Synthesis and Characterization of Novel AB and ABA Rod–Coil Block Copolymers

Two series of novel rod–coil block copolymers, poly(ɛ-caprolactone)-b-poly{2,5-bis[(4-methoxyphenyl) oxycarbonyl] styrene} (PCL-b-PMPCS) and poly{2,5-bis[(4-methoxyphenyl) oxycarbonyl] styrene}-b-poly(ɛ-caprolactone)-b-poly{2,5-bis[(4-methoxyphenyl) oxycarbonyl] styrene} (PMPCS-b-PCL-b-PMPCS), were successfully synthesized via atom transfer radical polymerization in chlorobenzene solution using macro-initiator and CuBr/Sparteine complex as catalyst. The results show that the number average molecular weight M_n increased versus the monomer conversion and that the polydispersity M_w/M_n was quite narrow (<1.35), which were the character of controlled polymerization. The structure of the block copolymers was experimentally confirmed by ¹H NMR. And the liquid crystalline behavior of them was studied using DSC and POM. The data obtained implied that the block copolymers with low molar percentage of PMPCS block could show T_m of PCL. While only the copolymers with long rigid segment PMPCS could form liquid crystalline phase, which was quite stable with a high clearing point.     

Electroluminescent Characteristics of DBPPV–ZnO Nanocomposite Polymer Light Emitting Devices

We have demonstrated that fabrication and characterization of nanocomposite polymer light emitting devices with metal Zinc Oxide (ZnO) nanoparticles and 2,3-dibutoxy-1,4-poly(phenylenevinylene) (DBPPV). The current and luminance characteristics of devices with ZnO nanoparticles are much better than those of device with pure DBPPV. Optimized maximum luminance efficiencies of DBPPV–ZnO (3:1 wt%) before annealing (1.78 cd/A) and after annealing (2.45 cd/A) having a brightness 643 and 776 cd/m² at a current density of 36.16 and 31.67 mA/cm² are observed, respectively. Current density–voltage and brightness–voltage characteristics indicate that addition of ZnO nanoparticles can facilitate electrical injection and charge transport. The thermal annealing is thought to result in the formation of an interfacial layer between emissive polymer film and cathode.     

Synthesis and Characterization of Linear and Tri-Block PLLA–PEG–PLLA Blends

This study was conducted to synthesize poly(L-lactide)–poly(ethylene glycol)–poly(L-lactide) triblock copolymer (PEGLA) with different poly(L-lactide) block length, and explore its applicability in a blend with linear poly(L-lactide) (3051D NatureWorks) with the intention of improving heat seal and adhesion properties at extrusion coating on paperboard. Poly(L-lactide)–poly(ethylene glycol)–poly(L-lactide) was obtained by ring opening polymerization of L-lactide using poly(ethylene glycol) (molecular weight 6000 g mol^?1) as an initiator and stannous octoate as catalyst. The structures of the PEGLAs were characterized by proton nuclear magnetic resonance spectroscopy. The melt flow and thermal properties of all PEGLAs and their blends were evaluated using dynamic rheology and differential scanning calorimeter. All blends containing 10 wt% of PEGLAs displayed similar zero shear viscosities to neat poly(L-lactide), while blends containing 30 wt% of PEGLAs showed slightly higher zero shear viscosity. However, all blends displayed higher shear thinning and increased melt elasticity (based on tan δ). No major changes in thermal properties were distinguished from differential scanning calorimetric studies. High molecular weight PEGLAs could be used in extrusion coating with 3051D without problems.     

Green Synthesis,Structural Characterization and Photocatalytic Activities of Chitosan-ZnO Nano‐composite

Journal of Inorganic and Organometallic Polymers and Materials - Chitosan was isolated from chitin, a direct derivative of snail shell, and further used to form a heterostructure with ZnO...     

Synthesis and Characterization of ZnO Nanowire–CdO Composite Nanostructures

ZnO nanowire–CdO composite nanostructures were fabricated by a simple two-step process involving ammonia solution method and thermal evaporation. First, ZnO nanowires (NWs) were grown on Si substrate by aqueous ammonia solution method and then CdO was deposited on these ZnO NWs by thermal evaporation of cadmium chloride powder. The surface morphology and structure of the synthesized composite structures were analyzed by scanning electron microscopy, X-ray diffraction and transmission electron microscopy. The optical absorbance spectrum showed that ZnO NW–CdO composites can absorb light up to 550 nm. The photoluminescence spectrum of the composite structure does not show any CdO-related emission peak and also there was no band gap modification of ZnO due to CdO. The photocurrent measurements showed that ZnO NW–CdO composite structures have better photocurrent when compared with the bare ZnO NWs.     

Synthesis and Characterization of Copper(II)–Cysteine/SiO2–Al2O3 as an Efficient and Reusable Heterogeneous Catalyst for the Oxidation of Aromatic Alcohols

In the present study, heterogeneous copper(II)–cysteine/SiO₂–Al₂O₃ catalyst was successfully prepared by a simple adsorption method. The physical and chemical properties of Cu(II)–cysteine/SiO₂–Al₂O₃ were investigated by X-ray diffraction, thermal gravimetric analyzer, FT–IR spectroscopy, Brunauer–Emmett–Teller, UV–Vis spectroscopy, scanning electron microscopy and atomic absorption spectrometer. The obtained composite was effectively employed as catalyst for selective oxidation of various aromatic alcohols to corresponding aldehydes in high yields using hydrogen peroxide as an oxidant under mild condition. The catalyst can be recycled over five times without significant loss of activity.     

Synthesis and Characterization of FePt/NiO Core–Shell Nanoparticles

Monodisperse FePt nanoparticles were successfully synthesized using the chemical polyol process. Annealing at the high temperatures is required to achieve the hard ferromagnetic behavior with L1₀ phase. Annealing causes the surfactant surrounding particles to be decomposed. Under such circumstances, FePt particles are agglomerated, and their size increases. In this research, NiO oxide particle with a high melting point was used for the first time as the shell around FePt core particles to prevent agglomeration. As a result, coercivity, H_c, of FePt and FePt/NiO nanoparticles after annealing at 750?°C are equal to 10 and 7?kOe, respectively.     

Synthesis and Characterization of AgBr–Silk Nanocomposite Under Ultrasound Irradiation

The growth of silver bromide nanoparticles on silk yarn was achieved by sequential dipping in alternating bath of potassium bromide and silver nitrate under ultrasound irradiation. The effect of concentration, power of ultrasound irradiation and the numerous of sequential dipping steps in growth of the AgBr nanoparticles on silk yarn were studied. The samples were characterized with powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and Inductive Coupled Plasma (ICP). The lower average size and the higher crowded AgBr nanoparticles upon silk yarn are the result of using ultrasound irradiation.     

Synthesis and Characterization of Nanoscale Mullite Powder

Nanoscale mullite powder were synthesized via solgel-SCFD and middle temperature treatment by using AIP (aluminum-isopropoxde)and TEOS(tetraethyl orthosilicate) as starting materials.Both of the binary aerogel of alumina-silica and calcined nanoscale materials were investigated by using TG-DSC(thermogravimetry-differential scanning calorimeter),TEM(transmission electron microscope),XRD(X-Ray diffractometer)and specific surface area and porosimetry.TG-DSC indicated the removal of most of the volatiles,i.e.15.98% up to about 700℃,and in the DSC curve,existence of two exothermic peak at about 445℃ and 1015℃ may be due to the crystallization of Si-O-Al-O in diphasic gels and mullitization and a small endothermic peak at about 805℃ indicated the decomposition of structural water molecules.On the colligation of the results of TG-DSC,XRD and TEM,the beginning temperature of mullitization in Al2O3-SiO2 aerogel system can be confirmed at about 1015℃.XRD results also showed the formation of mullite at the range 1100-1200℃.TEM and surface area and porosimetry results showed that the nanosized mullite were calcinated at 1100 and 1200℃ exhibited size 30nm and 50nm,specific surface area 138.91m^2/g and 95.81m^2/g.     

Polyaniline Coating on Iron–Synthesis and Characterization

Protective coating has been used widely for metal corrosion control. Polyaniline (PANi) films can be electrosynthesized by oxidation of aniline on a metal surface from an aqueous acid medium. In this study, an iron surface was coated by polyaniline thin film. While iron easily oxidizes in acid solutions, the electropolymerization reactions were carried out in dilute acidic media. Rust, fats, etc. on the surface of iron were removed by alkali-ethanol solution, dichloroethylene, and, finally, hydrochloride (HCl) solution (10%), respectively. Coating was carried out in different potential (1.0, 1.5, and 2.5 V). To observe the effect of elemental contents of iron samples, spectral analysis also was taken before electropolymerization. Especially, effects of chromium and nickel elements were investigated. Physical resistance of the coating was examined by “band test.” Dissolving and defective coatings were also tested in acidic solutions and common organic solvents. In addition, to observe the morphology of coating, photos of samples were taken by scanning electron microscope (SEM) and metal microscope (MM).     

Synthesis and Characterization of Metal Nanoparticle Embedded Conducting Polymer–Polyoxometalate Composites

Phosphomolybdate has been employed simultaneously as the oxidizing agent for the monomer polymerization and the reduced polyoxometalate is used as reducing agent for the reduction of metal ions. The composites thus obtained have been characterized and may have many potential applications.     

Synthesis and Characterization of Silica–Polymer Nanocomposites Functionalized with Piperazine for the Synthesis of β-Nitro Alcohols

Abstract  

In order to compare the activity and selectivity for the synthesis of β-nitro alcohols, piperazine was functionalized directly and after surface modification into the ordered mesoporous SBA-15 framework. The materials were characterized by powder X-ray diffraction, N₂-adsorption–desorption isotherm, FT-IR, SS-NMR and scanning electron microscopy. The catalyst synthesized via surface modification under solvent free conditions showed very high activity and selectivity of β-nitro alcohols compared to the one synthesized by direct functionalization of SBA-15. Finally the possible reaction pathways were explained mechanistically.     

Synthesis and Characterization of Polyindole–NiO-Based Composite Polymer Electrolyte with LiClO4

There has been an increasing interest in synthesizing the novel composite polymer electrolyte (CPE) for use in lithium batteries in recent years. This paper describes the preparation and characterization of CPE containing lithium perchlorate based on polyindole–NiO nanocomposite. NiO nanoparticles were added to the monomer solution before the polymer formation in the presence of a surfactant to get the PInNiO nanocomposite. The thermal properties, surface morphology, and structural studies of the electrolyte were investigated by TGA, SEM, TEM, and XRD. An enhanced conductivity of 2.62 × 10^?4 S cm^?1 at 45°C for the composite polymer electrolyte was determined from impedance studies.     

Synthesis, Characterization and HDS Activity of Carbon-Containing Ni–Mo Sulfide Nano-Spheres

Ni-promoted tetramethylammonium tetrathiomolybdate precursor was prepared by the aqueous solution precipitation method using (NH₄)₂MoS₄, (CH₃)₄NBr and NiCl₂.6H₂O as raw materials. Carbon-containing Ni–Mo sulfide nanospheres, namely Ni/C₁–MoS₂, were obtained by ex situ thermal decomposition of the precursor under N₂ atmosphere. Energy dispersive X-ray spectroscopy (EDS), low temperature N₂ adsorption (BET method), X-ray diffraction (XRD), scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM) techniques were employed to characterize these as–synthesized sulfide particles. The results showed that the average size of solid Ni–Mo sulfide nanospheres, with surface composition MoNi₀.₄₀S₀.₇₃C₁.₄₃, is 75 nm and the solid structure leads to low surface area of Ni/C₁–MoS₂. In addition, the introduction of methyl chain improved the dispersion of nickel phases and resulted in C/Mo ratio, 1.4. By comparison with catalytic performance of the Ni/MoS₂ catalyst counterpart, Ni/C₁–MoS₂ revealed lower HDS activity but higher direct desulfurization (DDS) selectivity. Lower stacking number of MoS₂ slabs (5 layers) and shorter slabs length of MoS₂ slabs (6 nm) explained higher DDS selectivity satisfactorily. The formation of carbon-containing Ni–Mo sulfide nanospheres was possibly due to surfactant effect of tetramethylammonium cations and the potential measure to increase their surface area was discussed as well in this work.     

Synthesis and Characterization of Hybrid Core–Shell Systems Based on Molecular Silicasols

New hybrid “rigid inorganic core–soft organic shell” systems based on molecular silicasols were synthesized by applying different synthetic schemes. Inorganic core was composed of molecular silicasols, which were synthesized from hyperbranched polyethoxysiloxane and tetraethoxysilane by polymer chemistry methods. Different organic modifiers were used to form soft shell of the hybrid particles. Obtained compounds were characterized by elemental analysis, GPC, IR and NMR spectroscopy. These systems will be designated for use as model objects for investigation of nanoparticles–polymer matrix interactions in polymer nanocomposites.     

Synthesis and Characterization of Some Poly(1,2-Phenylenedithiocarbamate)–Metal Complexes

Poly(1,2-phenylenedithiocarbamate) (PPDTC) was prepared by the reaction of 2-aminothiophenol with carbon disulfide followed by condensation through the removal of H₂S gas. PPDTC was used as a ligand to prepare four poly(1,2-phenylenedithiocarbamate)–metal complexes of iron(II), cobalt(II), copper(II), and lead(II), by refluxing with the metal salts. The polymer and its metal complexes were investigated by elemental analyses, UV–visible and IR spectroscopy, inherent viscosity, and magnetic susceptibility. The DC electrical conductivity variation with the temperature in the range 298–498 K of PPDTC and its polymeric copper complex was measured. Both polymer and polymer metal complexes showed an increase in electrical conductivity with an increase in temperature: typical semiconductor behavior. The proposed structure of the complexes is (MLX₂·mH₂O) _n .     

Synthesis and Characterization of the Inclusion Complex of β-cyclodextrin and Azomethine

A β-cyclodextrin (β-Cyd) inclusion complex containing azomethine as a guest was prepared by kneading method with aliquot addition of ethanol. The product was characterized by Fourier Transform Infrared (FTIR) spectrometer, ¹H Nuclear Magnetic Resonance (¹H NMR) and Thermogravimetric Analyzer (TGA), which proves the formation of the inclusion complex where the benzyl part of azomethine has been encapsulated by the hydrophobic cavity of β-Cyd. The interaction of β-Cyd and azomethine was also analyzed by means of spectrometry by UV-Vis spectrophotometer to determine the formation constant. The formation constant was calculated by using a modified Benesi-Hildebrand equation at 25 °C. The apparent formation constant obtained was 1.29 × 10⁴ L/mol. Besides that, the stoichiometry ratio was also determined to be 1:1 for the inclusion complex of β-Cyd with azomethine.     

Synthesis and Self-Assembly of β-Cyclodextrin Terminated DMA/NIPAM Diblock Copolymers

A series of β-cyclodextrin (β-CD) terminated diblock copolymers has been prepared via click reaction. The Huisgen cycloaddition between alkyne decorated copolymer and azide functionalized β-CD was performed in organic solvent in the presence of a Cu(I) catalyst, resulting in the formation of β-CD terminated diblock copolymers, which contain thermally responsive poly(N-isopropylacrylamide) (PNIPAM) block and hydrophilic poly(N,N-dimethylacrylamide) (PDMA) block. Using dynamic light scattering and fluorescence spectroscopy measurements, it is demonstrated that these β-CD functionalized block copolymers are capable of reversibly forming micelles in response to changes in solution temperature and that the critical micelle concentration, micellar size, and transition temperature are dependent on both the NIPAM block length and the polymer functionalization.