Damping properties of epoxy-based composite embedded with sol–gel-derived Pb(Zr<Subscript>0.53</Subscript>Ti<Subscript>0.47</Subscript>)O<Subscript>3</Subscript> thin film annealed at different temperatures

Pb(Zr_0.53Ti_0.47)O₃ (PZT) thin films were prepared on Pt/Ti/SiO₂/Si substrate by sol–gel method. The effect of annealing temperature on microstructure, ferroelectric and dielectric properties of PZT films was investigated. When the films were annealed at 550–850 °C, the single-phase PZT films were obtained. PZT films annealed at 650–750 °C had better dielectric and ferroelectric properties. The sandwich composites with epoxy resin/PZT film with substrate/epoxy resin were prepared. The annealing temperature of PZT films influenced their damping properties, and the epoxy-based composites embedded with PZT film annealed at 700 °C had the largest damping loss factor of 0.923.     

Dielectric properties of lead zirconate titanate thin films seeded with barium strontium titanate nanoparticles

A low temperature synthetic method recently proposed by the authors was applied to the fabrication of lead zirconate titanate (PZT) thin films containing crystalline seeds of barium strontium titanate (BST) nanoparticles. PZT precursor and the BST particles were prepared with complex alkoxide methods. Precursor solution suspending the BST particles was spin-coated on Pt/Ti/SiO₂/Si substrate to film thickness of 500–800 nm at particle concentrations of 0–25.1 mol%, and annealed at various temperatures. Seeding of BST particles prevented the formation of pyrochlore phases, which appeared at temperatures above 400 °C in unseeded PZT films, and induced crystallization of PZT into perovskite structures at 420 °C, which was more than 100 °C below the crystallization temperature of the unseeded PZT films. Measurement of dielectric properties at 1 kHz showed that the 25.1 mol% BST-seeded PZT films annealed at 450 °C had a dielectric constant as high as 300 with a dissipation factor of 0.05. Leakage current density of the film was less than 1×10⁻⁶ A/cm² at applied electric field from 0 to 64 kV/cm.     

RF sputtered PLZT thin film on Pt/Ti electrode

PLZT (7.5/65/35) thin films were deposited by rf magnetron sputtering on single crystal Si substrates using an oxide sintered target with excess PbO. The effects of postannealing and bottom Pt/Ti electrodes on the thin film crystal structures and ferroelectric properties were studied. Film deposited at 200°C or below crystallizes to a perovskite phase after annealing treatment at 550°C or above, and the crystal structure depends on the annealing treatment. The best crystal structures and electronic properties were obtained when the thin films were annealed at 600°C to 650°C for 1 h in O₂. For the Pt/Ti two-layer bottom electrode, the thickness of the Ti layer has a dominant effect. When the Ti layer was too thick or too thin, the PLZT thin film structures consist mainly of pyrochlore phases. However, using an appropriate Ti layer thickness, PLZT thin films having good crystal structures and ferroelectric properties can be obtained, with typical remanent polarization value of 220 mC/m² and coercive field strength of 6.5 MV/m     

Damping property of epoxy-based composite embedded with sol–gel-derived Pb(Zr<Subscript>0.53</Subscript>Ti<Subscript>0.47</Subscript>)O<Subscript>3</Subscript> thin film

The Pb(Zr_0.53Ti_0.47)O₃ (PZT) thin films were prepared on Pt/Ti/SiO₂/Si substrate by sol–gel method. The effect of the annealing holding time on microstructure, ferroelectric and dielectric properties was investigated. The single-phase PZT films were obtained with different annealing holding time. PZT films annealed for 30–90 min had better dielectric and ferroelectric properties. The epoxy/PZT film/epoxy sandwich composites were prepared, and the annealing holding time of PZT films influenced the damping property of the composites. The epoxy-based composites embedded with PZT films annealed for 90 min had largest damping loss factor of 0.906.     

MOD制备的PZT薄膜的相结构发展和成分分析

采用MOD工艺制备了PZT薄膜,利用XRD和TEM研究了焦绿石相向钙钛矿相的转变过程．制备在Pt／Ti／SiO₂／Si衬底上的PZT薄膜,其XRD分析显示焦绿石相在600℃完全转变为钙钛矿相;与之相比,Pt箔上无支持的PZT薄膜,其TBM分析表明PZT焦绿石相完全转变为钙钛矿相的温度更高,且与薄膜的厚度有关．XPS研究表明,薄膜表面含有化学吸附氧和污染碳,无其它杂质存在.表面富含少量Pb,其Zr／Ti比与化学计量比一致,但晶格中缺氧．     

Growth of Bi1.5MgNb1.5O7 thin films on Pt/Ti/SiO2/Si substrates by RF magnetron sputtering

In this letter, bismuth magnesium niobate (Bi_1.5MgNb_1.5O₇, BMN) thin films were deposited on Pt/Ti/SiO₂/Si substrates by using radio-frequency magnetron sputtering at various substrate temperatures. Based on the phase compositions and microstructures of these samples, we discussed the nucleation and growth of the BMN thin films and how the substrate temperature influenced these processes. The thin film begins to crystallize at 450 °C, and the annealed films were all composed of the cubic pyrochlore phase with a strong (222)-preferred orientation. The film deposited at 450 °C exhibited a large dielectric constant of 173, and a tunability of 26.6 % was obtained at a max dc bias field of 0.8 MV/cm.     

Sol-gel法制备多铁性Bi_(0.85)Eu_(0.15)FeO_3薄膜及其性能

采用Sol-gel法在Pt/Ti/SiO2/Si衬底上制备了Bi0.85Eu0.15FeO3薄膜。研究了退火温度对其晶相形成的影响,发现在较低温度退火(450℃)时,Bi0.85Eu0.15FeO3晶相开始形成,但存在杂相,而且结晶度较差;在490～600℃可以获得结晶较好的单相Bi0.85Eu0.15FeO3薄膜。同时对经550℃退火的薄膜的介电、铁电和铁磁性能进行了研究,结果表明,Bi0.85Eu0.15FeO3薄膜具有较好的介电及铁磁性能。当测试频率为1MHz时,薄膜的介电常数和介电损耗分别为80、0.024,饱和磁化强度约为26.2emu/cm3。     

Structural evaluation of sol-gel derived lead strontium titanate diffusion barrier for integration in lead zirconate titanate transducer design

Sol-gel derived Pb₄₀Sr₆₀TiO₃ (PST) thin film has been investigated as a diffusion barrier for integrating in PbZr₃₀Ti₇₀O₃ (PZT) device structures on Si substrates. PST film was deposited on SiO₂/Si substrate and annealed at a relatively low temperature range of 550-600 °C producing a crack-free, smooth and textured surface. Following deposition on PST/SiO₂/Si template PZT thin film was crystallised exhibiting random grain orientations and an insertion of the bottom Pt/Ti electrode forming PZT/Pt/Ti/PST/SiO₂/Si stacks promoted the preferred PZT (111) perovskite phase. PZT (111) peak intensity gradually decreased along with slight increase of the PZT (110) peak with increasing annealing temperature of the buffer PST film. The dielectric and ferroelectric properties of the PZT with barrier PST deposited at 550 °C were assessed. The dielectric constant and loss factor were estimated as 390 and 0.034 at 100 kHz respectively and the remnant polarisation was 28 µC/cm² at 19 V. The performance of the PZT/PST device structures was compared to similar PZT transducer stacks having widely used barrier TiO₂ layer.     

Characterization of lead zirconate titanate thin film deposition onto Pt/Ti/SiO2/Si substrates

Lead zirconate titanate, (Pb(Zr_0.52Ti_0.48)O₃PZT) thin films were deposited onto a Pt/Ti/SiO_2/Si substrate using radio frequency (r.f.) planar magnetron sputtering in this study. The deposited PZT thin films were almost amorphous before the annealing processes and developed a perovskite structure after the annealing process. If the annealing temperature was too low or annealing time too short, pyrochlore would form. However, if the annealing temperature was too high or annealing time too long, the thin film structure would degrade due to the volatilization of PbO. The significant finding in this experiment is that high quality perovskite PZT thin films on Pt/Ti/SiO_2/Si substrates can be obtained by adjusting the annealing temperature to a range of 650 °C to 850 °C and annealing time to a range from 5 to 80 min. In this experiment, the optimal annealing condition was an annealing temperature of 650 °C and time of 20 min. The properties of PZT thin film annealed at 650 °C for 20 min were dielectric constant _r = 869 free dielectric constant ^T ₃₃ = 893 piezoelectric constant d₃₃ = 2.03p m V^-1 piezoelectric constant g₃₃ = 2.57 x 10^-4 V m N^-1, remanent polarization P₁ = 112.5 nC cm^-2 and coercive field E_c= 0.061 kV cm^-1.     

Low-temperature crystallization of sol-gel-derived lead zirconate titanate thin films using 2.45 GHz microwaves

Lead zirconate titanate (PZT) thin films of thickness 420 nm were deposited on Pt/Ti/SiO₂/Si substrate using a spin coating sol-gel precursor solution, and then annealed using 2.45 GHz microwaves at a temperature of 450 °C for 30 min. The film has a high perovskite content and high crystallinity with a full width at half maximum of 0.35°. The surface roughness of the PZT thin film was 1.63 nm. Well-saturated ferroelectric properties were obtained with a remanent polarization of 46.86 μC/cm² and coercive field of 86.25 kV/cm. The film also exhibited excellent dielectric properties with a dielectric constant of 1140 and a dissipation factor of 0.03. These properties are superior to those obtained by conventional annealing at a temperature of 700 °C for 30 min.     

Bi2MoO6 dielectric thin films fabricated by thermal oxidation of Bi/Mo thin films at ultra-low temperature

Bi/Mo multilayer thin films are deposited on Si/SiO₂/Pt substrates by direct current magnetron sputtering. The effect of annealing temperature on the microstructure, dielectric and electrical properties of the as-sputtered films is characterized systematically. X-ray diffraction data indicate that the films annealed at 450–600 °C are a mixture of diphase with the main phase Bi₂MoO₆ and secondary phase Bi₂Mo₂O₉. Results of scanning electron microscope observation show that the films annealed at 500–550 °C are dense and uniform, in particular the films annealed at 500 °C exhibit optimal dielectric and electrical properties with dielectric constant as high as 37.5, dielectric loss 1.06 %, temperature coefficient of dielectric constant ?10.86 ppm °C^?1 at 1 kHz, and leakage current density of 1.46 × 10^?7 A mm^?2 at an electric field of 18.2 kV mm^?1. With the advantages of ultralow densification temperature (500 °C) and very high sputtering deposition rate (76 nm min^?1), it is anticipated that thermal oxidation method of the sputtered Bi/Mo thin films could be a promising technique for fabrication of Bi₂MoO₆ ceramic thin film embedded-capacitors.     

Structural and electrical characteristics of chemical solution derived (Bi3.2La0.4Nd0.4)Ti3O12 thin films

(Bi_3.2La_0.4Nd_0.4)Ti₃O₁₂ (BLNT) thin films were prepared on Pt/Ti/SiO₂/Si substrates by using chemical solution deposition technique, and the effects of annealing temperatures in the range of 550-750 °C on structure and electrical properties of the thin films were investigated. X-ray diffraction analysis shows that the thin films have a bismuth-layered perovskite structure with preferred (117) orientation. The surface morphology observation by field-emission scanning electron microscopy confirms that films are dense and smooth with uniformly distributed grains. The grain size of the thin films increases with increasing annealing temperature; meanwhile, the structural distortion of the thin films also increases. It was demonstrated that the thin films show good electrical properties. The dielectric constant and dielectric loss are 191 and 0.028, respectively, at 10 kHz for the thin film annealed at 600 °C, and the 2Pr value of the thin film annealed at 700 °C is 20.5 μC/cm² at an electric field of 500 kV/cm.     

Drying temperature effects on microstructure, electrical properties and electro-optic coefficients of sol-gel derived PZT thin films

Transparent lead zirconium titanate (PZT) thin film is suitable for a variety of electro-optic application, and the increasing of the electro-optic coefficient of PZT film is one of the important factors for this application. In this study, the main processing variable for improving an electro-optic coefficient was the drying temperature: 300, 350, 450 and 500°C in sol-gel derived PZT thin films. The highest linear electro-optic coefficient (1.65×10⁻¹⁰ (m/V)) was observed in PZT film dried at 450°C. The PZT film showed the highest perovskite content, polarization (P_max=49.58 μC/cm², P_r=24.8 μC/cm²) and dielectric constant (532). A new two-beam polarization (TBP) interferometer with a reflection configuration was used for electro-optic testing of PZT thin films which allows measurement of the linear electro-optic coefficient of thin film with strong Fabry–Perot (FP) effect usually present in PZT thin film.     

Micropore formation in lead zirconate titanate films

This paper presents an experimental study of the pyrochlore-to-perovskite phase transition in ferroelectric lead zirconate titanate (PZT) films grown on silicon substrates by rf magnetron sputtering and annealed in air or in an inert (argon) atmosphere at temperatures of up to 600°C and atmospheric pressure. Simultaneous thermal analysis results demonstrate that annealing in air leads to release of the latent heat of the phase transition, which is due to the conversion of lead oxide to lead orthoplumbate in the bulk of the PZT film. This transition is accompanied by changes in the densities of the perovskite phase and parent (pyrochlore) phase. In this case, the possibility of phase transformation should be ensured by changes in the volume of the system. The change in the volume of the film leads to the formation of micropores in the bulk of thin PZT films. The micropore size has been determined by scanning electron microscopy, and the phase composition of the films has been assessed by X-ray diffraction. We present experimental evidence that micropore nucleation and growth at the interface between the new and old phases in thin PZT films is due to the difference in density between these phases.     

Growth mechanism of chemical solution derived PZT films on MgO(100) substrate

PZT (Zr : Ti = 0.53 : 0.47) thin films were fabricated by chemical solution deposition with metal naphthenates used as starting materials. Effect of final annealing temperature on epitaxy and surface morphology of the films were investigated. PZT films prefired at 200°C were crystallized to be highly (00l)/(h00)-oriented at final annealing temperatures of 750°–800°C. The film annealed at 750°C was smooth and no distinct texture was exhibited, while the rosette-type microstructure caused by lead volatilization was observed in the films after annealing at 800°C.     

PZT thin film preparation by pulsed DC magnetron sputtering

Pulsed DC magnetron sputtering was used in this study to prepare lead zirconate titanate (Pb(Zr_xTi_1−x)O₃, PZT) thin films. A single metallic target was used for the deposition onto a Pt/Ti/SiO₂/Si substrate and parameters such as: pulse frequency, duty cycle, O₂/Ar flow ratio controlled so as to analyze the effect of the parameters on thin film deposition rate, crystalline structure and morphology. After the deposition, the thin film was annealed in a rapid thermal annealing (RTA) furnace. The experimental results showed that, when the pulse frequency was in the range of 10 kHz-100 kHz, along with the lowering of frequency and the oxygen argon flow rate ratio, the deposition rate gradually increased and the formation of PZT thin film perovskite phase was enhanced; however, if the oxygen argon flow rate ratio was too high, it caused the PZT thin film to generate a pyrochlore phase. However, when the duty cycle was in the range of 95%-75%, the highest deposition rate and better perovskite phase could be obtained in the range of 75%-80%.     

Growth of perovskite PZT and PLZT thin films

This paper reports preliminary results on the fabrication of perovskite PZT and PLZT thin films using a sputtering technique. For glass, quartz and sapphire substrates, it was necessary to raise the substrate temperature above 550 ° C to achieve perovskite tetragonal structures of interest. Growth at temperatures below 550 ° C yielded a major pyrochlore structure phase. Excess of PbO in the target was also required to maintain stoichiometry in these films.     

Gold island films on indium tin oxide for localized surface plasmon sensing

Mechanically, chemically and optically stable gold island films were prepared on indium tin oxide (ITO) substrates by direct thermal evaporation of thin gold films (2-6?nm) without the need for pre-?or post-coating. The effect of mild thermal annealing (150?°C, 12?h) or short high temperature annealing (500?°C, 1?min) on the morphology of the gold nanostructures was investigated. ITO covered with 2?nm gold nanoislands and annealed at 500?°C for 1?min was investigated for its ability to detect the adsorption of biotinylated bovine serum albumin using local surface plasmon resonance (LSPR), and its subsequent molecular recognition of avidin.     

Optical properties of pb(Zr,Ti)O(3) films prepared by aerosol deposition

The optical properties and related band structure of ferroelectric lead zirconate titanate [PZT, Pb(Zr0(0.6)Ti0(0.4))O(3)] films prepared on glass substrates at room temperature by aerosol deposition were investigated. The reflectance and transmittance of the PZT films were measured in the wavelength range from UV to nearinfrared. The measured optical spectra were analyzed using dielectric function models that describe optical transitions in the band gap region. Optical absorption of the as-deposited PZT films was found to be larger than that of the annealed PZT films in the near-infrared wavelength range. The analyzed results indicated that post-deposition annealing increased the band gap energy of the PZT films, corresponding to a decrease in optical absorption.     

退火温度对Pb(Zr_(0.53)Ti_(0.47))O_3薄膜结构及其性能的影响

采用sol-gel法在Pt/Ti/SiO_2/Si衬底上制备Pb(Zr_(0.53)Ti_(0.47))O_3薄膜.利用X射线衍射仪(XRD)和原子力显微镜(AFM)对其晶格结构和微观形貌进行了表征,通过改变退火温度制得了具有单一钙钛矿结构的Pb(Zr_(0.53)Ti_(0.47))O_3薄膜.然后将该薄膜与环氧树脂形成复合结构材料.对其铁电性能以及复合材料的阻尼性能进行了测试,结果表明,退火温度的升高有利于改善薄膜的铁电性能,在750℃下退火的Pb(Zr_(0.53)Ti_(0.47))O_3薄膜,其剩余极化值2Pr达到了68.6μC/cm~2, 矫顽场强2E_c达到158.7kV/cm;同时退火温度的升高还有利于薄膜致密度的提高,对复合材料的阻尼性能也有一定的改善,当退火温度达到800℃,复合材料的阻尼损耗因子达到最大值,阻尼温域最宽,阻尼性能最好.