Microhardness of ceramics produced from different alumina nanopowders by different techniques

Fine-grained ceramics (with a grain size on the order of a micron) have been produced by the spark plasma sintering (SPS) of various alumina nanopowders. We have compared the microhardness of ceramic samples prepared from 11 alumina nanopowders and that of composites based on such powders. The ceramics have been prepared by both SPS and a conventional technique (sequential pressing and sintering). We examine the effect of the phase composition and average particle size of the starting nanopowder on the microhardness of the ceramics.     

Synthesis and consolidation of iron nanopowders

A microwave plasma processing technique was used to synthesize iron nanopowders. The average particle size of these powders was ~10 nm and the surface area was measured to be 42m²/g. Powder production rates as high as 50 gm/hour were achieved. Magnetic property measurements on iron nanopowders yielded coercivities as high as 60 kA/m at 4 K, which decreased to ~0 A/m (a superparamagnetic transition) at room temperature. In this paper, the microwave plasma processing technique has been compared with other nanopowder synthesis techniques. Since the successful application of nanomaterials depends highly on the processing technology, results from consolidation studies on iron nanopowders are also presented. Iron nanopowders were consolidated to study performance parameters such as density, grain growth and other morphological changes. The nanopowder was consolidated using Plasma Pressure Consolidation (P²C) technique to 95% density, at a temperature and pressure of 850 °C and 63 MPa respectively. Microwave plasma synthesis is capable of producing metallic and ceramic nanopowders, which will sustain interest in research areas including magnetic storage, nano-fabrication of electronic materials and nanoglass, besides the field of catalysis.     

Tough yttria-stabilized zirconia ceramic by low-temperature spark plasma sintering of long-term stored nanopowders

Weakly agglomerated 1.75 and 3 mol% yttria stabilized zirconia nanopowders were used in this study after six years of storage in vacuum-processed plastic containers. The proper storage conditions of the Y-TZP nanopowders avoided the hard agglomeration. Untreated and bead-milled nanopowders were used to obtain dense ceramics by slip casting and subsequent low-temperature sintering. Fully dense nanostructured 1.75Y-TZP and 3Y-YZP ceramics with and without doping of 1 wt% Al2O3 were produced by an optimized spark plasma sintering (SPS) technique at the temperatures of 1050-1150 degrees C at a pressure of 100 MPa. The SPS has revealed the clear advantage of consolidation of the weakly agglomerated nanopowders without preliminary deagglomeration. The Vickers hardness of both the low-temperature and spark plasma sintered samples was found to lie in the range of 10.98-13.71 GPa. A maximum fracture toughness of 15.7 MPa m(1/2) (average 14.23 MPa m(1/2)) was achieved by SPS of the 1.75Y-TZP ceramic doped with 1 wt% Al2O3 whereas the toughness of the 3Y-TZP ceramics with and without alumina doping was found to vary between 3.55 and 5.5 MPa m(1/2).     

Red clay-based porous ceramic with pores created by yeast-based foaming technique

Red clay-based porous ceramic has been fabricated by using a biological foaming technique through reaction of yeast with starch in aqueous ceramic suspension. The starch plays a dual role as a growth substrate for gas bubble generation and a binder for ceramic particles. Starch-loaded ceramic slurries (55 wt% ceramic solid) were prepared, consisting of red clay, quartz, feldspar, and starch. Three types of starches were used, namely, cassava starch, corn starch, and rice flour. The rheological characterization of starch-loaded ceramic slurries showed shear thinning behavior. This resulted into a high foaming factor depending on the types of starches loaded and increased addition of yeast. Total fired porosities obtained were between 17 and 70%. These correspond to open porosities between 15% and 50%, and close porosities range from 6% to 35%. Microstructural investigation of the fired porous compacts showed irregular pore morphologies equipped with interconnecting channels that represent the open porosity.     

Synthesis of ZnO nanopowders by DC thermal plasma for dye-sensitized solar cells

Zinc oxide (ZnO) nanopowders were synthesized from commercially available micro-sized zinc powders (Aldrich Co., 98%, 10 μm) by a DC thermal plasma process at atmospheric pressure. The micro-sized zinc powders were vaporized in the plasma region, after which the plasma processing equipment was rapidly quenched, resulting in the formation of ZnO nanopowders with a size of less than 300 nm. Two different reaction gases of oxygen and carbon dioxide were used as the oxygen source and each gas flow rate was controlled as a process variable. The obtained ZnO nanopowders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). All synthesized ZnO nanopowders showed high crystalline wurtzite structures and the differences in their morphologies were strongly dependent on the operating variables. The photocurrent–voltage (J–V) curve of the ZnO nanopowders with a dye of ruthenium (II) 535 bis-TBA (N719, Solaronix) in redox electrolyte showed an overall energy conversion efficiency (η) of 2.54%, demonstrating that the application of the mass-producible ZnO nanopowders by thermal plasma processing to DSSC was feasible.     

Preparation of CuO nanopowders and their catalytic activity in photodegradation of Rhodamine-B

CuO nanopowders have been successfully synthesized in two different morphologies from same precursor using a facile gel to crystalline (reflux) and co-precipitation synthesis routes. SEM and TEM observations indicate that the morphology of the products depends on preparation technology, while XRD shows the formation of CuO nanocrystals with monoclinic crystal system in both cases. A comparison of morphological characterization of CuO nanopowders showed flower-like and aggregated nanoparticles in the form of clusters using reflux and co-precipitation techniques, respectively. Photocatalytic activity of the products in the aqueous solution of Rhodamine-B has been investigated under UV-light for a given time using UV–visible spectroscopy and the mineralization of organic substance was measured by total organic carbon (TOC) analysis. It was observed that the photocatalytic activity in the presence of flower-like CuO nanopowders was higher than that of observed with aggregated nanoparticles. Also the mechanisms for the formation of CuO nanopowders and the obtained results of photocatalytic degradation of Rhodamine-B are discussed.     

Discrepancy of room temperature ferromagnetism in Mo-doped In 2 O 3

Molybdenum-doped indium oxide nanopowders were synthesized via mechanical alloying with subsequent annealing at a relatively low temperature of 600  $^{\circ}$ C. The morphologies and crystal structures of the synthesized nanopowders were examined by using scanning electron microscopy (SEM) and X-ray diffraction patterns. X-ray diffraction pattern of the milled mixture shows the presence of both In₂O₃ phase and Mo element. The presence of broad peaks in the pattern confirms that the synthesized powders are nanosized. The X-ray diffraction of annealed samples at 600  $^{\circ}$ C shows the absence of Mo peaks revealing that the Mo was incorporated into the crystal lattices of In₂O₃. Interestingly, it was observed that the diffraction peaks were still broad in the annealed samples indicating the single phase at the nanoscale. From the XRD pattern, the calculated crystallite sizes were in the range of 12–18 nm. Magnetic properties of the synthesized Mo-doped In₂O₃ nanopowders were examined and it was found that the obtained nanopowders possess diamagnetic properties.     

Multiple nano-blast synthesis of PT/8Y-ZP composite nanopowders

We demonstrate a processing technique based on the synthesis of ceramic nanopowders and simultaneous impregnation with metallic nanoparticles by multiple 'nano-blasts' of embeded cyclotrimethylene trinitramine in preliminary engineered multi-component nano-reactors. 'Nano-blasts' of impregnated cyclotrimethylene trinitramine deagglomerate the nanopowder due to the high energetic impacts of the blast waves, while the decomposition of compounds and their solid-solubility is enhanced by the extremely high local temperature generated during the nano-explosions. We applied this technique to produce nanosized agglomerate-free 8 mol% yttria-doped cubic zirconia aggregates with an average size of 53 nm impregnated with 10 mass% of platinum particles of 2-14 nm.     

Ferromagnetic Resonance Investigation of Hexaferrite Nanoparticles Prepared by Sol-Gel Auto-Combustion Method

In this study, the magnetic and electromagnetic wave-absorbing properties of barium and strontium ferrite nanopowders prepared by a sol-gel technique were investigated. To study the structural characteristics of hexaferrites, X-ray diffraction analysis was used. Investigation of the morphologies of nanoparticles was carried out by field emission scanning electron microscopy. A vibrating sample magnetometer was used in order to examine the magnetic properties of synthesized hexaferrites at room temperature. Ferromagnetic resonance (FMR) was used to investigate ferromagnetic resonance of the powders. Experimental results indicated that the materials had hexagonal structures with desirable magnetic properties. A low-field absorption signal was observed with the same phase as the FMR absorption in barium hexaferrites.     

Nanocrystalline hydroxyapatite ceramics

The possibility of using high pressures in uniaxial pressing and rolling of nanopowders is investigated. Obtainment of a nanocrystalline hydroxyapatite ceramic intended for use in medicine is studied. The sintering temperature is reduced by approximately 600°C, and a ceramic with a grain size of less than 50 nm and high values of microhardness (up to 5.7 GPa) after annealing at 750°C is obtained. A substantial collective recrystallization of crystallite powder is overcome.     

Thermoplastic polymer nanocomposites for applications in optical devices

Polymer optical fibres (POF) have superior properties compared to glass fibres like e.g. high flexural strength, uncomplicated mechanical machining and inexpensive mass production. Dispersion of nanoscaled ceramic fillers in polymers allows the modification of the refractive index depending on the ceramic used and the aspired application. Current work deals with the development of a process chain to tailor the refractive index of PMMA using a UV-curable reactive resin and ceramic nanopowders as well as with the ageing behaviour of polymer nanocomposites. Improved dispersion techniques applying high shear forces to deagglomerate the ceramic powders lead to a refractive index shift depending on the ceramic fillers maintaining a transparency of resulting polymer nanocomposites sufficient for optical applications in the visible (633 nm) and in the infrared (1550 nm) regime. Optical devices were obtained using reaction moulding of the modified polymer nanocomposites as rapid prototyping method.     

Robocasting of dense yttria-stabilized zirconia structures

Advanced ceramic materials with complex design have become inseparable from the current engineering applications. Due to the limitation of traditional ceramic processing, ceramic additive manufacturing (AM) which allows high degree of fabrication freedom has gained significant research interest. Among these AM techniques, low-cost robocasting technique is often considered to fabricate complex ceramic components. In this work, aqueous ceramic suspension comprising of commercial nano-sized yttria-stabilized zirconia (YSZ) powder has been developed for robocasting purpose. Both fully and partially stabilized YSZ green bodies with complex morphologies were successfully printed in ambient conditions using relatively low-solid-content ceramic suspensions (<38 vol%). The sintered structures were able to retain the original morphologies with >94% of the theoretical density despite its high linear shrinkage (up to 33%). The microstructure analysis indicated that dense fully and partially stabilized YSZ with grain size as small as 1.40 ± 0.53 and 0.38 ± 0.10 μm can be obtained, respectively. The sintered partially stabilized YSZ solid and porous mesh samples (porosity of macro-pores >45%) exhibited hardness up to 13.29 GPa and flexural strengths up to 242.8 ± 11.4 and 57.3 ± 5.2 MPa, respectively. The aqueous-based ceramic suspension was also demonstrated to be suitable for the fabrication of large YSZ parts with good repeatability.     

Planar multilayer membranes on metallic supports

We have tested a number of approaches to producing oxygen-selective planar multilayer membranes with mixed conductivity of functional layers on metallic gauze as a key component of a porous support. The results demonstrate that the shrinkage mismatch can be considerably reduced via pressure sintering. The conditions for firing metallic gauzes and applying ceramic coatings have been established. We describe the optimal structure and processes for applying ceramic layers with the aim of producing planar multilayer membranes of catalytic membrane reactors for methane conversion. Mechanochemical ceramic processing was successfully used to produce ceramic nanopowders and modifying paste.     

Densification Peculiarities of Transparent MgAl<Subscript>2</Subscript>O<Subscript>4</Subscript> Ceramics—Effect of LiF Sintering Additive

A new method of doping of spinel nanopowders with LiF sintering additive has been proposed, consisting in its introduction via solution technology, which leads to improved sinterability of the ceramic. The effect of LiF doping on densification behavior, microstructure, and optical and mechanical properties of hot-pressed MgAl₂O₄ ceramics has been studied. Samples of MgAl₂O₄ optical ceramics with density close to that theoretically achievable have been produced by hot pressing of 0.5 wt % LiF-doped nanopowders at 1600°C for 1 h. It has been shown that addition of LiF changes crack propagation in spinel ceramic from transgranular to intergranular.     

Structure and properties of silver-doped calcium phosphate nanopowders

Stable and antimicrobial silver-doped calcium phosphate nanopowders were synthesized using sol–gel route by setting the atomic ratio of Ag/(Ag+Ca) at 3% and (Ca+ Ag)/P at 1.67. Prior to synthesis of nanopowders, influence of time of hydrolyzation on pH and density of precursors were comprehensively studied. Hydrolyzation time was found to have profound influence on pH of constituent precursors. Sufficient hydrolysis resulted in early maturation of sol. Scanning electron microscopy (SEM) showed the heterogeneous and agglomerated state of particles with average size of 3.9± 1.9 μm. Energy dispersive X-ray spectroscopy (EDX) presented uniform distribution of O, Ag, Ca and P elements in nanopowder. Fourier transform infrared spectroscopy (FTIR) confirmed the formation of apatitic structure, whereas X-ray diffraction (XRD) revealed the multiphase constitution of nanopowders primarily composed of β-TCP, Ag and other hybrid phases. Crystallite size and lattice parameters of β-TCP and Ag phases were increased with the rise in calcination temperature. Thermogravimetric analysis (TGA) showed three regions of weight change and indicated the high thermal stability of nanopowders. Disk diffusion method was used to test the antimicrobial resistance of nanopowders against Escherichia coli and Staphylococcus aureus bacterial strains. All nanopowders exhibited antimicrobial resistance against both E. coli and S. aureus bacteria.     

Microwave sintering of ZnO nanopowders and characterization for gas sensing

Thick ?lm gas sensors based on ZnO nanopowders were fabricated by using microwave sintering. The surface and cross section morphologies were characterized by ?eld-emission scanning electron microscopy (FE-SEM). The stability of the microstructure was studied by impedance spectroscopy. The results showed that the shape of the nanoparticles was not changed through microwave sintering, and the thick films had the more dense microstructures than that by muffle oven sintering. The resistance-temperature characteristic and the responses to toluene, methanol and formaldehyde revealed that the microwave sintering technique could effectively control the growth of ZnO nanoparticles, realize the uniform sintering of thick film, gain the stable microstructure and improve the response of sensor. In addition, the formative mechanism of the thick film microstructure was proposed according to microwave sintering mechanism.     

焙烧温度对滑动弧等离子体制备纳米TiO2光催化剂的影响

采用滑动弧等离子体制备出不同颗粒形貌和锐钛矿相初始含量(f_A)的纳米TiO₂粉体。采用X射线衍射(XRD)、透射电镜(TEM)和物理吸附仪对焙烧前后的样品进行表征, 考察了焙烧温度对纳米TiO₂的晶相组成、晶体粒径、比表面积(S_BET)和颗粒形貌的影响。通过光催化氧化亚甲基蓝反应评价样品焙烧后的光催化活性。结果表明, 滑动弧等离子体制备的纳米TiO₂的锐钛矿相向金红石相转变温度约为650℃, 锐钛矿相向金红石相的转变速率取决于焙烧温度、颗粒形貌和锐钛矿相初始含量。随焙烧温度升高, 球形颗粒的锐钛矿晶体粒径略微增大, S_BET缓慢减小; 非球形颗粒的锐钛矿晶体粒径快速增大, S_BET迅速减小。随着f_A的增加, 纳米TiO₂粉体的光催化表观反应速率常数(k)呈现三种不同的变化趋势: 当f_A<70%时, k随之缓慢增加; 当70%<f_A<85%时, k随之快速增加; 当f_A>85%时, k转为快速降低。     

Effect of polyvinyl alcohol additive on the pore structure and morphology of the freeze-cast hydroxyapatite ceramics

Porous hydroxyapatite (HAP) ceramics with different morphologies were fabricated by the freeze casting method. The morphologies of HAP ceramics were modified by adjusting the concentration of polyvinyl alcohol (PVA) additive in the HAP slurries. HAP ceramics without PVA additive were composed of non-interconnected macroscopic lamellar pores and porous ceramic walls. With PVA additive, the HAP ceramics were made up of small lamellar pores or three-dimensional reticulate pores and porous ceramic walls. PVA additive had no effect on the phase composition of HAP ceramics. The open porosity and pore connectivity were improved because of the addition of PVA.     

Characterization of ZrO2 and SiC ceramic thin films prepared by electrostatic atomization

ZrO₂ and SiC ceramic thin films and their bilayer have been successfully prepared by a newly developed electrostatic atomization technique. This technique can generate fine spray of ceramic suspensions in a micrometer sized range with a narrow size distribution which is crucial for preparation of uniform thin films of these ceramic materials. Compared to some other thin film deposition techniques, such as Chemical vapour deposition (CVD), physical vapour deposition (PVD) and plasma spray (PS) etc. the thin film deposition process using electrostatic atomization is not only cheap but also controllable. The prepared ZrO₂ and SiC thin films were investigated using scanning electron microscopy (SEM) and energy dispersion analysis (EDA) techniques. These thin films were observed to be homogenous with a particle size less than 10 m. The ZrO₂-SiC bilayer was found to have an abrupt interface, implying that the deposition process is controllable and also that functionally graded ceramic/ceramic materials can be prepared in this way if the thickness of each layer is accurately controlled.     

TA2纯钛微弧氧化陶瓷膜层的颜色和性能

在添加乙酸铜、乙酸镁的磷酸-氟锆酸钾电解液中对纯钛TA2基体进行微弧氧化处理,制备出颜色均匀的浅棕色陶瓷膜层。通过X射线衍射分析(XRD)、扫描电子显微分析(SEM)及附带的能谱(EDS),研究了陶瓷膜的表面和截面形貌、元素分布、相组成;用分光光度计测量了膜层的颜色,根据热震试验和三点弯曲法评价了膜层与基体的结合强度。结果表明:随着微弧氧化时间的延长,膜层中铜镁元素的含量增加,膜层的颜色随之发生变化,膜层与基体的结合强度降低。热震实验结果表明,膜层与基体有较高的结合强度。