A simple method to prepare solid nanoparticles of water-soluble salts using water-in-oil microemulsions

 A new and simple method to prepare solid nanoparticles of water-soluble salts using water-in-oil microemulsions is described. In particular, starting from water/sodium bis(2-ethylhexyl)sulfosuccinate/n-heptane microemulsions carrying inside the aqueous core of the reversed micelles some water-soluble salts [CaCl₂, Na₂HPO₄, Cu(NO₃)₂], after evaporation of the volatile components (water and apolar organic solvent), the resulting inorganic salt/surfactant composites were found to be totally dispersible in pure n-heptane. The presence of nanoparticles in these resuspended composites was ascertained by transmission electron microscopy observation of samples obtained by gentle evaporation of the organic solvent. Received: 8 July 1999/Accepted in revised form: 5 October 1999     

A novel method to prepare metal oxide electrode:Spin-coating with thermal decomposition

In this work,we propose a new spin-coating method coupling with high thermal decomposition,to prepare the tin-antimony(Sn-Sb) oxide electrode.The character of the spin-coating electrode was compared with the dip-coating electrode through X-ray diffraction(XRD),scanning electron microscopy(SEM),accelerated life test,cyclic voltammetry,and electrolytic degradability. The results showed that the spin-coating electrode had a better defined crystal form,a smoother and more compact surface than that of the dip-coating electrode.Service time of the spin-coating electrode was determined to be longer than 15 h,and it was less than 2 min for the dip-coating electrode.Electrochemical characterization analysis showed that the electrolytic degradability of the spin-coating electrode is better than that of the dip-coating electrode.     

A pre-organized monomer-reservoir strategy to prepare multidimensional phosphorescent organoplatinum nanocrystals and suprastructures

The preparation of multidimensional nano-and microstructures,in particular suprastructures with well-defined morphology and bright emissions,is a challenging task in supramolecular assembly.For this purpose,a new type of amphiphilic diplatinum complexes is presented as an excellent building block to assemble into highly phosphorescent nanofibers by supramolecular Pt…Pt interactions.These organoplatinum supramolecular fibers are further used as a pre-organized monomer reservior for the metal ion-triggered post-transformation into crystalline nanoneedles,nanorods,nanobunches,microplates,and microflowers with controllable morphology and bright phosphorescence.A reverse transformation of the obtained nanorods into nanofibers is demonstrated with the aid of ethylenediamine tetraacetic acid.In contrast,the direct treatment of diplatinum complexes with different metal ions fails to give well-defined nano and microstructures,suggestive of the pre-organized role of nanofibers for the morphological transformation.Preliminary applications of these nano-and suprastructures in sensing temperature and organic vapours by emission signal changes are demonstrated.In contrast to the conventional hierarchical assembly,the pre-organized monomer-reservoir strategy disclosed in this study offers a versatile method for the synthesis of organic nano and suprastructures with multidimensional morphology and controllable emission properties.     

A powerful method to prepare sulfur-rich macrocycles

Various cyclic polysulfanes (up to a 16-membered ring) have been selectively obtained from the corresponding disubstituted trityl-protected polysulfane benzene derivatives upon treatment with elemental iodine in the presence of silica gel. Depending on the position of the sulfur-rich moieties and the presence of a methylene linker between the benzene ring and sulfur atoms, two types of products containing either one or two benzene subunits have been isolated. The scope of the reaction, its selectivity, and mechanism are discussed.     

A novel method to prepare SPR sensor chips based on photografting molecularly imprinted polymer

A novel method to prepare surface plasmon resonance(SPR) sensor chips based on grafted imprinted polymer is explored. Benzophenone photografting system is used to grow molecularly imprinted polymer(MIP) films from the modified surface of gold substrate.The surface morphology and thickness of MIP films were investigated by scanning electronic microscope(SEM).The adsorption properties of sensor chip were studied by SPR spectroscopy.The results demonstrate that nano-MIP films can be constructed on the surface of gold substrate with the good adsorption of template molecules.     

A novel, mild, and facile method to prepare 6-methylidene penem derivatives

A novel and mild method was established to synthesize 6-methylidene penem compounds. This method entails a MgBr(2)/Et(3)N-promoted aldol-type condensation on 6-bromopenem 12 with an appropriately substituted aldehyde to yield the intermediate acetylated bromohydrin, which was smoothly converted to the final product with simultaneous deprotection of C3 carboxylic acid ester using activated zinc dust and phosphate buffer at pH 6.5. This process provides a useful variation of C-C bond formation method for penem derivatives and also serves as a practical synthetic method to prepare 6-exomethylenepenem derivatives without racemization at the C5 position.     

A novel method to prepare microporous and nanofibrous hydrogel scaffolds as neural tissue engineering

A new method to prepare poly (vinyl alcohol) hydrogels by nebulization method.is introduced. A blend of Poly (vinyl alcohol) (PVA), sodium gum malate (SGM) and cellulose nanofibers (CNFs) originated from Catha Edulis was prepared and tested as neural tissue substitutes. Glutaraldehyde (GLA) was used as a crosslinker. Presence of SGM and CNFs in the formulation improved the nebulization process of PVA solution as well as mechanical properties of the fabricated hydrogels. The tensile strength of neat PVA films attains 46.7 MPa, while the tensile strength was 94.23 MPa for crosslinked-PVA. The tensile strength was found to increase with the increase in the CNFs content in the PVA compared with PVA/SGM. These soft tissues were characterized by using FTIR, SEM, and DSC. Scanning electron microscopy (SEM) results showed that PVA/SGM/CNFs blends has a diameter about 50 ± 8µm. The hydrogels were tested also for antimicrobial activities against pathogenic bacteria like Candida albicans (fungus), Bacillus subtilis (G + Ve), Staphylococcus aureus (G + Ve), Proteus vulgaris (G ? Ve) and Erwinia carotovora (G ? Ve). Favorable mechanical, thermal properties and biodegradation nature of the hydrogels, as well as antimicrobial property indicate that prepared hydrogels are suitable for tissue engineering applications.     

A simple way to prepare PbS nanocrystals with morphology tuning at room temperature

A simple way to synthesize PbS nanocrystals with the ability to tune their morphology at room temperature is reported. The preparation utilizes an amine-catalyzed decomposition of a precursor and the amine was found to play dual roles as both the catalyst and the capping agent. Spherical PbS nanocrystals of diameters 5 to 10 nm were obtained when long chain alkylamines were used in the pot. When difunctional ethylenediamine was used instead, exclusively PbS dendrites can be isolated from the same precursor at room temperature. Uniform six- and four-armed dendrites are observed, with regular branches of approximately 20 nm in diameter growing in a parallel order. In a further step, morphology tuning of the dendrites to induce 1D growth into nanorods is achievable through the addition of a trace amount of stronger capping dodecanethiol molecules. Thus, PbS nanorods with aspect ratios of approximately 20 to 30 could be successfully obtained and illustrated. A possible formation mechanism is discussed and the initial step of the reaction mechanism was modeled with DFT calculations as a nucleophilic attack.     

A novel method to prepare polymer-ionic liquid gel under high pressure and its electrochemical properties

Sol–gel transition behavior of ionic liquid gel based on poly (ethylene glycol) (PEG) and ionic liquid 1-ethyl-3-methylimidazolium ethylsulfate [EMIM][EtSO₄] has been investigated under the pressure up to 250 MPa. The Temperature versus Pressure phase diagram of PEG/[EMIM][EtSO₄] gel is constructed, and it indicates that the melting point is an increasing function of pressure. Based on the phase diagram, the PEG/[EMIM][EtSO₄] gels are prepared by cooling under the pressure of 300 MPa and atmospheric pressure, respectively. From the differential scanning calorimetry result of the recovered samples, it is found that PEG/[EMIM][EtSO₄] gel prepared under high pressure has a higher crystallinity and smaller crystal size polymer network, comparing with under atmospheric pressure. The cyclic voltammograms and impedance spectra tests indicate that the PEG/[EMIM][EtSO₄] gel prepared under high pressure exhibit higher ionic conductivity comparing with atmospheric pressure. It could be speculated these excellent properties might be attributed to the loose gel structure and high ionic density induced by high pressure.     

Labeled avidin bound to water-soluble nanocrystals by electrostatic interactions

Semiconducting nanocrystals of three different sizes capped with 3-mercaptopropionic acid were synthesized in aqueous solutions. They can efficiently bind to an avidin biomolecule by the electrostatic attraction. The conjugation of avidin leads to a red shift and a decrease in the intensity of the fluorescence emission spectra of the nanocrystals. Moreover, the red shift of the fluorescence spectra of the bioconjugates depends strongly on the pH, ionic strength, quantity of avidin, and nanocrystal size.__________Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 12, pp. 2579–2583, December, 2004.     

Efficient method to prepare diethylphosphonacetamides

An efficient and versatile synthetic method is described to synthesize diethylphosphonacetamides in a single step.     

A new simple method to prepare hollow PES microspheres

A new simple method for the formation of hollow polyethersulfone (PES) microspheres was reported in this paper. Coaxial electrospraying equipment and nonsolvent precipitating bath were used to produce hollow microspheres in one step. The properties of the core solution affected the formation of hollow PES microspheres. To form hollow microspheres in one step, the core solution should be removed directly by a nonsolvent. Additionally, the core solution should also be used to occupy the internal space of microspheres and form a supporting layer at the interface between the core solution and the shell solution. The supporting layer formed by the micro-phase that was caused by the phase separation of the core or shell solution was the key factor for the formation of hollow PES microspheres. The performance of hollow microspheres produced by this method was excellent. This method provided a new simple way to form hollow polymer microspheres and can be extended to other polymers to prepare hollow microspheres in one step.     

A concise method to prepare linear 2,3-diazaoligoacene derivatives

In this Letter, we demonstrate that linear 2,3-diazanaphthalene (1), 2,3-diazaanthracene (2), and 2,3-diazatetracene (3) can be easily prepared through [4+2] cycloaddition reaction between 3,6-diphenyl-1,2,4,5-tetrazine as the diene and arynes as dienophiles, generated in situ from ortho-aminoarylcarboxylic acids. The physical properties and crystal packing of the prepared compounds 1–3 were fully investigated. In addition, the experimental data (e.g., band gap and band position) are further confirmed by theoretical studies.     

Size-controlled synthesis of highly water-soluble silver nanocrystals

We describe a modified polyol process for the synthesis of silver nanocrystals with uniform sizes ranging from several nanometers to 20 nm. The use of polyacrylic acid, in place of polyvinylpyrrolidone in the conventional polyol process, significantly limits the growth of silver nanocrystals, prevents the interparticle aggregation and fusion, and leads to a uniform population of samples with high water solubility. The size of nanocrystals can be conveniently tuned by controlling the reaction time, the concentration and chain length of the polymeric surfactants, and the reaction temperature. Uniform silver nanocrystals within sizes below 20 nm are preferred candidates over larger particles for applications where high density of optical absorption is required, for example, for photothermal conversion in cancer therapy.     

A versatile method to prepare difluorinated primary alcohols and its application to the syntheses of novel acyclic fluorinated nucleosides

The addition of fluorine to a molecule often leads to intriguing changes in the properties of the molecule. Many novel drug leads and drug candidates are the results of the incorporation of fluorine. This Letter presents a versatile method to create molecules with the general structure R₁R₂CHCF₂CH₂OH from ketone R₁(CO)R₂. The key steps of this synthetic method involve the formation of a cyclic thiocarbonate and the regioselective radical opening of the thiocarbonate to yield the corresponding primary alcohol –CF₂CH₂OH. Using this synthetic method, novel fluorinated analogs of ganciclovir and penciclovir have been prepared.     

A facile synthetic method to prepare fluorescently labeled ROMP polymers

[structure: see text] To probe the activities of sperm ADAM protein (fertilinbeta), we devised a general synthetic strategy to generate fluorescently labeled fertilinbeta oligopeptide polymers. Immunofluorescence studies with these polymers demonstrated that fertilinbeta polymers bind specifically to a protein receptor on the mouse egg plasma membrane.     

A facile method to prepare CdS/polystyrene composite particles

Nano-CdS/polystyrene composite particles were prepared via surfactant-free emulsion polymerization. 2-(Dimethylamino)ethyl methacrylate (DMEMA) was used as auxiliary monomer which co-polymerized with styrene (St) and provided the location for coordinating with Cd²⁺. By the coordination of Cd²⁺ ions to DMEMA, mono-disperse polystyrene with the Cd²⁺ ions on the particles surface were prepared successfully. With the release of S²⁻ ions from the thioacetamide (TAA), cadmium sulfide (CdS) was formed. Nano-CdS/PS composite particles could be synthesized via this facile method. The order of materials addition and the amount of initiator both are playing important roles to the final morphologies of the composite particles. In the method proposed in this study, no surfactant was used, and the stable emulsion was successfully obtained. UV–vis absorption and fluorescence measurement indicated the quantum dot effect in the resulted nano-CdS/PS composite particles. The possible composite particle formation mechanism was presented.     

Microwave-assisted synthesis of colloidal inorganic nanocrystals

Colloidal inorganic nanocrystals stand out as an important class of advanced nanomaterials owing to the flexibility with which their physical-chemical properties can be controlled through size, shape, and compositional engineering in the synthesis stage and the versatility with which they can be implemented into technological applications in fields as diverse as optoelectronics, energy conversion/production, catalysis, and biomedicine. The use of microwave irradiation as a non-classical energy source has become increasingly popular in the preparation of nanocrystals (which generally involves complex and time-consuming processing of molecular precursors in the presence of solvents, ligands and/or surfactants at elevated temperatures). Similar to its now widespread use in organic chemistry, the efficiency of "microwave flash heating" in dramatically reducing overall processing times is one of the main advantages associated with this technique. This Review illustrates microwave-assisted methods that have been developed to synthesize colloidal inorganic nanocrystals and critically evaluates the specific roles that microwave irradiation may play in the formation of these nanomaterials.     

Lanthanide-doped inorganic nanocrystals as luminescent biolabels

Trivalent lanthanide ions (Ln(3+)) doped inorganic nanocrystals (NCs) have currently attracted reviving interest and come to the forefront in nanophotonics owing to their potential applications in diverse fields such as luminescent biodetection and bioimaging. As an alternative to conventional biolabels, Ln(3+)-doped NCs show superior features including large stokes shift, multicolor fine-tuning, narrow emission band widths, high photostability, and low toxicity. Particularly, the long-lived luminescence and distinct upconversion (UC) of Ln(3+)-doped NCs are desirable for various bioapplications. The long-lived luminescence of Ln(3+) combined with time-resolved technique can efficiently suppress the interference from short-lived background, resulting in a high signal-to-noise ratio (S/N) and background-free measurements. Near-infrared excited UC emissions of Ln(3+) can bring no autofluorescence and no photodamage to cells or tissues, and thus UC NCs have been regarded as one of the most useful in vivo optical contrast agents. In this review, we outline the most recent development of Ln(3+)-doped NCs as biolabels from the controlled synthesis and surface functionalization of NCs to their bioapplications in heterogeneous and homogeneous biodetection as well as in vitro and in vivo bioimaging.     

A novel method to prepare a fast responsive,thermosensitive poly(N‐isopropylacrylamide) hydrogel

A fast responsive, thermosensitive poly(N‐isopropylacrylamide) (PNIPA) hydrogel was obtained after cold‐treatment of a swollen, untreated PNIPA hydrogel at low temperature for 24 h. After this treatment, the PNIPA hydrogel exhibits a faster deswelling rate than untreated PNIPA hydogel. This property is probably due to an enhancement of the regularity of macromolecular arrangement during the freezing process.