Fabrication of optical reflectors by using of elastomer with self-organized undulations

Back-surface diffusive reflectors have been widely applied in many optical systems to promote the efficiency used in system. In this work, we propose a novel way to fabricate a soft diffusive reflector by using of silicone (polydimethylsiloxane, PDMS). High-reflectance substrates were first fabricated by mixing nanoscaled TiO₂ powders with PDMS polymers, and then microscale wave-like undulations were spontaneously developed after the substrates were dipped into H₂SO₄/HNO₃ solutions. After optical examination, a TiO₂/PDMS plate comprising microscale undulations, which can surely serve as a reflector, could reflect and diffuse light effectively. Besides, all fabrication processes can be executed in the ambient environment and at low temperature. This proposed method has a potential for mass production in the future.     

The calorimetric investigation of the graphite–HNO3–R system (R=CH3COOH,H2SO4)

The interactions of highly oriented pyrolytic graphite with HNO₃–R (R=CH₃COOH, H₂SO₄) solution were investigated by Calvet type calorimeter at 305.5 K and X-ray diffraction. It was shown that in the graphite–98% HNO₃–100% CH₃COOH system the enthalpy of the formation and the stage number of graphite nitrate depends on HNO₃ percentage in the solution. Calorimetric investigation of the graphite–98% HNO₃–96% H₂SO₄ system demonstrated that the shape of the heat flow curves corroborates the co-intercalation of HNO₃ and H₂SO₄ into graphite. It was established that the formation of the first stage of ternary compounds of variable composition takes place.     

Surface modification of carbon nanotubes for enhancing BTEX adsorption from aqueous solutions

Carbon nanotubes (CNTs) were fabricated by the catalytic chemical vapor deposition method and oxidized by HCl, H₂SO₄, HNO₃ and NaOCl solutions for enhancing benzene, toluene, ethylbenzene and p-xylene (BTEX) adsorption in an aqueous solution. The surface nature of CNTs was changed after the H₂SO₄, HNO₃ and NaOCl oxidation, which makes CNTs that adsorb more BTEX. The NaOCl-oxidized CNTs show the greatest enhancement in BTEX adsorption, followed by the HNO₃-oxidized CNTs, and then the H₂SO₄-oxidized CNTs. The adsorption mechanism of BTEX via CNTs is mainly attributed to the π-π electron-donor-acceptor interaction between the aromatic ring of BTEX and the surface carboxylic groups of CNTs. The NaOCl-oxidized CNTs have superior adsorption performance of BTEX as compared to many types of carbon and silica adsorbents reported in the literature. This suggests that the NaOCl-oxidized CNTs are efficient BTEX adsorbents and that they possess good potential applications for BTEX removal in wastewater treatment.     

Modification of multi-walled carbon nanotubes for electric double-layer capacitors: Tube opening and surface functionalization

Multi-walled carbon nanotubes (MWCNTs) obtained opening the closed ends and using surface functionalization by means of a combination of partial oxidation in air and chemical modifications are characterized systematically in 0.3 M H₂SO₄ between 0 and 1.0 V, and these nanotubes were planned to be used as electrode materials in electric double-layer capacitors (EDLCs). Opening of MWCNTs, clearly observed by means of transmission electron microscopy (TEM), can be easily achieved by the partial oxidation in air through a seven-step temperature program identified by thermogravimetric/differential thermal analyses (TG/DTA). An increase in 175% specific capacitance is obtained for the MWCNTs, partially oxidized in air and chemically modified in H₂SO₄+HNO₃. The temperature-programmed desorption (TPD) data showed that evolutions of CO and CO₂ are, respectively, promoted by the application of partial oxidation in air and chemical modification in H₂SO₄+HNO₃. The above increase in specific capacitance for modified MWCNTs is attributed to an obvious increase in the BET surface area (double-layer capacitance) and the density of oxygen-containing surface functional groups (pseudocapacitance).     

Functionalization of carbon encapsulated iron nanoparticles

Carbon-encapsulated magnetic nanoparticles are a new class of materials where the core magnetic nanoparticle is protected from reactions with its environment by graphite shells. Having a structure similar to carbon nanotubes, these nanoparticles could be potentially functionalized using methods which are already applied to those structures. We present the effects of acidic treatments based on HCl, HNO₃, and H₂SO₄ on these nanoparticles highlighting the impact on their magnetic and surface properties. We show that acidic treatments based on HNO₃ can be successfully applied for the generation of carboxylic groups on the surface of the nanoparticles. Using methylamine as a model, we demonstrate that these functional groups can be used for further functionalization with amino-containing biomolecules via diimide-activated amidation.     

Improvement of the polishing treatment for niobium surfaces of superconducting cavity resonators

For superconducting cavities made from niobium sheet, which are interesting in the field of accelerator applications, smooth and defect free inner surfaces are needed to achieve a high unloadedQ along with high accelerating field strength. These can be obtained using chemical polishing procedures. Whereas normally a mixture of HF, HNO₃, and H₃PO₄ is applied, we chose the known bath containing HF, HNO₃, and H₂SO₄ and worked above 50 °C. The surface quality was judged by visual inspection using a light microscope as well as by microwave measurements of one spherical resonator. The new method gave less grain boundary etching and, with high field levels, an enlarged unloadedQ.     

Effects of different carbon precursors on synthesis of multiwall carbon nanotubes: Purification and Functionalization

Cyclohexanol and xylene were used as carbon precursors, for synthesis of multiwall carbon nanotubes (MWCNTs) arrays in a CVD system at temperature of 750 °C, using nitrogen as carrier gas and ferrocene as catalyst. Different characterization methods were employed to compare the MWCNTs structure synthesized by these two precursors. All scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermal gravimetric analysis (TGA) and Raman spectroscopy results illustrated that using cyclohexanol could significantly reduce formation of amorphous carbon and catalyst particles in the as-grown CNTs. The less amorphous carbon can be attributed to in situ oxidation in presence of oxygen atom of cyclohexanol. Characterizations showed that MWCNTs with high purity could be obtained using cyclohexanol as carbon precursor. The as-grown MWCNTs were purified by oxidation and acid treatment. Characterization of the purified MWCNTs using HNO₃/H₂SO₄ (1/3 or 1/1), 8 M HCl or 8 M HNO₃ was carried out. The results showed that 8 M HNO₃ could be considered as the best chemical to obtain more pure MWCNTs, less amorphous and metal particles and less damaged MWCNTs. The Raman spectroscopy results demonstrated that HNO₃/H₂SO₄ (1/3) treatment could more disorder the MWCNTs structure and this was attributed to the bigger destroying effect of this acid treatment. Furthermore, the TEM analysis of MWCNTs before and after acid treatment revealed that acid treatment could remove encapsulated catalyst particles. The FTIR analysis illustrated that purification of the MWCNTs with nitric acid could connect the functional groups onto the outer surface of MWCNTs and this resulted in more dispersion of the MWCNTs in water.     

Oxidation of Activated Carbon in Liquid Phase. Study by FT-IR

Surface chemistry of a commercial activated carbon (AC) and of products oxidized in liquid phase using aqueous solutions of a series of oxidizing agents (H₂SO₄, HNO₃, HClO₄, H₂O₂, O₃, ClO₂, KlO₄ and KMnO₄) has been studied by FT-IR. Oxidation led to surface groups and structures which, and also the extend of formation, depended on the oxidizing agent and the pH and concentration of the solution used. Most oxidizing agents proved to be effective for the formation of surface C[dbnd]O groups. Variations in pH of solutions of H₂O₂, KlO₄ and KMnO₄ unequally affected the oxidation of AC. This was unfavourable with the increase in concentration of the solutions of HNO₃ and KMnO₄. The reverse was noted with KlO₄.     

The influence of treatment duration on multi-walled carbon nanotubes functionalized by H2SO4/HNO3 oxidation

Variation in the nature of multi-walled carbon nanotubes (MWCNTs) subjected to different degrees of oxidation was investigated. The microstructure was determined by high resolution transmission electron microscopy (HRTEM) and X-ray diffraction (XRD) methods, and the surface chemistry was evaluated in terms of the functional groups determined by X-ray photoelectron spectroscopy (XPS) and thermal analysis-mass spectroscopy (TA-MS). In addition, TGA was used to indicate the thermal stability of the nanotubes. Results demonstrate that the graphitic structure of nanotubes oxidized with a mild mixture of H₂SO₄/HNO₃ was preserved. Decrease in the degree of crystallinity started with widening of the C(0 0 2) XRD diffraction peak, followed by this peak shifting towards lower angles. The oxygen content increased with increasing treatment time. A defect peak incorporated in deconvolution of XPS C1s spectra was helpful for detecting the generation of defect sites. The predominant surface functionalities of the nanotubes have been changed from basic to acidic groups after treatment for one day. The samples oxidized for two days had the most abundant surface -COOH and the highest oxidation resistance. The oxidation mechanism of MWCNTs in mild H₂SO₄/HNO₃ mixture was proposed, which was a successive and iterative process, including the initial attack on active sites, and next the hexagon electrophilic attack generating new defects and introducing more oxygen, and then the tubes becoming thinner and shorter.     

Cutting of multi walled carbon nanotubes

Multi walled carbon nanotubes (MCNT) synthesized by CVD method have been successfully cut into different lengths by controlling H₂SO₄/HNO₃ (5:3) oxidation time. During the cutting process H₂SO₄ and HNO₃ were added independently and the oxidation processes were carried out at a lower temperature to void excess weight loss and damage to MCNT. The resulting shorted MCNT (s-MCNT) formed stable dispersion state in the polar solvents without the help of surfactants that provided possibility for further functionalization and application. Moreover, NaOH solution was used to determine the total percentage of acidic sites and the total percentage of acidic sites are about 0.2-1%.     

Comparison of Mineral Acids in Wet Digestion of Plant Materials for Flame and Flameless Atomic Absorption Measurement of Metals

Various mineral acids are compared in measuring metals in plant materials by flame and flameless atomic absorption spectrometry. NBS-SRM 1571, Orchard Leaves, is utilized as the plant material. The combination of H₂SO₄ and HNO₃ is found to be the most suitable for measuring Fe, Mn, Cu and Zn by flame atomic absorption spectroscopy, while HNO₃ is found to be the best for measuring Cu, Mn, and Pb by flameless Atomic Absorption spectroscopy.     

Topographic control on silicone surface using chemical oxidization method

The paper describes a wet process for modifying the surface of polydimethylsiloxane (PDMS) using H₂SO₄/HNO₃ solutions. The oxidation on the surface of PDMS was confirmed by the examinations of Fourier transform infrared spectrometry (FTIR), contact angle of water drop and X-ray photoelectron spectroscopy (XPS). The hydrophobic surface of pristine PDMS was not only changed to hydrophilic, but also formed wrinkles on it after chemical modification. Bilayer systems, stiff oxidized PDMS layers were capped on soft PDMS foundations, would generate easily compressive stresses due to the large difference in volumetric contraction rates and led to form wrinkles on the surface. Experimental results demonstrated the periodicity of wrinkles was controllable by controlling the duration of oxidation. Therefore, wrinkles could be arranged orderly by the guidance of external forces before oxidization. The potential technology for generating and ordering wrinkles on the PDMS surface is valuable in the applications of pressure sensors, biology, micro-optics and nano-/micro-fabrication in the future.     

A facile method to modify carbon nanotubes with nitro/amino groups

Nitro groups (-NO₂) have been introduced on the surface of multi-walled carbon nanotubes (MWCNTs) by treatment with a mixture of concentrated H₂SO₄/HNO₃ solution at low temperature (60 °C). Such a low-temperature treatment simultaneously can well prevent MWCNTs from the structural damage. From the nitro-modified MWCNTs, MWCNTs can be readily modified with amino groups by reduction of nitro groups. The prepared amino-modified MWCNTs are highly soluble in polar solvents such as dimethylformamide (DMF), alcohol and acetone. Further, as a demonstration, MWCNTs can be functionalized with guest objects, provided by the strong bonding ability of amino groups.     

Electrochemical behaviors of the magnesium alloy substrates in various pretreatment solutions

Interface reactions and film features of AZ91D magnesium alloy in pickling, activation and zinc immersion solutions have been investigated. The surface morphologies of the specimens were observed with scanning electron microscope (SEM). Electrochemical behaviors of AZ91D magnesium alloy in the baths of pickling, activation and zinc immersion were analyzed based on the open circuit potential (OCP) - time curves in various solutions. The results show that the corrosive rate in HNO₃ + CrO₃ or HNO₃ + H₃PO₄ pickling solution was more rapid than in KMnO₄ pickling-activation solution. Both α phase and β phase of the substrates were uniformly corroded in HNO₃ + CrO₃ or HNO₃ + H₃PO₄ pickling solution, the coarse surface can augment the mechanical occlusive force between the subsequent coatings and the substrates, so coatings with good adhesion can be obtained. In HF activation solution, the chromic compound formed via HNO₃ + CrO₃ pickling was removed and a compact MgF₂ film was formed on the substrate surface. In K₄P₂O₇ activation solution, the corrosion products formed via HNO₃ + H₃PO₄ pickling were removed, a new thin film of oxides and hydroxides was formed on the substrate surface. In KMnO₄ pickling-activation solution, a film of manganic oxides and phosphates was adhered on the substrate surface. Zinc film was symmetrically produced via K₄P₂O₇ activation or KMnO₄ pickling-activation, so it was good interlayer for Ni or Cu electroplating. Asymmetrical zinc film was produced because the MgF₂ film obtained in the HF activation solution had strong adhesive attraction and it was not suitable for interlayer for electroplating. However, the substrate containing compact MgF₂ film without zinc immersion was fit for direct electroless Ni-P plating.     

Investigation of etch characteristics of non-polar GaN by wet chemical etching

We characterized the surface defects in a-plane GaN, grown onto r-plane sapphire using a defect-selective etching (DSE) method. The surface morphology of etching pits in a-plane GaN was investigated by using different combination ratios of H₃PO₄ and H₂SO₄ etching media. Different local etching rates between smooth and defect-related surfaces caused variation of the etch pits made by a 1:3 ratio of H₃PO₄/H₂SO₄ etching solution. Analysis results of surface morphology and composition after etching by scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) demonstrated that wet chemical etching conditions could show the differences in surface morphology and chemical bonding on the a-plane GaN surface. The etch pits density (EPD) was determined as 3.1 × 10⁸ cm⁻² by atom force microscopy (AFM).     

Synthesis and characterization of carbon nanotubes on carbon microfibers by floating catalyst method

In this paper, carbon nanotubes were synthesized on carbon microfibers by floating catalyst method with the pretreatment of carbon microfibers at the temperature of 1023 K, using C₂H₂ as carbon source and N₂ as carrier gas. The morphology and microstructure of carbon nanotubes were characterized by field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). The composition of carbon nanotubes was determined by energy dispersive X-ray spectroscopy (EDX). The results showed that the surface of treated carbon microfibers was thickly covered by carbon nanotubes with diameters of about 50 nm. EDX image indicated that the composition of carbon nanotubes was carbon. In comparison with the sample grown on untreated carbon microfibers surface, it was found that after carbon microfibers were boiled in the solution of sulfur acid and nitric acid (VH₂SO₄:VHNO₃ = 1:3) and immersed in the solution of iron nitrate and xylene, carbon nanotubes with uniform density can be grown on carbon microfibers surface. Based on the results, we concluded that the pretreatment of carbon microfibers had great effect on the growth of carbon nanotubes by floating catalyst method.     

Modification of polystyrene-based activated carbon spheres to improve adsorption of dibenzothiophene

Polystyrene-based activated carbon spheres (PACS) were modified with either air, HNO₃, (NH₄)₂S₂O₈, H₂O₂ or H₂ to improve their adsorption properties of dibenzothiophene (DBT). The texture and surface chemistry of PACS were characterized by N₂ adsorption, scanning electron microscopy (SEM), temperature-programmed desorption (TPD), X-ray photoelectron spectroscopy (XPS), acid-base titration and elemental analysis. The results showed that HNO₃ and (NH₄)₂S₂O₈ treatments introduced large amount of acidic groups such as carboxylic, lactones and anhydride groups, while air and H₂O₂ had relatively mild effects and introduced a small quantity of phenol, carbonyl and ether groups. In the HNO₃ treatment, the acidic groups might be fixed on the internal and external surface of PACS, which may act as active sites of adsorption, resulting in increase of the adsorption amount by 45%. Whereas H₂O₂ and (NH₄)₂S₂O₈ treatments might fix more oxygen-containing groups on the external surface, which may hinder DBT molecule enter into micropores, leading to rather lower adsorption capacity with the extent of oxidation. So, the concentration, distribution and types of the acidic functional groups are responsible for the removal of DBT.     

Atomic and molecular fluorescence as a stratospheric species monitor

The results of an extensive evaluation are presented assessing the potential of atomic and molecular fluorescence as a stratospheric monitor of the concentrations of any one of eighteen minor species. These include Cl, Cl₂, ClO, ClO₂, CO, H₂, HCHO, HCl, HNO₂, HNO₃, H₂S, NH₃, NO, NO₂, N₂O, O, OH and SO₂. All spectral regions from the vacuum u.v. through to the i.r. have been included. Where appropriate, detection limits (signal/noise ratio of unity) are presented for each species under various sample pressure conditions and are based on practical systems that could be constructed using current technology.The most promising systems, with typical detection limits indicated either as parts per million, billion or trillion by volume, are for CO(5ppb), NO₂(<1ppb), OH(0.2ppt) and O(50–200ppt). The fluorescence sensitivities for Cl(0.5–1 ppt), H₂(0.2 ppm at 10 torr sample pressure) and SO₂(1–10 ppb) are marginally insufficient at present for such a stratospheric application. Likewise HCHO(10 ppb) and NO(100 ppb) fluorescence detection may be of interest in other applications where sensitivity demands are not as severe. There are no promising analytical possibilities using direct fluorescence techniques for Cl₂, ClO₂, HCl, HNO₂, HNO₃, H₂S, NH₃ or N₂O. ClO fluorescence has not yet been characterized.It has been noted, for various reasons, that i.r. fluorescence techniques in general cannot be exploited in the development of sensitive analyzers. However, by far the most surprising outcome of this study has been the recognition of the analytical potential of vacuum u.v. fluorescence. For some species, under certain conditions, extremely high sensitivities are possible even with samples in air at atmospheric pressure.     

Capacitance and H2SO4 adsorption in the pores of activated carbon fibers

H₂SO₄ adsorption was studied by solid-state ²H-NMRand temperature-programmed desorption (TPD) on a series of pitch-based activated carbon fibers (ACFs), and compared to their electric double-layer capacitance in H₂SO₄ and Et₄NBF₄. Three states of H₂SO₄ were found by magic angle spinning (MAS)²H-NMR, namely species adsorbed on the walls, trapped in the pores, and staying over the outer surface of the ACFs, respectively. Protons of H₂SO₄ are strongly fixed on the walls of small pores whereas in the larger pores they are rather mobile due to exchange. The adsorbed protons on the pore walls contribute to the capacitance while their exchange with the protons of H₂SO₄ in the pores appears to decrease their contribution to the capacitance. The capacitance of ACFs with smaller surface area is correlated to the amount of SO₂ desorbed by TPD up to 200 °C. By contrast, for other ACFs of larger surface area the amount up to the same temperature was found to be much larger than their capacitance. The contribution of H₂SO₄ adsorbed in the latter ACFs is much less effective for their capacitance.     

n-GaAs表面全息光栅的形成及表面等离振子电磁耦子发光测定

本文讨论n-GaAs表面采用H₂O₂-H₂SO₄系光加速腐蚀形成衍射光栅的方法,以及Ag/n-GaAs肖脱基势垒二极管表面等离振子电磁耦子发光的测定。 关键词：