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1.
The formation of self-organized porous titania is achieved by electrochemical anodization under a potentiostatic regime. Anodic titanium oxide (ATO) was fabricated by a three-step self-organized anodization of the Ti foil in an ethylene glycol electrolyte containing 0.38 wt% of NH4F and 1.79 wt% of H2O. Anodizing was carried out at the constant cell potential ranging from 30 to 70 V at the temperature of 20 °C. It was found that nanoporous TiO2 arrays can be obtain only after a short duration of the third step (10 min). The influence of anodizing potential on the structural parameters of porous anodic titania including pore diameter, interpore distance, wall thickness, porosity and pore density was extensively studied. The linear dependencies between interpore distance, pore diameter and wall thickness upon the anodizing potential were found. The regularity of pore arrangement was monitored qualitatively by fast Fourier transforms (FFTs) of top-view FE-SEM images. It was found that the best arrangement of nanopores is observed at 40 V. This finding was confirmed by the analysis of pore circularity. The highest circularity of pores was observed once again at 40 V.  相似文献   

2.
We investigated the formation of self-organized zirconium titanate nanotubes by anodizing a Ti-35Zr alloy in 1 M (NH4)2SO4 + 0.1-2.0 wt.% NH4F electrolytes. The morphology and composition of the zirconium titanate nanotube are controlled by the applied electrochemical conditions. The outer diameter of nanotubes is controlled by the anodization potential in the range between 1 and 100 V (versus Ag/AgCl). Tubes with diameters from 14 to 470 nm can be grown. The nanotube length correlates with the anodic charge up to a length where significant dissolution of the nanotube layer is observed. The wall thickness, composition of the nanotubes and porosity of the nanotube layer are significantly affected by the fluoride ion concentration. The length limiting factor of the nanotube growth is found to be the diffusion of ionic species in the electrolyte.  相似文献   

3.
Carbon nanotubes (CNTs) with larger diameter were synthesized over anodic titanium oxide (ATO) template by CVD method using acetylene as carbon source. The porous titanium oxide was obtained by anodization of titanium metal in a mixture of 1 M H2SO4 + 0.5% HF electrolyte at a constant applied potential of 40 V. The XRD analysis of anodized titanium revealed that rutile and anatase forms of TiO2 are formed due to anodization. Further, SEM analysis was used to follow the development of pores on titanium surface. The TEM analysis revealed that the formed CNTs are straight and hollow with uniform wall thickness as well as larger diameter (70–80 nm). HRTEM study showed that the formed CNTs are multi-walled and their wall thickness is around 2–3 nm. Further, the structural features of the formed CNTs were studied by XRD. Raman spectroscopy was used to study the degree of graphitization of CNTs. The Lewis acid sites of TiO2 present in the internal surface of the pores play an important role in the catalytic decomposition of acetylene and hence the formation of CNTs. When increasing the carbon deposition time, the wall thickness of CNTs is not increased significantly, indicating that the decomposition of acetylene is due to Lewis acid sites of TiO2 and not due to thermal decomposition. Further, the morphology of CNTs formed over ATO template was compared with that of CNTs formed on Co electrodeposited ATO. There is no significant difference in morphology as well as wall thickness was observed between the CNTs grown over ATO with and without Co catalyst. But, still further investigations are necessary to study the structural differences between the CNTs grown over ATO with and without Co catalyst.  相似文献   

4.
Self-aligned nanoporous TiO2 templates synthesized via dc current electrochemical anodization have been carefully analyzed. The influence of environmental temperature during the anodization, ranging from 2 °C to ambient, on the structure and morphology of the nanoporous oxide formation has been investigated, as well as that of the HF electrolyte chemical composition, its concentration and their mixtures with other acids employed for the anodization. Arrays of self-assembled titania nanopores with inner pores diameter ranging between 50 and 100 nm, wall thickness around 20–60 nm and 300 nm in length, are grown in amorphous phase, vertical to the Ti substrate, parallel aligned to each other and uniformly disordering distributed over all the sample surface. Additional remarks about the photoluminiscence properties of the titania nanoporous templates and the magnetic behavior of the Ni filled nanoporous semiconductor Ti oxide template are also included.  相似文献   

5.
The aim of the work was to develop an optimized routine for apple drying. The interaction of the drying parameters air temperature (35–85°C), dew point temperature (5–30°C), and air velocity (2.0–4.8 m/s) with drying time, color changes, and shrinkage was determined. Non-invasive online measurement techniques in the form of artificial vision systems in visible and infrared spectrum were developed and applied to guarantee an uninterrupted process. Quantification methods for the determination of color and shape changes of apple slices were established based on the images taken.

Results show that digital images are a feasible alternative for the monitoring of the relative changes in L* (R2 = 0.92, p < 0.001), a* (R2 = 0.96, p < 0.001), and b* (R2 = 0.96, p < 0.001) during the drying of apples. It was observed that the color parameters as a function of moisture content follow a third-order development while shrinkage was linear (p < 0.001). The developed models for drying time tdr (R2 = 0.99, p < 0.001), Total Color Difference ΔE (R2 = 0.95, p < 0.001), and shrinkage S (R2 = 0.68, p < 0.05) illustrate high interdependencies of the factors involved for the quality criteria studied. Throughout the parameter space investigated, increasing air velocity was shown to have a positive effect on the quality criteria investigated.  相似文献   

6.
The series of trichlorotitanium 2-(2-pyridinyliminomethyl)phenolates, [4,6-tBu2C6H2O-2-CHNC5R1-4N]TiCl3 (R1-4 = H (1); R1,3,4 = H, R2 = Me (2); R1,2,4 = H, R3 = Me (3); R2,4 = H, R1,3 = Me (4); R1,3 = H, R2 = CF3, R4 = Cl (5)), were synthesized and characterized by elemental analysis and 1H/13C NMR spectroscopy. The molecular structures of the representative complexes 2 and 4 were confirmed by single-crystal X-ray diffraction, and revealed distorted octahedral geometry at titanium. In the presence of MAO, all titanium pro-catalysts showed good activities for ethylene polymerization with good thermal stability at the optimum temperature of 50 °C. In comparison with the ethylene polymerization results, the activity observed for the co-polymerization of ethylene/1-hexene was far lower, but the polymers produced were of high molecular weight. For the co-polymerization of ethylene/1-octene, enhanced catalytic activity was observed, with 1-octene incorporation of up to 3.83 mol%.  相似文献   

7.
Anodic aluminum oxide (AAO) membranes with a highly ordered nanopore arrangement typically serve as ideal templates for the formation of various nanostructured materials. A typical procedure of the template preparation is based on a two-step self-organized anodization of aluminum carried out at the temperature of about 1-3 °C. In the current study, AAO templates were fabricated in 0.3 M oxalic acid under the anodizing potential range of 30-65 V at a relatively high electrolyte temperature ranging from 20 to 30 °C. Due to a high rate of porous oxide growth, about 5-10-fold higher than in low-temperature anodizing, the process of the template fabrication can be shorten significantly. Similarly to the low-temperature anodization, the best hexagonal pore arrangement is observed for samples anodized at 40 V. With a prolonged duration of the first anodizing step the order degree of triangular nanoporous lattice, observed after the second anodization, improves considerably. The effects of the anodizing potential and the process duration on the structural features of porous anodic alumina such as: pore diameter (Dp), interpore distance (Dc), porosity (P), pore density (n) and anodizing ratio (BU) were investigated in details at various temperatures. The obtained results were compared with theoretical predictions and data reported in the literature.  相似文献   

8.
In an investigation of structure–property–processing relationships for SWCNT thin film piezoresistive sensors, the gauge factor of the sensors for a small tensile deformation (less than 2% strain) was found to be close to unity and showed negligible dependence on the film thickness and SWCNT bundle length (L) and diameter (d). However, for a large tensile deformation (20–30% strain), the film thickness and the microstructure of SWCNTs had a compounding effect on the piezoresistive behavior. A gauge factor of ∼5 was obtained for the sensors fabricated with SWCNT bundles of short length and thin diameter (L = 549 nm and d = 3.7 nm) with thicker films. Furthermore, the gauge factor of the sensors was found inversely proportional to the excluded volume Vex of SWCNT bundles (Vex  1/L2 d).  相似文献   

9.
In this paper we present new experimental data on the steady-state, mean squared, fluctuation velocity, or granular temperature, of Geldart B polymer, glass, nickel, and stainless steel monodispersed spheres averaged over the wall of a gas fluidized bed, as a function of gas flow and sphere diameter. The granular temperature is obtained by Acoustic Shot Noise technology—namely power spectral analysis of the steady state vibrational energy of the wall excited by random sphere impact, and calibrated by hammer excitation over the wall. The new data extends to polymer and metallic spheres the experimental discovery of a 1996 paper of Cody et al. that the fluctuation velocity of Geldart B glass spheres when scaled to the gas superficial velocity, Us, is inversely proportional to sphere diameter, directly proportional to a fundamental length scale, DoB, and is a universal function of U = (Us / Umf). We also demonstrate that the new data is consistent with the diameter dependence of the fluctuation velocity that can be derived from both the 1997 paper of Menon and Durian, who measured random sphere motion near the wall through the spectroscopy of scattered laser light, and the 1992 paper of Rahman and Campbell, who measured the average granular pressure of random sphere impact on a porous steel membrane. While the inverse scaling of the fluctuation velocity with sphere diameter, and the existence of a fundamental length scale for gas fluidization, DoB, had not been a feature of any published fundamental model, or computer simulation, of the steady state granular temperature of spheres in gas fluidized beds, we show that it is a feature of two recent dense kinetic fluidization models published in 1999, by Buyevich and Kapbasov, and Koch and Sangani. Both theories implicitly define a fundamental length scale for the fluctuation velocity, D? = (μf2 / ρp2g)1 / 3, where ρp is the sphere density, μf is the gas viscosity, and g is the laboratory gravitational field. The new data for polymer, glass, nickel and stainless steel spheres presented in this paper, defines DoB = (56 ± 2)D?. We use the Anderson-Jackson stability model to show that the length scale DoB, also defines a stability length scale, such that for D < DoB(D > DoB), the uniform dense phase of the fluidized bed is stable (unstable), against one dimensional, first order fluctuations in sphere concentration. The length scale, DoB is thus the theoretical equivalent to the empirical scaling length introduced by Geldart, DB/A, to distinguish spheres (D > DB/A) that bubble at fluidization, from spheres (D < DB/A) that fluidize before bubbling. Finally, we present new experimental data, on the remarkable changes in the granular temperature, bed expansion, and bed collapse time, between Geldart B and Geldart A monodispersed glass spheres, and compare that data to granular temperature, and bed expansion, for Geldart A rough, non-spherical, log-normal dispersed diameter catalytic particles.  相似文献   

10.
The present work demonstrates that morphology of TiO2?CWO3 composite nanotubes formed by alloy anodization can be tuned by controlling applied voltages and time. Distinctive tube morphology can be formed by applying a voltage of more than 80?V. Nanotube diameter and length have a linear relationship with the anodization voltage with a current efficiency of almost 100?%. Furthermore, compared to pure TiO2, the composite nanotubes show a very uniform tube diameter along the tube axis even at the extended anodization time.  相似文献   

11.
A series of novel half-metallocene-type titanium complexes CpTiCl2[PhNC(R2)CHC(R1)O] (2a, R1 = Cy, R2 = CF3; 2b, R1 = tBu, R2 = CF3; 2c, R1 = Ph, R2 = CF3; 2d, R1 = Ph, R2 = CH3) have been synthesized by treating CpTiCl3 with the corresponding bidentate β-enaminoketonato ligands PhNC(R2)CHC(R1)OH in the presence of triethylamine. Single crystal X-ray diffraction revealed that complex 2b adopts distorted square-pyramid geometry around the titanium center. The complexes 2a-d were investigated as the catalysts for ethylene polymerization and the copolymerization of ethylene with norbornene. All the complexes were active towards ethylene (co)polymerization in the presence of modified methylaluminoxane, and produced high molecular weight (co)polymers. The catalytic activity and the norbornene incorporation were highly dependent upon catalyst and reaction conditions employed. Among four complexes, 2c exhibited both high catalytic activity and efficient norbornene incorporation under the same conditions, affording high molecular weight copolymers with unimodal molecular weight distributions.  相似文献   

12.
《Ceramics International》2015,41(7):8735-8741
Highly ordered copper doped TiO2 nanotube arrays (CuTiO2NTs) thin-film were prepared in an aqueous solution containing NH4F and different concentrations of copper nitrate via the electrochemical oxidation of titanium substrates. The resulting nanotubes were characterized by FE-SEM, XRD, XPS and EDX. The CuTiO2NTs showed a tube diameter of 40–90 nm and wall thickness of 20–30 nm. Diffuse reflectance spectra showed a shift toward longer wavelengths relative to pure TiO2 nanotubes (TiO2NTs). The visible light photo-catalytic activity of the CuTiO2NTs electrodes was evaluated by the removal of methylene blue (MB) dye and the production of hydrogen. The results showed that CuTiO2NTs samples exhibited better photo-catalytic activity than the TiO2NTs. This work demonstrated a feasible and simple anodization method to fabricate an effective, reproducible, and inexpensive visible-light-driven photo-catalyst for hydrogen evolution and environmental applications.  相似文献   

13.
Experimentally, it was shown that using a gas-dynamic correction in the plasma torch operation mode of jet expansion absence increases the efficiency of DC synthesis more than 10 times. Moreover, the diameter of the homogeneous part of a coating is increased not less than twice in relation to the diameter of the plasma jet.The theoretical explanation of the obtained result is given. It was shown that at subsonic speed of plasma flow spreading along the substrate radius, this effect can only be obtained at Reynolds numbers not exceeding the critical value RrRr cr=13456.The maximum area of uniform thickness DC is not less than 6 cm2.  相似文献   

14.
《Ceramics International》2020,46(6):7306-7323
This study aimed to prepare nanoporous anodic alumina on AA3003-H14 aluminum alloy using a mild anodization process with minimal working voltage and treatment time. The microstructural features, mechanical properties, and tribocorrosion behavior of the coatings were assessed to determine the optimum conditions for the fabrication of nanoporous anodic alumina on AA3003-H14 alloy. The microstructural analysis showed both uniform and nonuniform pore nucleations during anodization in H2SO4/C2H2O4, H2SO4/H2CrO4, and EG/H2O/NH4F electrolytes, where the optimal nanoporous structure with an average thickness, porosity, pore diameter, and interpore distance of 382 nm, 19%, 16 nm, and 35 nm, respectively, was developed after a short-time mild anodization for 30 min at constant potential of 12 V using 15 wt% H2SO4 electrolyte. The XRD profiles indicated formation of a highly-disordered and amorphous nanoporous anodic alumina. Due to the loss of mechanical properties after heat treatment at 450 °C for 90 min, Vickers microhardness of the samples decreased drastically from 124 to 90.5 HV, respectively. The wear analysis indicated an improved tribological behavior by mild electrochemical anodization owing to the development of nanoporous anodic alumina, which acted as the liquid lubricant reservoir and increased the tribological performance of the workpiece. In addition, the heat treated specimen showed the lowest corrosion rate of 0.079 mm.y-1 and utmost corrosion protection efficiency of 95.24% following exposure in palm oil methyl ester (B100). This novel nanoporous configuration not only endows excellent tribological performance in the biofuel combustion environment, but also particularly decreases consumption of liquid lubricants through a facilitated multiphase lubrication mechanism.  相似文献   

15.
Glass for pharmaceutical packaging requires high chemical durability for the safe storage and distribution of newly developed medicines. In borosilicate pharmaceutical glasses which typically contain a mixture of different modifier ions (alkali or alkaline earth), the dependence of the chemical durability on alkaline earth oxide concentrations is not well understood. Here, we have designed a series of borosilicate glasses with systematic substitutions of CaO with MgO while keeping their total concentrations at 13 mol% and a fixed Na2O concentration of 12.7 mol%. We used these glasses to investigate the influence of R = [MgO]/([MgO] + [CaO]) on the resistance to aqueous corrosion at 80°C for 40 days. It was found that this type of borosilicate glass undergoes both leaching of modifier ions through an ion exchange process and etching of the glass network, leading to dissolution of the glass surface. Based on the concentration analysis of the Si and B species dissolved into the solution phase, the dissolved layer thickness was found to increase from ~100 to ~170 nm as R increases from 0 to 1. The depth profiling analysis of the glasses retrieved from the solution showed that the concentration of modifier ions (Na+, Ca2+, and Mg2+) at the interface between the solution and the corroded glass surface decreased to around 40%–60% of the corresponding bulk concentrations, regardless of R and the leaching of modifier cations resulted in a silica-rich layer in the surface. The leaching of Ca2+ and Mg2+ ions occurred within ~50 and <25 nm, respectively, from the glass surface and this thickness was not a strong function of R. The leaching of Na+ ions varied monotonically; the thickness of the Na+ depletion layer increased from ~100 nm at R = 0 to ~200 nm at R = 1. Vibrational spectroscopy analysis suggested that the partial depletion of the ions may have caused some degree of the network re-arrangement or re-polymerization in the corroded layer. Overall, these results suggested that for the borosilicate glass, replacing [CaO] with [MgO] deteriorates the chemical durability in aqueous solution.  相似文献   

16.
Sesame seed is a rich source of dietary lignans   总被引:6,自引:0,他引:6  
The variation in the contents of sesamin and sesamolin was studied in oils extracted from 65 samples of sesame seeds (Sesamum indicum L.) from plants with shattering (n=29), semishattering (n=7), and nondehiscent (n=29) capsules. The oil content ranged from 32.5 to 50.6% and was greater in white than black seeds (P<0.001). The sesamin and sesamolin contents in seeds ranged from 7 to 712 mg/100 g (mean±SD, 163±141 mg/100 g) and from 21 to 297 mg/100 g (101±58 mg/100 g), respectively, with no difference between black and white seeds. Thus, there was a wide variation in the contents of sesamin and sesamolin, which were positively correlated (R 2=0.66, P<0.001). There were negative correlations between the contents of sesamin and the contents of sesaminol (R 2=0.37) and sesamolinol (R 2=0.36) and between the content of sesamolin and those of sesaminol (R 2=0.35) and sesamolinol (R 2=0.46) (P<0.001). Sesame seeds had an average of 0.63% lignans, making them a rich source of dietary lignans.  相似文献   

17.
Porous geopolymer foams are promising lightweight materials combining strong strength and adsorption properties. A waste-based porous open-cell geopolymer (POG) was synthesized by one-pot method and investigated in terms of unconfined compressive strength (UCS), pore distribution and adsorption ability. This paper investigates the effect of preparation conditions (raw materials and stabilizing/foaming agents proportion, modulus, curing temperature) on the performance of POG. Results indicated that POG was successfully prepared by industrial wastes (blast furnace slag, BFS) and municipal wastes (water treatment residue, WTR). The appropriate range of conditions were determined for the preparation of POG (H2O2 = 1.50 ~ 2.50 wt%, K12 = 1.50 ~ 2.00 wt%, modulus = 1.25 ~ 2.00, and temperature = 60 ~ 70 °C). Under these conditions, the UCS in the range 1.77 ~ 4.77 MPa, and the total porosity in the range 35.19 ~ 69.97 vol%. The extreme environments resulted in the form of instable structure and discontinuous pore structure. The statistical results demonstrated that the total porosity, mean diameter, and max diameter of POG are significantly negative correlated with UCS, and the relationship of total porosity and UCS can be described by Ryshkevith (R2=0.8459) and Schiller model (R2=0.8689). Compared to the geopolymer bulk, POG showed significant adsorption advantage for heavy metal cations and cationic dyes, and the adsorption removal rates of POG for Cd2+, Cu2+, Pb2+, and MB rising to 92.25%, 119.80%, 110.77%, and 163.98%, respectively. The adsorption mechanisms are mainly based on the negative charge of [AlO4]- tetrahedron and cation exchange between heavy cations and Na+ or Ca2+ in internal matrix. This study indicated that the BFS and WTR are feasible solid wastes for the fabrication of POG, which can be applied in the filtration and adsorption fields for contaminants removal.  相似文献   

18.
《Ceramics International》2021,47(23):33028-33038
Natural pozzolan is a promising precursor for the synthesis of alkali-activated geopolymers. However, the acid activation of pozzolan is very poorly developed. In this respect, this paper presents an optimization study of the synthesis of geopolymers based on pozzolan and phosphoric acid using the Design Of Experiments (DOE) methodology. Indeed, a Box Behnken Design (BBD) associated with the Response Surface Methodology (RSM) is used. The analysis of variance ANOVA showed that the factors used for the modeling are significant in their sets. Thus, the study of the adjustment confirms the validation of the established models, by very high values of adjusted coefficient of determination (R2Adj-Cs = 95.63%, R2Ad-PWV = 95.73%, R2Adj-D = 97.62%, R2Adj-P = 98.24%, R2Adj-WA = 95.52%). Similarly, the RSM tool showed that the optimal conditions to elaborate a geopolymer with good physicomechanical properties (Compressive strength = 21.57 MPa, P-wave velocity = 2110 m/s, Density = 1.95 g/cm3, Porosity = 12.8%, Water absorption = 6.06%) are as follows: Si/P = 1.25, H2O/H3PO4 = 2, and Li/So ratio = 0.9. Microstructural characterization of the optimal geopolymer by XRD and FTIR showed that the pozzolan is actively reacted with phosphoric acid, under the optimal conditions found by the Box Behnken Design model. This is revealed by the formation of a significant amount of amorphous phase, the formation of a new monetite-like mineral phase as well as the formation of Si–O–P bonds, which are the basis of the physicomechanical properties found.  相似文献   

19.
Supercritical fluid extraction of flaxseed oil with carbon dioxide was performed. Effects of particle size, pressure, temperature and the flow rate of supercritical carbon dioxide (SC-CO2) were investigated. Response surface methodology was used to determine the effects of pressure (30–50 MPa), temperature (50–70 °C) and SC-CO2 flow rate (2–4 g/min) on flaxseed oil yield in SC-CO2. The oil yield was represented by a second order response surface equation (R 2 = 0.993) using the Box-Behnken design of experiments. The oil yield increased significantly with increasing pressure (p < 0.01), temperature (p < 0.05) and SC-CO2 flow rate (p < 0.01). The maximum oil yield from the response surface equation was predicted as 0.267 g/g flaxseed for 15 min extraction of 5 g flaxseed particles (particle diameter <0.850 mm) at 50 MPa pressure and 70 °C temperature, with 4 g/min solvent flow rate. Total extraction time at these conditions was predicted as 22 min.  相似文献   

20.
Frank P. Bell  Edna V. Hubert 《Lipids》1982,17(10):672-675
The effect of chlorpromazine, a major tranquilizer, on arterial lipid metabolism was studied in vitro in rat aortas incubated with [14C] acetate and [14C] mevalonate as lipid precursors. Chlorpromazine at a level of 0.25 mM in the incubation medium significantly reduced the incorporation of [14C] acetate into free fatty acids (p<0.01) and total phospholipids (p<0.001) but not triglycerides. Chlorpromazine also altered the pattern of arterial phospholipids synthesized from [14C] acetate by significantly increasing the relative proportion of phosphatidylinositol plus phosphatidylserine (p<0.02) and reducing the relative proportion of sphingomyelin (p<0.001). [14C] Acetate incorporation into the combined fractions of steryl esters plus hydrocarbons and sterols plus diglycerides was also significantly reduced (p<0.001) by 0.25 mM chlorpromazine. Studies with [14C] mevalonate showed that chlorpromazine is also an inhibitor of sterol biosynthesis in arterial tissues as evidenced by 35–40% reductions (p<0.05) in the formation of14C-labeled squalene and C27 sterols.  相似文献   

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