is [0 0 1]. In Case II the scratch plane and the scratch direction are (1,−1,2) and [1 1 1], respectively. To validate the MD simulation the nanoscratch testing was conducted using the TriboIndenter. The simulation results reveal that the vertical force and the lateral force tend to increase with the scratch displacement for both cases. Case I has smaller forces than Case II. However, the coefficient of friction for both cases is similar, which is in good agreement with the experimental value. The crystallographic orientation also affects the scratch hardness. The scratch hardness of Case I is smaller than that of Case II.     

Characterization of lead zirconate titanate--lanthanum ruthenate thin film structures prepared by chemical solution deposition

In this work, the results of compositional and microstructural analysis of lead zirconate titanate--lanthanum ruthenate thin film structures prepared by chemical solution deposition are discussed. The cross-section transmission electron microscope (TEM) micrographs of the La-Ru-O film deposited on a SiO2/Si substrate and annealed at 700 degrees C revealed RuO2 crystals embedded in a glassy silicate matrix. When the La-Ru-O film was deposited on a Pt/TiO2/SiO2/Si substrate, RuO2 and La4Ru6O19 crystallized after annealing at 700 degrees C. After firing at 550 degrees C randomly oriented lead zirconate titanate (PZT) thin films crystallized on the La-Ru-O/SiO2/Si substrate, while on La-Ru-O/Pt/TiO2/SiO2/Si substrates PZT thin films with (111) preferred orientation were obtained. No diffusion of the Ru atoms in the PZT film was found. Ferroelectric response of PZT thin films on these substrates is shown in comparison with the PZT film deposited directly on the Pt/TiO2/SiO2/Si substrate without a La-Ru-O layer.     

Influence of substrate orientation on the morphologyand orientation of LaNiO3 thin films

LaNiO₃ thin films were successfully prepared by a chemical method from citrate precursors. The LNO precursor solution was spin‐coated onto Si (100) and Si (111) substrates. To obtain epitaxial or highly oriented films, the deposited layers were slowly heated in a gradient thermal field, with a heating rate of 1° min^?1, and annealed at 700°C. The influence of different substrate orientations on the thin film morphology was investigated using atomic force microscopy and X‐ray diffraction analysis. Well‐crystallized films with grains aligned along a certain direction were obtained on both substrates. Films deposited on both substrates were very smooth, but with a different grain size and shape depending on the crystal orientation. Films deposited on Si (100) grew in the (110) direction and had elongated grains, whereas those on Si (111) grew in the (211) direction and had a quasi‐square grain shape.     

High-temperature tribological properties of spark-plasma-sintered Al2O3 composites containing barite-type structure sulfates

Al₂O₃–50BaSO₄–20Ag, Al₂O₃–50BaSO₄–10SiO₂, Al₂O₃–50(mass%)SrSO₄, Al₂O₃–50PbSO₄–5SiO₂, Al₂O₃–50BaSO₄ and Al₂O₃–50BaCrO₄ composites (mass%) were prepared by spark plasma sintering and their microstructure and high-temperature tribological properties were evaluated. Al₂O₃–50BaSO₄–20Ag composites (mass%) showed the lowest friction coefficients at the temperature ranging from 473 to 1073 K. Thin Ag film was observed on the wear tracks of the composites above 473 K. In addition, the friction coefficients of Al₂O₃ composites containing SrSO₄ and PbSO₄ were as low as those of Al₂O₃–BaSO₄ and Al₂O₃–BaCrO₄ composites at the temperatures up to 1073 K. The thin films formed on the wear tracks of the Al₂O₃–SrSO₄ composites were composed of Al₂O₃ and SrSO₄ phases, while the films formed on the wear tracks of the Al₂O₃–PbSO₄–SiO₂ composites consisted of Al₂O₃, PbSO₄ and SiO₂ phases.     

Deposition and Nanotribological Characterization of Sub-100-nm Thick Protective Ti-Based Coatings for Miniature Applications

Ti-based protective thin films with thicknesses below 100 nm, intended for miniature applications were deposited using physical vapor deposition magnetron sputtering. X-ray diffraction (XRD), scanning electron microscopy, and atomic force microscopy were employed for the assessment of microstructure, morphology, film thickness, surface topography, and roughness. XRD pattern showed the formation of f.c.c TiN, TiCN, and TiC phases with different preferred orientations for films prepared in Ar/N₂, Ar/N₂ + C₂H₂, and Ar/C₂H₂ gas mixtures, respectively. Nanotribological performance was investigated using multipass nanoscratch technique at variable applied normal loads (100–400 μN). The nanoscale coefficient of friction was found to be in the 0.08–0.1 range, a sufficiently low value showing the potential of these films for miniature applications, such as microelectromechanical systems. The nanowear resistance at mean contact pressures in the range of 5–8.5 GPa for each sample was evaluated in terms of the average residual wear depth and an abrasive-dominated wear mechanism was found.     

SnSe2薄膜的载流子与声子动力学研究

基于自建的超快抽运探测实验系统,研究了化学气相沉积法生长的SnSe₂薄膜的超快载流子与声子动力学。对SnSe₂薄膜随抽运能量密度变化的载流子弛豫过程的测量结果表明该薄膜具有超快的载流子热化过程和皮秒至纳秒时间尺度的复合过程。伴随着光生载流子的超快激发和能量弛豫,SnSe₂薄膜发生晶格热化,产生了特定频率的相干声学声子。通过分析声学声子振荡信号随抽运能量密度变化的规律,揭示了SnSe₂薄膜产生的相干声学声子的特性。研究结果对SnSe₂薄膜在光电器件领域的应用研究具有一定的参考价值。