Friction and wear of epoxy/TiO2 nanocomposites: Influence of additional short carbon fibers, Aramid and PTFE particles

An epoxy-based nanocomposite containing graphite powder (7 vol%) and nano-scale TiO₂ (4 vol%) was developed for tribological evaluation. A series of composites containing additional fillers such as short carbon fibers (SCF), Aramid and polytetrafluoroethylene (PTFE) particles was developed and evaluated in adhesive and low amplitude oscillating wear modes. The incorporation of SCF and Aramid particles resulted in a remarkable improvement in the sliding wear resistance. However, SCF impaired the low amplitude oscillating wear resistance. The further addition of PTFE to the SCF filled nanocomposites reduced the friction and wear under both wear conditions. However, an adverse effect of PTFE was found for the Aramid particles filled nanocomposites. Under sliding conditions, the lowest wear rate and coefficient of friction showed the 2–4 vol% PTFE filled SCF nanocomposite. Aramid particles containing nanocomposites (without PTFE) exhibited the best wear and friction behavior under low amplitude oscillating wear conditions among the selected composites. The wear mechanisms were studied by scanning electron microscopy.     

Photoluminescence properties of the Yb:Er co-doped Al2O3 thin film fabricated by microwave ECR plasma source enhanced RF magnetron sputtering

The Yb:Er co-doped Al₂O₃ thin film was deposited on oxidized silicon wafers by microwave ECR plasma source enhanced RF magnetron sputtering, and annealed from 800 °C to 1000 °C. The photoluminescence at 1.53 μm of thin film was obtained under room temperature. The mixture phase structure of γ and θ is observed by XRD, and the compositions of the thin film are investigated by EPMA. The maximum PL intensity was achieved with O₂:Ar at 1:1, annealing temperature at 900 °C, and experimental ratio of Yb:Er at 1:3.6. The energy transfer mechanism between Er and Yb ions is supported by theoretical analysis and experiment results.     

Formation, characterization and magnetic properties of carbon-encapsulated iron carbide nanoparticles

Fe₃C nanoparticles encapsulated in carbon shell with a size range of 20–50 nm were obtained in large scale by reacting anhydrous FeCl₃, hexamethylenetetramine and metal Na in an autoclave at 650 °C. Magnetization measurements show that the as-obtained materials display superparamagnetic properties at room temperature. A possible formation mechanism of the core–shell nano-structures was discussed.     

Preparation and optical properties of sol–gel derived Er-doped Al2O3–Ta2O5 films

Thin films of the system xAl₂O₃–(100 − x)Ta₂O₅–1Er₂O₃ were prepared by a sol–gel method and a dip-coating technique. The influences of the composition and the crystallization of the films on Er³⁺ optical properties were investigated. Results of X-ray diffraction indicated that the crystallization temperature of Ta₂O₅ increased from 800 to 1000 °C with increased values of x. In crystallized films, the intensities of the visible fluorescence and upconversion fluorescence tend to decrease with an increase in x values, due to the high phonon energy of Al₂O₃; the strongest fluorescence is observed in a crystallized film for x = 4 heat treated at 1000 °C. In amorphous films obtained by heat treatment at relatively low temperatures the Er³⁺ fluorescence could not be observed because strong fluorescence from organic residues remaining in the films thoroughly covered the Er³⁺ fluorescence. On the other hand, the Er³⁺ upconversion fluorescence in the amorphous films was observed to be stronger than that in the crystallized films. The strongest upconversion fluorescence is observed in an amorphous film for x = 75 heat treated at 800 °C.     

Kinetics of gas phase reduction of nickel chloride in preparation for nickel nanoparticles

We investigated the chemical kinetics of NiCl₂ reduction to apply to the synthesis of nickel nanoparticles in a tubular furnace reactor. The conversion of NiCl₂ increased monotonically with reaction temperature up to 99% at 950 °C, and in turn, the rate constant of the reaction increased from 78 to 286 with an increase in the temperature from 800 to 950 °C. The reaction rate was estimated to be the first order with respect to chloride concentration, and the rate constant obeyed the Arrhenius law, of which the activation energy and pre-exponential factor were 103.79 kJ/mol and 7.34 × 10⁶ min⁻¹, respectively. Taking advantage of the kinetics, we synthesized crystalline nickel nanoparticles with average primary particle size ranging from 31 to 106 nm by systematically controlling the reactor temperature and chloride concentration.     

Effect of β-spodumene on the phase development in an alumina/aluminium-titanate system

The effect of β-spodumene additions on the in situ phase formation and abundances in an Al₂O₃–Al₂TiO₅ system in the temperature range 1000–1400 °C has been studied by neutron diffraction and differential thermal analysis. Results show that β-spodumene began to decompose by phase separation and partial melting at 1290 °C, followed by complete melting at 1330 °C. Formation of Al₂TiO₅ was observed to occur at 1310 °C and its abundance increased with temperature. The addition of β-spodumene as a sintering aid did not cause its reaction with alumina or rutile to form additional phases. Addition of β-spodumene in excess of 5 wt% resulted in pronounced vitrification, which partly recrystallised when cooled to room temperature. The temperatures of Al₂TiO₅ formation and melting of β-spodumene are consistent with the results of differential thermal analysis.     

Tribological and mechanical properties of the composites made of carbon fabrics modified with various methods

Carbon fabric (CF) was modified with strong HNO₃ etching, plasma bombardment, and anodic oxidation, respectively. The modified carbon fabric was then used to prepare carbon fabric composites (CFC) by dip-coating in a phenolic resin and the relative mass content of carbon fabric in the carbon fabric composites is 65%. The friction and wear behaviors of the carbon fabric composites were evaluated with a Xuanwu-III high temperature friction and wear tester, and their mechanical properties were evaluated on a Shimadzu™ universal materials testing machine, respectively. The changes in the chemical compositions of the unmodified and modified carbon fabrics were analyzed by means of X-ray photoelectron spectroscopy. The morphologies of the worn surfaces of the unmodified and modified carbon fabric composites were analyzed by means of scanning electron microscopy. It was found that the friction-reduction and anti-wear properties of the carbon fabric composites were improved by anodic oxidation, plasma bombardment, and strong HNO₃ etching, so were the mechanical properties and load-carrying capacity. The composite made of the carbon fabric modified with anodic oxidation showed the best tribological and mechanical properties, and the one made of the carbon fabric etched with HNO₃ had the poorest tribological and mechanical properties among the three kinds of the tested composites. The active groups were produced during the oxidation process, which contributed to strengthen the bonding strength between the carbon fabric and the adhesive and hence to improve the tribological and mechanical properties of the composites made of the modified carbon fabric. The friction and wear properties of the carbon fabric composites were closely dependent on the environmental temperature. Namely, the wear rates of the composites at elevated temperature above 180 °C were much larger than that below 180 °C, which was attributed to the degradation and decomposition of the adhesive resin at excessively elevated temperature. Moreover, the composite made of the carbon fabric modified with anodic oxidation had better thermal stability than the one made of the unmodified carbon fabrics.     

Sol–gel thin film deposition and characterization of a new optically active compound: Er2Ti2O7

This paper reports on the first sol–gel thin film preparation of a new optically active compound: Er₂Ti₂O₇ (ETO). Optical, microstructural and spectroscopic properties of ETO films annealed in a temperature range 300–1000°C are studied. This work shows that the porosity and microstructure of ETO films depend closely on the heat-treatment temperature. Photoluminescence (PL) has been observed for films heat-treated at 600°C or more. The PL decay appears strongly influenced by quenching effects. For thin films treated at 600°C, quenching is essentially due to the presence of hydroxyl groups. After heat-treatment at 800°C or more, quenching can be explained by the high concentration of erbium atoms and by their distribution in the ETO lattice.     

Enhancement of the wear resistance of epoxy: short carbon fibre, graphite, PTFE and nano-TiO2

Enhancements of the wear resistance of epoxy using various fillers, e.g. short carbon fibre (CF), graphite, polytetrafluoroethylene (PTFE) and nano-TiO₂, have been systematically investigated in the present study. Wear properties were carried out on a block-on-ring apparatus. The best wear resistant composition was achieved by a combination of nano-TiO₂ with conventional fillers; as an example, epoxy+15 vol% graphite+5 vol% nano-TiO₂+15 vol% short-CF exhibits a specific wear rate of 3.2×10⁻⁷ mm³/Nm, which is about 100 times lower when compared to the neat epoxy. Worn surfaces were investigated using a scanning electron microscope and an atomic force microscope, from which it is assumed that a mechanism of nanoscale rolling governs this positive effect of the nanoparticles. The main concept of this paper is to strength the importance of integrating various functional fillers in the design of wear resistant polymer composites.     

Preparation of cobalt oxide nanoparticles and cobalt powders by solvothermal process and their characterization

Co₃O₄ nanoparticles and cobalt (fcc-Co) powders were successfully synthesized by solvothermal process from a single precursor. The reaction of Co(Ac)₂ with sodium dodecylbenzenesulfonate (SDBS) shows evident-dependent temperature effect. At 180 °C, Co(Ac)₂ reacts with SDBS to produce precursor CoCO₃ plate structures, which are assembled by small nanoparticles. At the temperature of 250 °C, the precursor CoCO₃ can be gradually decomposed to form Co₃O₄ nanoparticles with diameter of ca. 70 nm. While, at 250 °C, the reaction of Co(Ac)₂ with SDBS also produce precursor CoCO₃ nanoparticles/plates, but the CoCO₃ nanoparticles/plates would only decompose to give metal Co. In this process, SDBS acts as not only a surfactant but also a reagent. Magnetic measurements reveal that the as-prepared Co₃O₄ nanoparticles exhibit weak ferromagnetic properties and Co powders show ferromagnetic properties. In addition, a possible formation mechanism was elaborately discussed.     

Effect of annealing on the structural and optical properties of non-coated and silica-coated ZnS:Mn nanoparticles

The Mn²⁺-doped ZnS nanoparticles stabilized by sodium citrate were synthesized through a simple chemical route. Using the ZnS:Mn nanoparticles as seeds, the silica-coated ZnS:Mn nanocomposites were formed in isopropanol by the controlled hydrolysis of tetraethyl orthosilicate. The photoluminescence spectra confirmed that the Mn²⁺ ions were incorporated into the ZnS nanoparticles. The annealing effect on the structural and optical properties of these particles was studied over a range of 100–400 °C. The results of X-ray diffraction and photoluminescence showed that the silica shell not only improved the thermal stability but also resisted the lattice-deformation and oxidation of the particles. The thermal analysis further confirmed that the non-coated ZnS:Mn nanoparticles were unstable beyond 200 °C.     

Icosahedral Al62Cu25.5Fe12.5 phase in the presence of carbon

Previous studies have suggested that contamination by carbon of the i-Al₆₂Cu_25.5Fe_12.5 quasicrystalline phase can cause destabilization of the aperiodic structure. Hence, the possibility of carbon diffusion into AlCuFe quasicrystalline thin films and the possible subsequent degradation of the quasicrystalline structure were investigated at room temperature through to 600 °C. The study shows that a carbon layer deposited on the AlCuFe quasicrystalline thin film did not diffuse into the AlCuFe over the temperature range tested whatever the oxide thickness between carbon and alloy. Moreover, the carbon did not react with any of the alloy elements as has been shown with aluminium in the presence of oxygen. Post-deposition annealing at 600 °C of the amorphous alloy, fabricated by simultaneous electron beam evaporation on an amorphous carbon substrate used for transmission electron microscopy (TEM), also leads to a pure quasicrystalline phase thin film without any carbon diffusion from the substrate.     

Ablation behavior of ZrB2–SiC ultra high temperature ceramics under simulated atmospheric re-entry conditions

ZrB₂–20vol%SiC ultra high temperature ceramic (UHTC) was prepared by hot-pressing. Ablation tests of the flat-face models were conducted under ground simulated atmospheric re-entry conditions using arc-jet testing with heat fluxes of 1.7 MW/m² and 5.4 MW/m² under subsonic conditions, respectively. There was little weight or configuration change after ablation at a heat flux of 1.7 MW/m². However, ZrB₂–SiC composite underwent severe ablation and whose surface temperatures exceeded 2300 °C at a heat flux of 5.4 MW/m². Sharp-shape leading edge models were ablated under supersonic conditions with the stagnation pressure and Mach number of 1.2 atm and 2.7 M, respectively, and sharp-shaped leading edge C/SiC models were also ablated under the same condition for comparison. ZrB₂–SiC composite exhibited an excellent thermal-oxidative and configurational stability in the simulated re-entry environment compared with C/SiC material. Results indicate that ZrB₂–SiC ultra high temperature ceramics are the potential candidates for leading edges. The temperature limit for UHTC is controlled by the softening and degradation of the formed oxide scale.     

Electrochromic properties of nanocrystalline MoO3 thin films

Electrochromic MoO₃ thin films were prepared by a sol–gel spin-coating technique. The spin-coated films were initially amorphous; they were calcined, producing nanocrystalline MoO₃ thin films. The effects of annealing temperatures ranging from 100 °C to 500 °C were investigated. The electrochemical and electrochromic properties of the films were measured by cyclic voltammetry and by in-situ optical transmittance techniques in 1 M LiClO₄/propylene carbonate electrolyte. Experimental results showed that the transmittance of MoO₃ thin films heat-treated at 350 °C varied from 80% to 35% at λ = 550 nm (ΔT =  45%) and from 86% to 21% at λ ≥ 700 nm (ΔT =  65%) after coloration. Films heat-treated at 350 °C exhibited the best electrochromic properties in the present study.     

Carbon-enriched coal fly ash as a precursor of activated carbons for SO2 removal

Carbon-enriched coal fly ash was evaluated in this work as a low-cost adsorbent for SO₂ removal from stack gases. The unburned carbon in coal fly ash was concentrated by mechanical sieving and vegetal oil agglomeration. The carbon concentrates were activated with steam at 900 °C in order to develop porosity onto the samples. The performance of these samples in the SO₂ abatement was tested in the following conditions: 100 °C, 1000 ppmv SO₂, 5% O₂, 6% water vapor. A good SO₂ removal capacity was shown by some of the studied samples that can be related to their textural properties. Cycles of SO₂ adsorption/regeneration were carried out in order to evaluate the possibility of thermal regeneration and re-use of these carbons. Regeneration of the exhausted carbons was carried out at 400 °C of temperature and a flow of 25 ml/min of Ar. After each cycle, the SO₂ removal capacity of the sample decreases.     

Microwave dielectric properties and microstructures of MgTa2O6 ceramics with CuO addition

The effect of CuO addition on the microstructures and the microwave dielectric properties of MgTa₂O₆ ceramics has been investigated. It is found that low level-doping of CuO (up to 1 wt.%) can significantly improve the density of the specimens and their microwave dielectric properties. Tremendous sintering temperature reduction can be achieved due to the liquid phase effect of CuO addition observed by scanning electronic microscopy (SEM). The sintered samples exhibit excellent microwave dielectric properties, which depend upon the liquid phase and the sintering temperature. With 0.5 wt.% CuO addition, MgTa₂O₆ ceramic can be sintered at 1400 °C and possesses a dielectric constant (_r) of 28, a Q × f value of 58000 GHz and a temperature coefficient of resonant frequency (τ_f) of 18 ppm/°C.     

Glass-free LTCC microwave dielectric ceramics

The sintering behavior, microstructure and microwave dielectric properties of complex pyrophosphate compounds AMP₂O₇ (A = Ca, Sr; M = Zn, Cu) were investigated in this paper. All compounds could be densified below the temperature of 950 °C without any glass addition, and exhibit low permittivity (_r < 8), high Q × f value and negative temperature coefficient of resonant frequency. The Q × f value was discussed from the point of view of bond strength. The chemical compatibility with silver and copper was also investigated. All compounds seriously react with silver at 700 °C. However SrZnP₂O₇ could be co-fired with copper in reduced atmosphere. The microwave dielectric properties of SrZnP₂O₇ sintered at 950 °C in reducing atmosphere are: _r = 7.06, Q × f = 52781 GHz, τ_f = −70 ppm/°C. In terms of its lower sintering temperature, chemical compatibility with copper and good microwave dielectric properties, SrZnP₂O₇ ceramic is very promising for low temperature co-fired ceramic (LTCC) applications.     

Characterization of the thorium phosphate-hydrogenphosphate hydrate (TPHPH) and study of its transformation into the thorium phosphate-diphosphate (β-TPD)

The preparation of thorium phosphate-diphosphate (Th₄(PO₄)₄P₂O₇, TPD) was developed through the precipitation of thorium phosphate-hydrogenphosphate hydrate (Th₂(PO₄)₂(HPO₄)·H₂O, TPHPH) at 150–160 °C in closed PTFE container or in autoclaves. From EPMA analyses and SEM observations, the initial precipitate was single phase and multilayered. The behaviour of TPHPH (orthorhombic system with a = 21.368(2) Å, b = 6.695(1) Å and c = 7.023(1) Å) was followed when heating up to 1250 °C. It was first dehydrated leading to the anhydrous thorium phosphate-hydrogenphosphate (TPHP, orthorhombic system with a = 21.229(2) Å, b = 6.661(1) Å and c = 7.031(1) Å at 220 °C) after heating between 180 and 200 °C. This one turned progressively into the new low-temperature variety of TPD (called -TPD, orthorhombic system with a = 21.206(2) Å, b = 6.657(1) Å and c = 7.057(1) Å at 300 °C) correlatively to the condensation of hydrogenphosphate groups into diphosphate entities. These three phases (TPHPH, TPHP and -TPD) exhibit closely related 2D layered structures, therefore different from the 3D structure of the thorium phosphate-diphosphate (high-temperature variety). This latter compound, now called β-TPD, was obtained by heating -TPD above 950 °C. All the techniques involved in this study (XRD, Raman and IR spectroscopy, ¹H and ³¹P NMR) confirmed the successive chemical reactions proposed.     

Low temperature metal oxide film deposition and reaction kinetics in supercritical carbon dioxide

An effective method is developed for low temperature metal oxide deposition through thermal decomposition of metal diketonates in supercritical carbon dioxide (scCO₂) solvent. The rates of Al(acac)₃ (Aluminum acetyl acetonate) and Ga(acac)₃ (Gallium acetyl acetonate) thermal decomposition in scCO₂ to form conformal Al₂O₃ and Ga₂O₃ thin films on planar surfaces were investigated. The thermal decomposition reaction of Al(acac)₃ and Ga(acac)₃ was found to be initialized at  150 °C and 160 °C respectively in scCO₂ solvent, compared to  250 °C and 360 °C in analogous vacuum-based processes. By measuring the temperature dependence of the growth rates of metal oxide thin films, the apparent activation energy for the thermal decomposition of Al(acac)₃ in scCO₂ is found to be 68 ± 6 kJ/mol, in comparison with 80–100 kJ/mol observed for the corresponding vacuum-based thermal decomposition reaction. The enhanced thermal decomposition rate in scCO₂ is ascribed to the high density solvent which effectively reduces the energy of the polar transition states in the reaction pathway. Preliminary results of thin film deposition of other metal oxides including ZrO_x, FeO_x, Co₂O₃, Cr₂O₃, HfO_x from thermal decomposition of metal diketonates or fluorinated diketonates in scCO₂ are also presented.     

Temperature effects of PTFE diffusers

Poly(tetrafluoroethylene) (PTFE) is the most commonly used diffuser material in ultraviolet irradiance measurements. The temperature sensitivities of five PTFE diffusers were measured over a broad temperature range. The transmittance change varied from −0.015%/°C to −0.1%/°C. At 19 °C there was an unexpected abrupt change in transmittance ranging from 1% to 3%. This change is due to the change of the crystal structure of PTFE at 19 °C. Temperature sensitivity decreases significantly the accuracy of high precision measurements, especially if the temperature of the diffusers is not stabilized.