Magnetoelectric composite thick films of PZT–PMnN + NiZnFe2O4 by aerosol-deposition

Highly dense magnetoelectric composite films with 10 μm-thick of high piezoelectric voltage coefficient material, 0.9Pb(Zr₅₇Ti₄₃)O₃–0.1Pb(Mn_1/3Nb_2/3)O₃ (PZT–PMnN) and magnetostrictive material, Ni_0.8Zn_0.2Fe₂O₄ (NZF), were fabricated on a platinized Si substrate using aerosol deposition (AD). With increasing magnetic NZF content, dielectric and ferroelectric properties were gradually decreased while magnetizations were improved. The 20% NZF added composite thick film were found to exhibit the maximum ME coefficient. This optimal NZF content is the same as that of bulk ME composite materials. It is noticeable that AD can control the content ratio of ME composite films by controlling the powder composition. The fabricated ME composite films have high ME voltage coefficient coupling because of high density without severe inter-reactions of two phases.     

Electrical properties of high density PZT and PMN–PT/PZT thick films produced using ComFi technology

To achieve high actuation forces in piezoelectric film actuators and transducers it is desirable to have relatively thick films. Sol-gel derived films are often limited in the maximum thickness that is obtainable due to the increased probability of cracking and delamination during processing. Composite film (ComFi) technology combines conventional sol-gel processing with ceramic powder processing to enable thick (>2 μm) ferroelectric films to be deposited onto silicon substrates at temperatures as low as 710 °C. Ten micrometre thick films have been fabricated using three different piezoelectric powders [hard doped PZT, soft doped PZT and PMN–PT(85–15)]. The resultant films have high densities with relative permittivities of 800, 900 and 1800, respectively. The d₃₃ piezoelectric coefficients were found to be lower than corresponding values for the bulk material. This has been attributed to a combination of small grain size and the clamping effects of the rigid substrate. Hysteresis loop measurements show that greater fields are required to achieve a similar degree of polarisation to that of the bulk material. This indicates that the presence of the substrate also affects the ability to pole the material so further reducing the observed piezoelectric coefficient.     

Effect of annealing temperature on ferroelectric electron emission of sol–gel PZT films

In this work, the influence of annealing temperature on the ferroelectric electron emission behaviors of 1.3-μm-thick sol–gel PbZr_0.52Ti_0.48O₃ (PZT) thin film emitters was investigated. The results revealed that the PZT films were crack-free in perovskite structure with columnar-like grains. Increasing annealing temperature led to the growth of the grains with improved ferroelectric and dielectric properties. The remnant polarization increased slightly from 35.3 to 39.6 μC/cm² and the coercive field decreased from the 56.4 to 54.6 kV/cm with increasing annealing temperature from 600 to 700 °C. The PZT film emitters exhibited remarkable ferroelectric electron emission behaviors at the threshold voltage above 95 V. The film annealed at 700 °C showed a relatively lower threshold voltage and higher emission current, which is related to the improved ferroelectric and dielectric properties at higher annealing temperature. The highest emission current achieved in this work was around 25 mA at the trigger voltage of 160 V.     

Preparation of multi-coating PZT thick films by sol–gel method onto stainless steel substrates

PbZr_0.45Ti_0.55O₃ ferroelectric films have been prepared by sol–gel method, using alkoxide precursor compounds and multi-layer technique. The gel films were deposited by spin-coating onto stainless steel substrates. In order to obtain crystallization in the perovskite phase, the samples were annealed at 600–700°C for 1 min. The dependence of the electric properties on the heat-treatment temperature is studied, and the coercive electric field as a function of the material thickness is determined. By SEM photography, the microstructure of the films could be shown to be homogeneous.     

Phase,microstructure and ferroelectric properties of new complex-structured ferroelectric ceramics in the PZT–SBN system

This study aimed to fabricate and characterize new complex-structured ceramics with formula (1-x)Pb(Zr_0.52Ti_0.48)O₃–xSrBi₂Nb₂O₉ or (1-x)PZT–xSBN (where x=0, 0.1, 0.3 and 0.5 weight fraction). The ceramics were prepared by a solid-state mixed-oxide method and sintered at temperatures between 1000 and 1250 °C. Optimum sintering temperature for this system was found to be 1050 °C for 3 h dwell time. X-ray diffraction patterns of (1-x)PZT–xSBN powders showed peak intensities of two-phase mixture corresponding to the relative amount of each phase as a result of SBN addition. Microstructure of (1-x)PZT–xSBN ceramics showed a variation in grain shape and grain size. The small addition of SBN (x=0.1) was also found to improve ferroelectric properties of pure PZT ceramic.     

Electrocaloric and pyroelectric properties of PZT and PMN–PNN–PZT thin films

The electrocaloric effects (EC) of PZT and PMN–PNN–PZT films were evaluated. PZT and PMN–PNN–PZT thin films with a thickness of 500 nm were fabricated by state-of-the-art chemical solution deposition from a precursor solution with PZT and (PMN?PNN)/PZT=30/70. The polarization hysteresis loop was found to be slim and nonlinear, with smaller hysteretic behavior compared with PZT. The pyroelectric properties evaluated from polarization change and current measurement show that the properties of PMN–PNN–PZT films are superior to those of non-doped PZT films. The electrocaloric temperature changes ΔT due to applied ΔE were calculated. PZT and PMN–PNN–PZT films exhibited ΔT of 2.1 K and 3.6 K at 237.5 °C under a field of 500 kV/cm, respectively. Thermal-electrical energy converters based on pyroelectric effects were investigated for energy harvesting and possible use in ultralow-power sensor modules. The possibilities of pyroelectric energy harvesting using these PZT films were also investigated.     

Understanding ferroelectric performances of spin-coated odd–odd nylon thin films

Ferroelectric properties of organic odd–odd nylon spin-coated thin films are investigated. Nylon 11-11, 9-13, and 11-13 are prepared by melt polymerization of the nylon salt consisting of the corresponding dicarboxylic acid and diamine. The obtained nylon is spin coated to obtain thin films with the thicknesses in the range of 85–108 nm. After spin coating, the sample films are subjected to several thermal history procedures, namely the films are either melt quenched or thermally annealed at various temperatures. The melt-quenched films are in the γ crystal phase that is directly related to the ferroelectricity of the sample thin films. Enhanced ferroelectricity is measured for the sample films that are thermally annealed at 165 °C. The remanent polarization is significantly affected by the crystallite size. Ferroelectric switching of the thin films is studied by applying a sinusoidal voltage with the frequencies of 1, 10, 100, 1 k, and 10 kHz. The switching speed is evaluated from the full width at half-maximum of the switching current. A switching speed of 4.7 × 10³ s⁻¹ (switching time of 210 μs) is measured for 1 kHz switching. The remanent polarization is strongly decreased by increasing the switching frequency, whereas the coercive field is increased. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47595.     

Magnetoelectric effect in composite structures based on ferroelectric–ferromagnetic perovskites

Composite structures based on ferroelectric BaTi_0.85Sn_0.15O₃ and Ba_0.996Y_0.004TiO₃ substrates and La_0.775Sr_0.225MnO₃ films deposited on them, which have a perovskite structure, have been prepared. The effect of different methods of film deposition on the properties of films has been studied. A detailed analysis and comparison of electrophysical properties and structure of ceramic and film ferromagnetics prepared by different methods has been carried out. The effect of the chemical composition of the substrate on the temperature of phase transition in manganite films has been studied. The possibility to control the magnetoresistivity of ferromagnetic films by electric field has been shown.     

Electrophoretic deposition of functionally-graded NiO–YSZ composite films

Functionally-graded NiO–8 mol % YSZ composite films were prepared by a controlled voltage-decay electophoretic deposition (EPD) process. The films consisted of three layers with varying NiO concentrations and porosities. Effects of different parameters including the type of the organic media, solid concentration, NiO:YSZ ratio, and iodine on the stability of EPD suspensions and deposition kinetics were studied. A stable NiO–YSZ suspension was attained in isopropanol with NiO–YSZ ratio of 60:40 and iodine concentration of 0.5 mM. The composite film contained varying NiO concentration from 46 wt.% near the substrate to 32 wt.% close to the electrolyte with 42 wt% NiO in the intermediate region. The thickness of each layer is about 10, 44 and 68 μm, respectively. The prepared anode could be promising for solid oxide full cells as it compromises good contact to the electrode with higher corrosion resistance and active reaction zone with the electrolyte.     

Self-polarized ferroelectric PVDF homopolymer ultra-thin films derived from Langmuir–Blodgett deposition

It was found that Langmuir–Blodgett (LB) deposition process led to the direct formation of ferroelectric β phase in poly(vinylidene fluoride) (PVDF) homopolymer ultra-thin films, in which the molecular chains were parallel to the substrates and the dipoles were aligned perpendicular to the substrates. Theoretical analysis and experimental results further showed that the mechanism of forming the β phase and the dipole orientation were attributed to the hydrogen bonds formed between the PVDF molecules and water through the LB deposition. A large local effective piezoelectric coefficient (d_zz) of ?49.4 pm/V was observed in the self-polarized PVDF LB film.     

Microstructure and texture of polycrystalline 3C–SiC thick films characterized via EBSD

Cubic silicon carbide (3C–SiC) is an excellent protective film on graphite and has been fabricated via laser chemical vapor deposition (LCVD) with an extremely high deposition rate by our research group. To understand comprehensively its growth behavior, the polycrystalline 3C–SiC thick films with the preferred orientation of <111> and <110> were characterized by diverse measurements, especially electron back-scatter diffraction (EBSD). Along the growth direction of the <110>-oriented 3C–SiC, the microstructure changed from equiaxed grains to elongated grains with <111> orientation, and eventually the <110>-oriented columnar grains. The stacking faults in the <110>-oriented 3C–SiC could be marked as <11–20>-oriented 6H–SiC. On the other hand, in the <111>-oriented 3C–SiC films, the microstructure changed from mainly equiaxed grains to large columnar grains. The high-density stacking faults in <111>-oriented 3C–SiC films may lead to the identification of the nominal 2H, 4H and 6H polytypes by Raman spectra and EBSD. The (0001) planes of 2H-, 4H–SiC are perpendicular to the growth direction, while that of 6H–SiC are parallel.     

‘纯’和‘净’与紫砂

紫砂在很大程度上是要寻求一种,不容许有丝毫瑕疵,如同人们对玉的品质要求一样。     

‘纯’和‘净’与紫砂

紫砂在很大程度上是要寻求一种,不容许有丝毫瑕疵,如同人们对玉的品质要求一样。     

2，4，4‘’‘’—三氯—2‘’‘’—羟基二苯醚的合成

2，4，4'—三氯—2'—氨基二苯醚经浓H2S04与NaNO2形成的亚硝酰硫酸重氮化，重氮盐在75％H2S04与溶剂组成的混合物中水解，产物的红外光谱和质谱分析表明，2，4，4'—三氯—2'—羟基二苯醚的合成是成功的。研究了重氮化剂浓度和溶剂种类对合成反应的影响，采用15-22％的亚硝酰硫酸重氮化，在浓硫酸用量大幅度减少的情况下，收率提高，达36．5％；邻二氯苯为合适的水解溶剂。     

Boosting lithium-ion transport capability of LAGP/PPO composite solid electrolyte via component regulation from ‘Ceramics-in-Polymer’ to ‘Polymer-in-Ceramics'

The design and regulation of the ion transport channels in the polymer electrolyte is an important means to improve the lithium ion transport behavior of the electrolyte. In this work, we for the first time combined the high ionic conductive inorganic ceramic electrolyte Li_1.5Al_0.5Ge_1.5(PO₄)₃ (LAGP) with flexible polypropylene oxide (PPO) polymer electrolyte to synthesize a high-filling LAGP/PPO composite solid electrolyte film and regulated the ion transport channels from ‘Ceramics-in-Polymer’ mode to ‘Polymer-in-Ceramics' mode by optimizing the ratio of LAGP vs. PPO. The results reveal that when the LAGP content <40%, the electrolyte belongs to ‘LAGP-in-PPO’, and then changes to ‘PPO-in-LAGP’ when the LAGP content exceeds 40%. Compared with ‘LAGP-in-PPO’, the ‘PPO-in-LAGP’ shows better comprehensive properties, especially for the 75% LAGP-filled PPO electrolyte, the room-temperature ionic conductivity is as high as 3.46 × 10^?4 Scm^?1, the ion migration number and voltage stable window reach 0.83 and 4.78 V respectively. This high-filled composite electrolyte possesses high tensile stress of 40 MPa with a strain of 46% and withstands working environment up to 200 °C. The NCM622/Li solid-state battery composed of this electrolyte also presents good rate and cycle performances with a capacity retention of 80% after 230 cycles at 0.3C because of its high ion transport capability and good inhibition of lithium dendrites. This composite structural design is expected to develop high-performance solid-state electrolytes suitable for high-voltage solid-state lithium batteries.     

Preparation and corrosion assessment of electrodeposited Ni–SiC composite thin films

Ni–SiC composite thin films were successfully prepared via direct-current (DC) and ultrasonic pulse-current (UPC) deposition. The morphologies, mechanical properties, and corrosion properties of the films were investigated via atomic force microscopy, X-ray diffraction (XRD), Vickers hardness test, scanning electron microscope (SEM), cyclic polarization, and gravimetric analysis. The results show that the Ni–SiC composite thin films synthesized via UPC deposition possess a compact and exiguous surface morphology. The XRD results indicate that the average grain diameters of Ni and SiC in the UPC-deposited thin film are 63.6 and 38.5 nm, respectively. The maximum microhardness values for the DC- and UPC-deposited Ni–SiC composite thin films prepared are 871.7 and 924.3 HV, respectively. In the corrosion tests, the UPC-deposited films have a higher corrosion resistance than those prepared by DC deposition with the same SiC content.     

Al2O3–cyanate ester hybrid thick films through aerosol deposition and resin infiltration

Al₂O₃–cyanate ester hybrid thick films had high Al₂O₃ contents over 75 vol.% were fabricated as 3D integrated substrates. The Al₂O₃–cyanate ester hybrid thick films were completed by resin infiltration of the cyanate ester into the porous Al₂O₃ thick films deposited by aerosol deposition (AD). Al₂O₃ particles were packed as high-density layers in the porous Al₂O₃ thick films by controlling the carrier gas flow rate using AD at room temperature. As dielectric substrate materials, the Al₂O₃–cyanate ester hybrid thick films had dielectric constant of 7.6 and quality (Q) factor of 390, and both were nearly independent of the measuring frequency.