Synthesis and characterization of ternary AL-C-N compound

Efficient hydrogenated diamond-like carbon (DLC) film deposition in a plasma reactor that features both the capacitive and inductively coupled operation regimes is reported. The hydrogenated DLC films have been prepared on silicon wafers using a low-frequency (500 kHz) inductively coupled plasma (LF ICP) chemical vapor deposition (CVD) system. At low RF powers, the system operates as an asymmetric capacitively coupled plasma source, and the film deposition process is undertaken in the electrostatic (E) discharge regime. The films deposited in the electrostatic mode feature graphite-like structure. Above the mode transition threshold, the high-density inductively coupled plasma is produced in the electromagnetic (H) discharge regime. Raman spectrometry suggests the possibility to control relative proportions of sp2 and sp3 hybridized carbon. Variation of the DC substrate bias results in dramatic modification of the film structure from the polymeric (unbiased substrates) to the diamond-like (optimized bias). It has been shown that the deposition rate and hardness of the DLC film are much higher in the H-mode deposition regime. For a 20 m Torr H-mode CH4+Ar gas mixture discharge, the DLC film exhibits mechanical hardness of 18 GPa, Young's modulus of 170 GPa, and compressive stress of 1.3 GPa.

Preparation, characterization of surfactants modified clay minerals and nitrate adsorption

Organic surfactants modified clay minerals are usually used as adsorbents for hydrophobic organic contaminants remediation; this work however has shown organoclays can also work as adsorbents for hydrophilic anionic contaminant immobilization. Organoclays were prepared based on halloysite, kaolinite and bentonite and used for nitrate adsorption, which are significant for providing mechanism for the adsorption of anionic contaminants from waste water. XRD was used to characterize unmodified and surfactants modified clay minerals. Thermogravimetric analysis (TG) was used to determine the thermal stability and actual loading of surfactant molecules. Ion chromatography (IC) was used to determine changes of nitrate concentration before and after adsorption by these organoclays. These organoclays showed different removal capacities for anionic ions from water and adsorption mechanism was investigated.

Photophysical characterization of light-emitting poly(indenofluorene)s

Time-resolved photoluminescence spectroscopy experiments of three poly(2,8-indenofluorene) derivatives bearing different pendant groups are presented. A comparison of the photophysical properties of dilute solutions and thin films provides information on the chemical purity of the materials. The photophysical properties of poly(2,8-indenofluorene)s are correlated with the morphological characteristics of their corresponding films. Wide-angle X-ray scattering experiments reveal the order in these materials at the molecular level. The spectroscopic results confirm the positive impact of a new synthetic approach on the spectral purity of the poly(indenofluorene)s. It is concluded that complete side-chain substitution of the bridgehead carbon atoms C-6 and C-12 in the indenofluorene unit, prior to indenofluorene ring formation, reduces the probability of keto formation. Due to the intrinsic chemical purity of the arylated derivative, identification of a long-delayed spectral feature, other than the known keto band, is possible in the case of thin films. Controlled doping experiments on the arylated derivative with trace amounts of an indenofluorene-monoketone provide quantitative information on the rates of two major photophysical processes, namely, singlet photoluminescence emission and singlet photoluminescence quenching. These results allow the determination of the minimum keto concentration that can affect the intrinsic photophysical properties of this polymer. The data suggest that photoluminescence quenching operates in the doped films according to the Stern-Volmer formalism.

Synthesis, characterization and organic field effect transistor performance of a diketopyrrolopyrrole-fluorenone copolymer

A diketopyrrolopyrrole (DPP) with fluorenone (FN) based low band gap alternating copolymer (PDPPT-alt-FN) has been synthesized via Suzuki coupling. PDPPT-alt-FN exhibits a deep HOMO level with a lower band gap. Fabricated organic thin film transistors using PDPPT-alt-FN as a channel semiconductor show p-channel behaviour with the highest hole mobility of 0.083 cm2 V-1 s-1 measured in air.

Sol-gel synthesis and characterization of cubic bismuth zinc niobium oxide nanopowders

Bismuth zinc niobium oxide (BZN) was successfully synthesized by a diol-based sol-gel reaction utilizing metal acetate and alkoxide precursors. Thermal analysis of a liquid suspension of precursors suggests that the majority of organic precursors decompose at temperatures up to 150°C, and organic free powders form above 350°C. The experimental results indicate that a homogeneous gel is obtained at about 200°C and then converts to a mixture of intermediate oxides at 350–400°C. Finally, single-phased BZN powders are obtained between 500 and 900°C. The degree of chemical homogeneity as determined by X-ray diffraction and EDS mapping is consistent throughout the samples. Elemental analysis indicates that the atomic ratio of metals closely matches a Bi1.5ZnNb1.5O7 composition. Crystallite sizes of the BZN powders calculated from the Scherrer equation are about 33–98 nm for the samples prepared at 500–700°C, respectively. The particle and crystallite sizes increase with increased sintering temperature. The estimated band gap of the BZN nanopowders from optical analysis is about 2.60–2.75 eV at 500-600°C. The observed phase formations and measured results in this study were compared with those of previous reports.

Pyrene based conjugated materials: synthesis, characterization and electroluminescent properties

In this work, three novel pyrene cored small conjugated molecules, namely 1,3,6,8-tetrakis(6-(octyloxy)naphthalene-2-yl)pyrene (PY-1), 1,3,6,8-tetrakis((E)-2-(6-(n-octyloxy)naphthalene-2-yl)vinyl)pyrene (PY-2) and 1,3,6,8-tetrakis((6-(n-octyloxy)naphthalene-2-yl)ethynyl)pyrene (PY-3) have been synthesized by Suzuki, heck and Sonogashira organometallic coupling reactions, respectively. The effects of single, double and triple bonds on their optical, electrochemical, and thermal properties are studied in detail. These are all materials fluorescent and they have been used in organic light-emitting diodes (OLEDs) and their electroluminescent properties have been studied.

Optical Characterization of the Hole Polaron in a Series of Diketopyrrolopyrrole Polymers Used for Organic Photovoltaics

Abstract: A strategy that is often used for designing low band gap polymers involves the incorporation of electron-rich (donor) and electron-deficient (acceptor) conjugated segments within the polymer backbone. In this paper we investigate such a series of Diketopyrrolopyrrole (DPP)-based co-polymers. The co-polymers consisted of a DPP unit attached to a phenylene, naphthalene, or anthracene unit. Additionally, polymers utilizing either the thiophene-flanked DPP or the furan-flanked DPP units paired with the naphthalene comonomer were compared. As these polymers have been used as donor materials and subsequent hole transporting materials in organic solar cells, we are specifically interested in characterizing the optical absorption of the hole polaron of these DPP based copolymers. We employ chemical doping, electrochemical doping, and photoinduced absorption (PIA) studies to probe the hole polaron absorption spectra. While some donor-acceptor polymers have shown an appreciable capacity to generate free charge carriers upon photoexcitation, no polaron signal was observed in the PIA spectrum of the polymers in this study. The relations between molecular structure and optical properties are discussed. Keywords: organic solar cell; organic photovoltaic; diketopyrrolopyrrole; chemical doping; spectroelectrochemistry; photoinduced absorption; hole polaron

Characterization of the sulphate mineral coquimbite, a secondary iron sulphate from Javier Ortega mine, Lucanas Province, Peru – Using infrared, Raman spectroscopy and thermogravimetry

The mineral coquimbite has been analysed using a range of techniques including SEM with EDX, thermal analytical techniques and Raman and infrared spectroscopy. The mineral originated from the Javier Ortega mine, Lucanas Province, Peru. The chemical formula was determined as ðFe3þ 1:37; Al0:63ÞP2:00ðSO4Þ3 9H2O. Thermal analysis showed a total mass loss of 73.4% on heating to 1000 C. A mass loss of 30.43% at 641.4 C is attributed to the loss of SO3. Observed Raman and infrared bands were assigned to the stretching and bending vibrations of sulphate tetrahedra, aluminium oxide/hydroxide octahedra, water molecules and hydroxyl ions. The Raman spectrum shows well resolved bands at 2994, 3176, 3327, 3422 and 3580 cm 1 attributed to water stretching vibrations. Vibrational spectroscopy combined with thermal analysis provides insight into the structure of coquimbite.

Structural characterization of the borate mineral inyoite – CaB3O3(OH)5⋅4(H2O)

We have studied the mineral Ca(H4B3O7)(OH)⋅4(H2O) or CaB3O3(OH)5⋅4(H2O) using electron microscopy and vibrational spectroscopy. The mineral has been characterized by a range of techniques including X-ray diffraction, thermal analysis, electron microscopy with EDX and vibrational spectroscopy. Electron microscopy shows a pure phase and the chemical analysis shows the presence of calcium only. The nominal resolution of the Raman spectrometer is of the order of 2 cm−1 and as such is sufficient enough to identify separate bands for the stretching bands of the two boron isotopes. Raman and infrared bands are assigned to the stretching and bending modes of trigonal and tetrahedral boron and the stretching modes of the hydroxyl and water units. By using a combination of techniques we have characterized the borate mineral inyoite.

SEM, EDX, infrared and Raman spectroscopic characterization of the silicate mineral yuksporite

The mineral yuksporite (K,Ba)NaCa2(Si,Ti)4O11(F,OH)⋅H2O has been studied using the combination of SEM with EDX and vibrational spectroscopic techniques of Raman and infrared spectroscopy. Scanning electron microscopy shows a single pure phase with cleavage fragment up to 1.0 mm. Chemical analysis gave Si, Al, K, Na and Ti as the as major elements with small amounts of Mn, Ca, Fe and REE. Raman bands are observed at 808, 871, 930, 954, 980 and 1087 cm−1 and are typical bands for a natural zeolite. Intense Raman bands are observed at 514, 643 and 668 cm−1. A very sharp band is observed at 3668 cm−1 and is attributed to the OH stretching vibration of OH units associated with Si and Ti. Raman bands resolved at 3298, 3460, 3562 and 3628 cm−1 are assigned to water stretching vibrations.

Initial design and physical characterization of a polymeric device for osmosis-driven delayed burst delivery of vaccines

Achieving the combination of delayed and immediate release of a vaccine from a delivery device without applying external triggers remains elusive in implementing single administration vaccination strategies. Here a means of vaccine delivery is presented, which exploits osmosis to trigger delayed burst release of an active compound. Poly(-caprolactone) capsules of 2 mm diameter were prepared by dip-coating, and their burst pressure and release characteristics were evaluated. Burst pressures (in bar) increased with wall thickness (t in mm) following Pburst = 131.t + 3.4 (R2 = 0.93). Upon immersion in PBS, glucose solution-filled capsules burst after 8.7 ± 2.9 days. Copolymers of hydrophobic  -caprolactone and hydrophilic polyethylene glycol were synthesized and their physico-chemical properties were assessed. With increasing hydrophilic content, the copolymer capsules showed increased water uptake rates and maximum weight increase, while the burst release was earlier: 5.6 ± 2.0 days and 1.9 ± 0.2 days for 5 and 10 wt% polyethylene glycol, respectively. The presented approach enables the reproducible preparation of capsules with high versatility in materials and properties, while these vaccine delivery vehicles can be prepared separately from, and independently of the active compound.

Raman and infrared spectroscopic characterization of the silicate mineral lamprophyllite

The mineral lamprophyllite is fundamentally a silicate based upon tetrahedral siloxane units with extensive substitution in the formula. Lamprophyllite is a complex group of sorosilicates with general chemical formula given as A2B4C2Si2O7(X)4, where the site A can be occupied by strontium, barium, sodium, and potassium; the B site is occupied by sodium, titanium, iron, manganese, magnesium, and calcium. The site C is mainly occupied by titanium or ferric iron and X includes the anions fluoride, hydroxyl, and oxide. Chemical composition shows a homogeneous phase, composed of Si, Na, Ti, and Fe. This complexity of formula is reflected in the complexity of both the Raman and infrared spectra. The Raman spectrum is characterized by intense bands at 918 and 940 cm−1. Other intense Raman bands are found at 576, 671, and 707 cm−1. These bands are assigned to the stretching and bending modes of the tetrahedral siloxane units.

Synthesis, characterization, and electronic structure studies of cubic Bi1.5ZnTa1.5O7 for photocatalytic applications

Bi1.5ZnTa1.5O7 (BZT) has been synthesized using an alkoxide based sol-gel reaction route. The evolution of the phases produced from the alkoxide precursors and their properties have been characterized as function of temperature using a combination of thermogravimetric analysis (TGA) coupled with mass spectrometry (MS), infrared emission spectrometry (IES), X-ray diffraction (XRD), ultraviolet and visible (UV-Vis) spectroscopy, Raman spectroscopy, and N2 adsorption/desorption isotherms. The lowest sintering temperature (600∘C) to obtain phase pure BZT powders with high surface area (14.5m2/g) has been determined from the thermal decomposition and phase analyses.The photocatalytic activity of the BZT powders has been tested for the decolorization of organic azo-dye and found to be photoactive under UV irradiation.The electronic band structure of the BZT has been investigated using density functional theory (DFT) calculations to determine the band gap energy (3.12 eV) and to compare it with experimental band gap (3.02 eV at 800∘C) from optical absorptionmeasurements. An excellent match is obtained for an assumption of Zn cation substitutions at specifically ordered sites in the BZT structure.