Niobium‐Doped Titania Photocatalyst Film Prepared via a Nonaqueous Sol‐Gel Method

Niobium‐doped Titanium dioxide (Nb:TiO₂) transparent films were successfully deposited on glass substrates using a non‐aqueous sol‐gel spin coating technique. The effect of Nb concentration on the structural and photocatalytic properties of Nb:TiO₂ films was studied using X‐ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), and UV visible spectroscopy. The films with 12 at.% (atomic percent) Nb doped TiO₂ showed excellent photocatalytic activity through 97.3% degradation of methylene blue (MB) after 2 h of UV irradiation.     

The Effect of Electric Field on Sintering and Electrical Conductivity of Titania

The effect of DC electric field on sintering, and on the electrical conductivity of undoped rutile, TiO₂ (99.99%), has been investigated at fields ranging from 0 V to 1000 V/cm. The experiments were carried out at a constant heating rate of 10°C/min with the furnace temperatures reaching up to 1150°C. The sintering behavior falls into two regimes: at lower fields, up to 150 V/cm, sintering is enhanced, but densification occurs gradually with time (Type A or FAST sintering). At higher fields sintering occurs abruptly, and is accompanied by a highly nonlinear increase in conductivity, which has been called flash sintering (Type B or FLASH sintering). Arrhenius plots of conductivity yield an activation energy of 1.6 eV in Type A and 0.6 eV in Type B behavior; the first is explained as ionic and the second as electronic conductivity. The evolution of grain size under both types of sintering behavior are reported. These results highlight that the dominant mechanism of field‐assisted sintering can change with the field strength and temperature. We are in the very early stages of identifying these mechanisms and mapping them in the field, frequency, and temperature space.     

Electrical Properties of Porous Titania Ceramic Humidity Sensors

Ceramic humidity sensors made with pure TiO₂ powder as the starting material are investigated. The sensor can be reversibly operated without repeated high-temperature thermal desorption, and the conductance versus relative humidity (rh) sensitivity of the sensor is more than 4 orders of magnitude in the range ∼15% to 95% rh at 400 Hz and 25°C. The sensor can be polarized similar to electrolytes in the charging process, and the degree of polarization is enhanced with increasing rh. The conduction carriers of the sensor in the humid atmosphere are ions and electrons, and ions are the dominant conduction carrier. The relative dielectric dispersion k'(ω) is almost proportional to ω^−1.84 for rh ∼50% to 95% at low frequencies, where ω is the angular frequency. An inductive effect is also observed in a low-humidity atmosphere, which implies desorption of water vapor with the regeneration of the adsorption sites.     

Characterization and Tribological Investigation of Sol–Gel Titania and Doped Titania Thin Films

Titania (TiO₂) and doped TiO₂ ceramic thin films were prepared on a glass substrate by a sol–gel and dip-coating process from specially formulated sols, followed by annealing at 460°C. The morphologies of the original and worn surfaces of the films were analyzed with atomic force microscopy (AFM) and scanning electron microscopy. The chemical compositions of the obtained films were characterized by means of X-ray photoelectron spectroscopy (XPS). The tribological properties of TiO₂ and doped TiO₂ thin films sliding against Si₃N₄ ball were evaluated on a one-way reciprocating friction and wear tester. The AFM analysis shows that the morphologies of the resulting films are very different in nanoscale, which partly accounts for their tribological properties. XPS analysis reveals that the doped elements exist in different states, such as oxide and silicate, and diffusion took place between the film and the glass substrate. TiO₂ films show an excellent ability to reduce friction and resist wear. A friction coefficient as low as 0.18 and a wear life of 2280 sliding passes at 3 N were recorded. Unfortunately, all the doped TiO₂ films are inferior to the TiO₂ films in friction reduction and wear resistance, primarily because of their differences in structures and chemical compositions caused by the doped elements. The wear of the glass is characteristic of brittle fracture and severe abrasion. The wear of the TiO₂ thin film is characteristic of plastic deformation with slight abrasive and fatigue wear. The doped TiO₂ thin films show lower plasticity than the TiO₂ thin film, which leads to large cracks. The propagation of the cracks caused serious fracture and failure of the films.     

Preparation of Fluorine-Containing Indium Tin Oxide Sputtering Targets using Spark Plasma Sintering Process

Fluorine-containing indium tin oxide (F-ITO) sputtering targets were prepared using spark-plasma-sintering (SPS) process. The initial powder, which was prepared by reacting ITO with HF, was sintered to the 10 cm-disks with nearly 90% of the theoretical density by the SPS process. The resulting disks were consisted of ITO and InOF, and the fluorine content was about 4 at.%. Using the F-ITO disks as sputtering target, thin films were deposited on the glass substrates. The electrical conductivity and optical transmission of the deposited films were comparable to those of the conventional ITO films, while the surface roughness of the films was much improved.     

Effect of BBS‐Based Frit on the Low Temperature Sintering and Electrical Properties of KNN Lead‐Free Piezoceramics

Using BaO–B₂O₃–SiO₂ (BBS)‐based frit as sintering aid, the K_0.49Na_0.51NbO₃ (KNN) + x wt% BBS (x = 1.0, 1.5, 2.0 and 2.5) lead‐free piezoelectric ceramics were successfully fabricated by solid‐state reaction method under low‐sintering temperature of 1000°C. The effect of BBS frit doping amount on the structure and electrical properties of the ceramics was investigated. The KNN ceramics with 1.5 wt% BBS frit showed optimal properties as follows: piezoelectric constant d₃₃ = 108 pC/N, planar electromechanical coupling coefficient k_p = 41%, mechanical quality factor Q_m = 225, relative dielectric constant ε_r = 410, dielectric loss tanδ = 0.57% and Curie temperature T_c = 400°C. This ceramic sample should be a good lead‐free candidate for actuators or high temperature sensors application due to its ultra‐low tanδ, relatively high Q_m and T_c.     

Effects of Deposition Inclination Angle on Microstructure and Electrical Properties of Al‐Doped ZnO Coating Films

A flat plate in the deposition stage is designed to be tilted flexibly to form an inclination angle (θ) between an ion beam and the direction normal to a polyethylene terephthalate (PET) substrate. Five kinds of PET/aluminum‐doped zinc oxide specimens were prepared to examine the effects of inclination angle on the microstructures, crystals, chemical compositions, and electrical properties. An increase in the inclination angle results in X‐ray diffraction peak intensity variations in ZnO and a reduction in the composite d‐spacing. As the measure of the oxygen vacancies, the O₂‐peak intensity ratio (IR_O2) obtained using the X‐ray photoelectron spectrometry (XPS) is evaluated. The IR_O2 value increased with increasing the inclination angle, and it is proportional to the porosity integration over the visible light wavelengths. An increase in IR_O2 is favorable for the reduction in composite grain size (g_Composite). A smaller composite grain size (g_Composite) of ZnO particles and a larger energy gap (E_g) can be obtained from applications of nonzero inclination angle. An appropriate nonzero inclination angle increases hardness and reduced elastic modulus and decreases the carrier concentration and carrier mobility of the specimen significantly.     

CuO和B2O3复合掺杂对BaTi2O5陶瓷的降温烧结与电性能研究

采用非均相共沉淀法制备Ba Ti2O5粉体,以固相烧结法制备了Cu O和B2O3复合掺杂的Ba Ti2O5陶瓷,并对样品进行了XRD、SEM表征和电性能测试。结果表明:掺杂后制得的Ba Ti2O5陶瓷在1100℃烧结2 h的致密度达到96.71%,晶粒发育较完整,在室温下具有良好的铁电滞后特征,在测试频率1 KHz时,Ba Ti2O5陶瓷的介电常数为εr=71.96,说明在烧结过程中加入复合烧结助剂Cu O和B2O3可以促进液相形成并减少了气孔率,从而提高了陶瓷的致密度和介电性能。     

Thermoelectric Properties of Pb‐Doped BiCuSeO Ceramics

A high‐performance thermoelectric BiCuSeO oxyselenides has been prepared by a simple fabrication approach. Phase composition and microstructure analysis indicate that the obtained ceramic samples are almost BiCuSeO phase with plate structure. Our results show that Pb‐doped BiCuSeO bulks have good electrical conductivity, large Seebeck coefficient, and low thermal conductivity. A large power factor ~672 μ/Wm/K² at 573 K can be observed in the BiCuSeO ceramic by the 10% Pb doping, and the dimensionless figure of merit (ZT) can reach 0.95 at 873 K, which makes them promising candidates for thermoelectric applications.     

Optical and Microwave Dielectric Properties of Zn‐Doped MgAl2O4 Transparent Ceramics Fabricated by Spark Plasma Sintering

(Mg_1?xZn_x)Al₂O₄ transparent ceramics were fabricated by spark plasma sintering technique at 1325°C for 10 min. A small mount of Zn²⁺ addition to MgAl₂O₄ ceramics was very effective to the performance improvement, while further increase in Zn‐doped content would give rise to the optical transmittance deterioration. The optical and microwave dielectric properties of MgAl₂O₄ transparent ceramics were improved by Zn substitution for Mg. The in‐line transmittance of the (Mg_1?xZn_x)Al₂O₄ (x = 0.02) ceramics can be as high as 70% at λ = 550 nm and 86.5% at λ = 2000 nm, respectively. The dielectric constant ε_r of (Mg_1?xZn_x)Al₂O₄ just varied from 8.32 to 8.54, however, the Q × f value increased significantly up to a maximal value of 66,000 GHz at x = 0.02. Moreover, the τ_f of (Mg_1?xZn_x)Al₂O₄ transparent ceramics changed from ?74 to ?65.5 ppm/°C. With the increasing of Zn‐doped content, the average grain size and the porosity increased, which was the primary reason for the change in optical and microwave dielectric properties.     

Electromechanical Properties of Acceptor‐Doped Lead‐Free Piezoelectric Ceramics

We have studied the processing and electromechanical properties of Mn and Fe‐doped 0.88[Bi_0.5Na_0.5TiO₃]–0.08[Bi_0.5K_0.5TiO₃]–0.04[Bi_0.5Li_0.5TiO₃] piezoelectric ceramics prepared by the mixed oxide route. Different amounts of Mn (0.01, 0.014, 0.015, 0.016, 0.017, 0.02, 0.022) or Fe (0.0125, 0.015, 0.0175) were doped to this lead‐free piezoelectric composition. Ceramics were sintered at different temperatures (1075°C–1150°C) to achieve the highest density and mechanical quality factor. Mn or Fe doping resulted in a considerable enhancement of Q_m in both planar and thickness resonance modes. In 1.5 mol% Mn‐doped ceramics sintered at 1100°C, a planar Q_m of about 970 and tanδ of 0.88% were obtained. In Fe‐doped ceramics, a planar Q_m as high as 900 was achieved. Acceptor dopants also resulted in decreasing the coupling coefficients, the piezoelectric charge coefficient, and the dielectric constant.     

The Physical and Antimicrobial Properties of Silver Doped Hydroxyapatite Sintered by Microwave and Conventional Sintering

In this paper, the silver-doped hydroxyapatite (AgHAp) nanoparticles were successfully synthesized by conventional and microwave sintering. The structural and antibacterial properties of AgHAp without heat treatment (AgHAp-90) and after heat treated at 800 and 1000?°C by conventional (AgHAp-800CS, AgHAp-1000CS) and microwave sintering (AgHAp-800MS, AgHAp-1000MS) were discussed respectively. The results of X-ray diffraction and fourier transform infrared spectroscopy suggested that the pure phase of AgHAp nanoparticles were obtained at 800?°C, but the β-TCP phase was observed when the temperature up to 1000?°C. Scanning electron microscopy images showed that the morphology and size of the nanoparticles changed with the improvement of temperature. The energy dispersive X-ray analysis identified the existence of Ag, Ca, P. The antibacterial test of AgHAp showed the excellent antimicrobial activity against gram-negative strains Escherichia coli and gram-positive strains Staphylococcus aureus. Also, the results showed the AgHAp had a smaller effect on gram-positive strains compare with gram-negative strains, and the antimicrobial activity of particles sintered by microwave was better than samples sintered by conventional. It showed the great advantages of microwave sintering. The silver ion releasing in solution was measured by the inductively coupled plasma and elucidated the results of antibacterial tests.     

钐掺杂BaZrO3电解质的制备与电学性能研究

通过高温固相法合成了BaZr_(1-)_xSm_xO_(3-)_δ(x=0.05, 0.1, 0.15, 0.2)电解质材料,并对材料的物相结构进行了XRD表征。分别在空气和4%H_2O/H_2中,温度范围为500～800℃下,通过电化学工作站测试了该电解质材料的电学性能。研究发现,稀土元素Sm的掺杂对BaZrO_3电解质材料的电学性能有重大影响,当Sm元素的掺杂量为0.15时,电解质的电导率达到最大值。结果表明,Sm的掺杂可以有效提高BaZrO_3电解质材料的电导率。     

Understanding the Flash Sintering of Rare‐Earth‐Doped Ceria for Solid Oxide Fuel Cell

A novel electrical current applied technique known as flash sintering has been applied to rapidly (within 10 min) densify electrolytes including Ce_0.8Gd_0.2O_1.9 (GDC20), Ce_0.9Gd_0.1O_1.95 (GDC10), and Ce_0.8Sm_0.2O_1.9 (SDC20) for application in Solid Oxide Fuel Cells (SOFCs). The densification temperature for the three electrolytes was 554°C, 635°C, and 667°C, respectively, which is far below conventional sintering temperatures. All specimens after flash sintering maintained the pure fluorite structure and exhibited a well‐densified microstructure. To investigate the flash‐sintering mechanism, we have applied Joule heating effect with blackbody radiation theory, and found that this theory could reasonably interpret the flash‐sintering phenomenon by matching theoretically calculated temperature with the real temperature. More importantly, one of the materials inherent properties, the electronic conductivity, has been found correlated with the onset of flash sintering, which indicates that the electrons and holes are the primary current carriers during the start of flash‐sintering process. As a result, potential densification mechanisms have been discussed in terms of spark plasma discharge.     

Photoluminescence and Temperature Dependent Electrical Properties of Er‐Doped 0.94Bi0.5Na0.5TiO3‐0.06BaTiO3 Ceramics

Er‐doped 0.94Bi_0.5Na_0.5TiO₃‐0.06BaTiO₃ (BNT‐6BT: xEr, x is the molar ratio of Er³⁺ doping) lead‐free piezoceramics with x = 0–0.02 were prepared and their multifunctional properties have been comprehensively investigated. Our results show that Er‐doping has significant effects on morphology of grain, photoluminescence, dielectric, and ferroelectric properties of the ceramics. At room temperature, the green (550 nm) and red (670 nm) emissions are enhanced by Er‐doping, reaching the strongest emission intensity when x = 0.0075. The complex and composition‐dependent effects of electric poling on photoluminescence also have been measured. As for electrical properties, on the one hand, Er‐doping tends to flatten the dielectric constant‐temperature (ε_r‐T) curves, leading to temperature‐insensitive dielectric constant in a wide temperature range (50°C–300°C). On the other hand, Er‐doping significantly decreases the ferroelectric‐relaxor transition temperature (T_F–R) and depolarization temperature (T_d), with the T_F–R decreasing from 76°C to 42°C for x = 0–0.02. As a result, significant composition‐dependent electrical features were found in ferroelectric and piezoelectric properties at room temperature. In general, piezoelectric and ferroelectric properties tend to become weaker, as confirmed by the composition‐dependent piezoelectric coefficient (d₃₃), planar coupling factor (k_p), and the shape of polarization‐electric field (P–E), current‐electric field (J–E), bipolar/unipolar strain‐electric field (S–E) curves. Furthermore, to understand the relationship between the T_F–R/T_d and the electrical properties, the composition of x = 0.0075 has been intensively studied. Our results indicate that the BNT‐6BT: xEr with appropriate Er‐doping may be a promising multifunctional material with integrated photoluminescence and electrical properties for practical applications.     

Translucent Yttria‐ and Silica‐Doped Mullite Ceramics with Anisotropic Grains Produced by Spark Plasma Sintering

Translucent, high‐performance, mullite ceramics with anisotropic grains were prepared by the spark plasma sintering (SPS) of a powder mixture consisting of commercial mullite powder, which already contained small amounts of alumina (θ and α) and silica (cristobalite) (≤3 wt% in total), to which 2 and 1 wt% of yttria and amorphous silica was admixed, respectively. The combination of low‐viscosity Y₂O₃–Al₂O₃–SiO₂ transient liquid formation and SPS sintering provided enhanced densification, also provoking anisotropic grain growth (which became exaggerated after 20 min of SPS dwell time), at a relatively low sintering temperature of 1370°C. In this way, it was possible to meet the conflicting demands for obtaining a dense mullite ceramic with anisotropic grains, ensuring good mechanical properties, while preserving a noticeable light transmittance. In terms of mechanical and optical properties, the best results were obtained when SPS dwell times of 5 and 10 min were employed. The as‐sintered samples possessed densities in the range 3.16–3.18 g/cm³, anisotropic grains with an aspect ratio (AR) of 7 and a grain thickness of approximately 0.45 μm, a flexural strength between 350 and 420 MPa, a Vickers indentation toughness and a hardness of approximately 2.45 MPa·m^1/2 and 15 GPa, respectively, and an optical transmittance of between 30% and almost 50% in the IR range.     

Thermal Properties of Hf‐Doped ZrB2 Ceramics

The effect of Hf additions on the thermal properties of ZrB₂ ceramics was studied. Reactive hot pressing of ZrH₂, B, and HfB₂ powders was used to synthesize (Zr_1?x,Hf_x)B₂ ceramics with Hf contents ranging from x = 0.0001 (0.01 at.%) to 0.0033 (0.33 at.%). Room‐temperature heat capacity values decreased from 495 J·(kg·K)^?1 for a Hf content of 0.01 at.% to 423 J·(kg·K)^?1 for a Hf content of 0.28 at.%. Thermal conductivity values decreased from 141 to 100 W·(m·K)^?1 as Hf content increased from 0.01 to 0.33 at.%. This study revealed, for the first time, that small Hf contents decreased the thermal conductivity of ZrB₂ ceramics. Furthermore, the results indicated that reported thermal properties of ZrB₂ ceramics are affected by the presence of impurities and do not represent intrinsic behavior.     

Glass Additive Influence on the Sintering Behaviors,Magnetic and Electric Properties of Bi–Zn Co‐Doped Co2Y Ferrites

The Bi₂O₃–B₂O₃–ZnO–SiO₂ (BB35SZ) glass effects on the sintering behavior and magnetic properties of Bi–Zn co‐doped Co₂Y ferrites were investigated in developing low‐temperature‐fired ferrites. The results indicate that BB35SZ glass can be used as a sintering aid to reduce the densification temperature of Co₂Y ferrites from 1300°C to 900°C. The 2(Ba_0.9Bi_0.1O)·2(Zn_0.4Co_0.4Cu_0.2O)·6(Fe_1.97Zn_0.03O₃) ferrite with 4 wt% BB35SZ glass can be densified below 900°C, exhibiting an initial permeability of 3.4 and quality factor of 55. This process provides a promising candidate for multilayer chip magnetic devices for microwave applications.     

Electrical Properties of Gallium-Doped Zinc Oxide Films Prepared by RF Sputtering

Ga-doped polycrystalline ZnO films on glass substrates were prepared by sputtering the targets, which had been prepared by sintering disks consisting of ZnO powder and various amounts of Ga₂O₃, to investigate the effects of gallium doping and sputtering conditions on electrical properties. Optimizing the RF power density, argon gas pressure, and gallium content, transparent Ga-doped ZnO films with resistivity less than 10⁻³Ω·cm were obtained. Electron concentrations for undoped and Ga-doped ZnO films were on the order of 10¹⁸ and 10²¹/cm³, respectively. The Ga-doped ZnO films became degenerate when the electron concentration exceeded ∼ 10¹⁹/cm³, and the optical band gap increased with increasing carrier concentration because of the increase of Fermi energy in the conduction band.     

Insulating and Other Physical Properties of CoO‐Doped Zinc Oxyfluoride‐Borate Glass‐Ceramics

Zinc oxy fluoro borate glasses mixed with different concentrations of CoO (ranging from 0 to 2.0 mol%) are synthesized and subsequently crystallized. The scanning electron microscopy pictures have exhibited crystallinity. Differential scanning calorimetric studies have indicated that the prepared samples consist of multiple crystal phases. The X‐ray diffraction patterns have indicated that the glass‐ceramic samples are composed of αZn(BO₂)_2, (Zn)₃(BO₃)_2, CoF₂, CoF₃, Co₃FB₇O₁₃, ZnCo₂O₄, Co₃O₄ crystalline phases. The optical absorption and photoluminescence studies have indicated that there is a gradual increase of tetrahedral cobalt ion concentration with increase of CoO concentration in the glass network. IR spectroscopic studies have pointed out increased degree of polymerization of the zinc oxy fluoro borate glass network with increase of CoO content. The analysis of results of dielectric properties indicated increase of insulating strength of the glass‐ceramics with increase of CoO content. Finally, the dielectric breakdown strength of the samples is measured at room temperature in air medium and it is found to increase from 12.9 to 19.2 kV/cm with increase of CoO from 0.2 to 2.0 mol%. The reasons for such increase of breakdown strength are discussed quantitatively in terms of dielectric parameters with aid of data on spectroscopic properties.