Synthesis and characterization of ordered mesoporous silicon carbide with high specific surface area

Ordered mesoporous silicon carbide with a high specific surface area was prepared using poly(methlysilylene)ethynylene by utilizing mesoporous silica SBA-15 as a template which was etched off after pyrolysis in an argon atmosphere. The obtained sample is mainly composed of randomly oriented β-SiC crystallites, and it exhibits an ordered mesoporous structure, a high surface area of 511 m²/g, a large pore volume of 0.61 cm³/g, and narrow pore-size distributions of 4 nm. The rough surface and high order of the material that result from the strong interconnections of the SiC products are the main reasons for such high surface areas. The mesoporous ceramics have stability even after re-treatment at 900 °C for 2 h under an air atmosphere.     

Synthesis of ZnS nanoparticles into the pore of mesoporous silica spheres

The ZnS nanoparticles were exclusively synthesized in the pores of the mesoporous silica (MS) particles which had been coated with two bilayers of poly(allylamine hydrochloride) (PAH)/poly(styrene sulfonate) (PSS) via the layer-by-layer (LbL) self-assembly technique. Measurements and analysis of XRD and TEM showed that the ZnS nanocrystals were inserted into the pores of the MS spheres. This approach can be used to prepare composite materials involving functional inorganic nanoparticles which have potential application in biological immunoassay and photoelectronic fields.     

Facile synthesis of MnCO3 hollow dumbbells and their conversion to manganese oxide

Manganese carbonate (MnCO₃) hollow dumbbells were synthesized via a polyol process. Based on the structural analysis of the samples obtained at different reaction times, a mechanism of nucleation-growth-aggregation-ripening was proposed to account for the formation of the hollow dumbbells. Moreover, the manganese oxide has also been obtained from the MnCO₃ crystals after thermal transformation in laboratory air, and the phase of final product could easily be controlled to be either MnO₂ or Mn₂O₃, simply by altering the calcination conditions. The manganese oxide powder products possessed mesoporosity and essentially preserved the pristine morphology of the MnCO₃ precursor.     

Spherical mesoporous silica templated with ionic liquid and cetyltrimethylammonium bromide and its conversion to hollow spheres

Spherical mesoporous silica was synthesized using a mixture of 1-methyl-3-octylimidazolium chloride and cetyltrimethylammonium bromide as the structure-directing agent. The obtained silica was characterized by X-ray powder diffraction, scanning electron microscope, transmission electron microscope, and ¹³C NMR spectroscopic techniques. The results show that the spherical silica possesses worm-like mesopores and larger mesopores, with the sizes about 6-50 nm. It is very interesting that the spherical mesoporous spheres were converted to hollow ones after reflux in boiling water. The treatment results in the generation of the hollow interior by dissolving the silica core. Meanwhile, the silica shell is well retained, which is confirmed by SEM and TEM images.     

Synthesis of high surface area mesoporous bioactive glass nanospheres

Mesoporous bioactive glass (MBG) nanospheres having the composition of SiO₂-CaO-P₂O₅ with both a large specific surface area (∼ 1040 m² g^− 1) and pore volume (1.54 cm³ g^− 1) were prepared using the ionic surfactant, cetyltrimethyl-ammonium bromide (CTAB), as a template. The size of the nanospheres depends on the amount of CaO that is incorporated and can be controlled over the range of diameters from 20 to 200 nm under dilute aqueous condition. In vitro bioactivity studies were carried out in simulated body fluid (SBF). Cytotoxicity tests of the MBG nanospheres were also performed by observing their influence on J774 macrophages at various concentrations.     

Synthesis of cubic type hollow silica particles

Cubic-type hollow silica particles were prepared from Fe₂O₃-SiO₂ core-shell composite particles by selectively leaching the iron oxide core materials using acidic solution. The cubic Fe₂O₃ core particles were obtained by the hydrolysis reaction of iron salts. The Fe₂O₃-SiO₂ core-shell type particles were prepared by the deposition of a SiO₂ layer onto the surface of Fe₂O₃ particles using a two-step coating process. The first step involved primary coating with sodium silicate solution followed by subsequent coating by controlled hydrolysis of tetraethoxysilicate (TEOS). The core Fe₂O₃ was removed by dissolution in an acidic solution which gave rise to the hollow type silica particles. Scanning electron microscopic observation clearly revealed that the morphology is closely related to those of core the Fe₂O₃ particles. The cross sectional view determined by transmission electron microscopy revealed a silica shell with a thickness of about 50 nm. The porous texture of the hollow type silica particles is further characterized by nitrogen adsorption-desorption isotherm measurements.     

Synthesis of hollow spheres with mesoporous silica nanoparticles shell

Hollow spheres with mesoporous silica nanoparticles shell were synthesized with the use of cetyltrimethylammonium bromide (CTAB) and polystyrene (PS) hollow spheres as dual templates. The key to this study is that the uneven surface of the template provides nucleation sites for mesoporous nanoparticles, resulting in the formation of hollow spheres with mesoporous silica nanoparticles shell. The final products with hierarchical mesopores can be obtained through a simple one-step approach.     

A dual template method for synthesizing hollow silica spheres with mesoporous shells

PS/silica core/shell composites were synthesized by the modified Stöber method using polystyrene spheres and cetyltrimethylammonium bromide as dual templates under room temperature. The silicate species and the templates were self-assembled to form mesoporous silica shell on the surface of the PS spheres. Hollow silica spheres with mesoporous shell were obtained by removing the polymer core and the templates through calcination. The hollow silica spheres showed high specific surface area of 1099.5 m²/g and narrow pore size distribution centered at 2.31 nm.     

Synthesis and characterization of ordered mesoporous silica by using polystyrene microemulsion as templates

A simple room temperature synthesis of pure mesoporous silica by using a homemade and functional template: polystyrene microemulsion is reported. The process consists of HCl-catalysed sol-gel reactions of tetraethyl orthosilicate (TEOS) in polystyrene microemulsion, followed by removal of the template via solvent extraction or calcining. X-ray diffraction, Transmission Electron Microscope and N₂ adsorption-desorption isotherms are then used to characterize the mesostructure. The results indicate that the synthesized mesoporous silica has a large BET surface area with more than 900 m²/g, large pore volume with more than 0.8 cm³/g and ordered mesopore-structure. This provides a possible way to control the meso-structure and pore size of mesoporous materials via potential functional templates.     

Synthesis of high surface area mesoporous carbonates in novel ionic liquid

High surface area mesoporous SrCO₃, CaCO₃ and MnCO₃ with straw-like bundles morphology were synthesized in a novel imidazolium pyruvate ionic liquid. These carbonates were characterized by X-ray diffraction, Fourier transform infrared spectra and transmission electron microscopy. The results revealed that these carbonates have pure orthorhombic and rhombohedral structures, respectively, and the prepared products all show the unique straw-like morphology. Mesoporous properties and high surface areas of SrCO₃(118 m²/g), CaCO₃(43 m²/g) and MnCO₃ (122 m²/g) were also confirmed by the corresponding N₂ sorption analyses.     

Facile one-pot synthesis and drug storage/release properties of hollow micro/mesoporous organosilica nanospheres

Novel hollow micro/mesoporous organosilica nanospheres (HMOSNs) of uniform diameter and shell thickness of about 90 nm and 15 nm, respectively, and with wormlike micro/mesoporous shell full of uramido groups, have been successfully fabricated by a facile one-pot route. The micro/mesoporosity of the synthesized HMOSNs has been characterized by small-angle and wide-angle X-ray diffraction (XRD), scan electron microscopy (SEM), transmission electron microscopy (TEM) and nitrogen adsorption-desorption measurements. The drug storage and release properties of the synthetic HMOSNs are measured by using ibuprofen (IBU) as a model drug, and a high drug storage capacity of 531 mg IBU per gram HMOSNs and a steady drug release behavior are exhibited.     

Synthesis of a mesoporous silica hollow microsphere using polyvinyl alcohol

A mesoporous silica hollow microsphere was synthesized in the presence of polyvinyl alcohol for the first time. The synthesized material was characterized by various instrumental techniques such as small-angle X-ray scattering, scanning electron microscopy, transmission electron microscopy, N₂ adsorption measurement and Fourier transform infrared spectroscopy. I have succeeded in incorporating an Ultraviolet ray absorber, 2, 2´, 4, 4´ tetrahydroxy benzophenone by mixing it after synthesis. However an attempt to incorporate by mixing before synthesizing it changes the morphology. In addition to polyvinyl alcohol, the use of other polymers such as polyvinyl pyrrolidine and polyethylene glycol also changes the morphology into dry leaves or fibers.     

Sustained electromagnetic properties of Ni-Zn-Co nanoferrites for the high-frequency applications

Nano nickel-zinc-cobalt ferrites of composition Ni_0.49Zn_0.49Co_0.02Fe₂O₄ were prepared by a citrate precursor method. X-ray diffraction, transmission electron microscopy and scanning electron microscopy confirmed the size, structure and morphology of the nanoferrite. After appropriate treatments, the average grains size is about 50 nm and material shows almost constant complex permeability and permittivity in the frequency range from 10 to 200 MHz, equal to ~ 9.1 + j0.51 (loss tangent ~ 0.05) and ~ 4.4 + j0.16 (loss tangent ~ 0.036), respectively. The refractive index n is close to 6.5. Relaxation phenomenon takes place above 200 MHz, an unusual value for spinel ferrites. Owing to these electromagnetic properties, Ni-Zn-Co nanoferrites should be useful for high-frequency applications.     

Morphologically controlled synthesis of mesoporous alumina using sodium lauroyl glutamate surfactant

Mesoporous alumina with various morphologies has been successfully synthesized by a proper sol-gel process using sodium lauroyl glutamate surfactant as a template. Both the mesostructures and morphologies of the resulting alumina can be effectively controlled by adjusting the concentration of the sodium lauroyl glutamate surfactant present in the reaction system. Through characterization by X-ray diffraction, transmission electron microscopy, and N₂ physisorption, the effects of sodium lauroyl glutamate on the mesostructure and morphology of the resulting materials have been investigated in detail, and a possible formation mechanism of the controlled morphologies is proposed. The resulting mesoporous materials showed a potential application in adsorption of toxic organic compounds, which was attributed to the porous structure, high BET surface area, and large pore volume.     

Synthesis and characterization of NiAl2O4 nanoparticles obtained through gelatin

Nanoparticles of NiAl₂O₄ were synthesized by heating (500-1000 °C) the dried resin resultant of a mixture in aqueous solution of gelatin, NiCl₂·6H₂O and AlCl₃·6H₂O. The particle size and microstrain were calculated from the line broadening of X-ray powder diffraction peaks through the Rietveld method refinement: these are 3.9-16 nm and − 0.743-0.139%, respectively. The NiAl₂O₄ nanoparticles were characterized by X-ray powder diffraction (XRPD), thermo gravimetric analysis (TG), BET and TEM techniques.     

Synthesis and structural evolution of hollow flower-type mesoporous silica microspheres

Hollow flower-type mesoporous silica microspheres (designated as HFMSs) with tunable smaller pores and lager pores in the shell have been successfully synthesized via a structural difference-based selective etching treatment of solid silica core/mesoporous silica shell (sSiO₂@mSiO₂) microspheres. The structure of sSiO₂@mSiO₂ microspheres could evolve to rattle-type, hollow structure, flower-type structure, and peanut-type structure from core/shell structure just by varying the etching agent from Na₂CO₃ solution to ammonia solution and adjusting the concentration of etching agent, respectively. Transmission electron microscopy, scanning electron microscopy, and nitrogen adsorption–desorption analysis are applied to characterize the synthesized samples. The mechanism of such a structural evolution is explained in this work.     

Microstructural evolution of iron oxide hollow nanoparticles toward iron oxide nanotubes in a prolonged sintering condition

Prolonged sintering of iron oxide hollow nanoparticles (HNPs) during chemical vapor condensation (CVC) at 800 °C for 6 h showed some interesting morphologies of the iron oxide nanotubes. TEM and XRD studies confirmed that single-walled nanotubes of a mixed phase of α, β, and γ-Fe₂O₃, with a wall thickness of less than 10 nm and an outer diameter of approximately 50 nm were synthesized. The formation of iron oxide nanotubes was thought to be an evolution of iron oxide HNPs based on the sintering.     

Synthesis of silica nanoboxes via a simple hard-template method and their application in controlled release

Silica nanoboxes have been successfully synthesized via a simple hard-template method at room temperature. The MnCO₃ nanocubes are firstly employed as the hard template. Scanning electron microscopy (SEM) is used to characterize silica nanoboxes and indicates the hollow structure of products. The shell thickness of nanoboxes can be well controlled by the amount of tetraethylorthosilicate (TEOS) and the surface area is calculated through the N₂ adsorption-desorption isotherm. Based on these results, a plausible mechanism is proposed to explain the formation of silica nanoboxes. In addition, preliminary tests demonstrate that the silica nanoboxes are capable of being loaded and releasing Rhodamine B, thus showing a great potential in the controlled delivery applications.     

A novel kind of porous carbon nitride using H-magadiite as the template

A novel kind of porous carbon nitride was prepared by pyrolysis of polymerized ethylenediamine using H-magadiite as the template. This material was characterized by XRD, FT-IR, XPS, and nitrogen sorption at 77 K. The BET surface area, pore volume and the median pore width are 436 m²/g, 0.69 cm³/g and 0.84 nm, respectively, based on the N₂ sorption. Using glass carbon electrodes modified by this material, an excellent linear determination range (0.05-0.99 μM) with a low detected concentration limit of 6.9 × 10^− 3 μM could be obtained on the determination of differential pulse voltammetries of dopamine in the presence of 400-fold excess of ascorbic acid.     

Preparation of hierarchical porous carbon by post activation

A series of hierarchical porous carbons (HPCs) have been prepared by a combination of soft-templating and post activation. As evidenced by N₂ sorption tests, the pristine mesopores were basically preserved and micropores were generated on the mesopore wall of mesoporous carbon (MC). The micropore generation on the mesoporous skeleton can be controlled by simply adjusting the KOH ratio and activation temperature. The BET surface area, mesopore surface area and total pore volume of the HPCs increase monotonously with increasing activation temperature and KOH/MC ratio. In contrast, the micropore surface area reaches the maximum at the ratio of KOH/MC of 4. Further increase of KOH/MC ratio and activation temperature reduces the micropore surface area. Structural characterizations confirm that the main mesopore channel was preserved during activation.