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Crystalline Si core–amorphous SiOx shell nanoparticles were synthesized from SiCl4 using an atmospheric microwave plasma process and their microstructures were investigated. It was found that the amorphous SiOx shell thickness was determined by varying the applied microwave power. The increase of applied power directly increased the length of the flame at the end of the plasma. Through observation of the microstructures with varying lengths of the flame, it was found that a highly crystalline Si phase was formed in the plasma and amorphous SiOx phase was formed in the flame. The longer flame resulted in the thicker SiOx shell around the Si core. The electrochemical properties of the varying SiOx shell thicknesses were also investigated in that the synthesized Si-SiOx nanoparticles were used as anode materials in a lithium-ion battery (LIB). Thin shells such as native oxide did not influence the electrochemical behaviour of the Si core, whilst some shells were too thick to allow Li-ions to react with the Si core. Using Si-SiOx nanoparticles with the optimum SiOx:Si ratio of 18:82, the following electrochemical properties were obtained: a first reversible capacity of 932 mAh/g, an initial columbic efficiency (ICE) of 52.5%, and a capacity retention of 83.7% at the 100th cycle.

Nanoparticles having four different ratios of crystalline silicon (Si) cores and amorphous SiOx shells were synthesized by using a microwave-generated plasma. Their microstructures were analyzed to find quantitative relationships with electrochemical properties. By measuring XRD, SEM, HR-TEM, and Raman spectra of four samples with different core-shell microstructures, the quantitative fractions of crystalline Si core and amorphous SiOx shell in the nanoparticles were calculated. Also, electrochemical properties of the nanoparticles were measured and compared with the calculated fractions. The electrochemical properties such as the initial reversible capacity, the initial coulombic efficiency, and the capacity retention exhibited tendencies remarkably similar to those implied by the calculated fractions. Analysis of each sample's dQ/dV profile also gave us good evidence of understandable relationships between the fractions and electrochemical properties. Details of calculating the fractions from microstructural data are given, with suitable consideration having been given to the fact that several assumptions could lead to errors during the analysis. The approach introduced in this research offers a good means of analysis with which to further the optimal design of nanoparticle microstructure for Li-ion battery anodes.

We synthesized silicon (Si) nanoparticles using an atmospheric microwave plasma process, and investigated the effects of hydrogen (H2) injection on their microstructure during the synthesis. Two nozzles were applied to inject H2 (swirling and rectilinear H2). Our microstructural analysis indicated that the amount and method of H2 injection were critical for completion of the reaction from silicon tetrachloride (SiCl4) to Si, as well as to obtain highly crystalline Si nanoparticles. The swirling H2 was especially critical due to its formation of vortex flow, which allowed relatively long residence time of the H-ions in plasma. The Si nanoparticles synthesized by the atmospheric plasma process had core-shell structures that consisted of crystalline Si cores with amorphous SiOx shells of 5–15 nm thickness. We also investigated the feasibility of the synthesized Si nanoparticles as anode materials in a lithium-ion battery (LIB). For the core-shell structured Si nanoparticles, we obtained the first reversible capacity of 1204 mAhg−1, and a capacity retention of 82.2% at the 50th cycle.

Effects of SiOx or C shells on electrochemical properties of Si nanoparticles were investigated. SiOx shells with thickness of 10~15 nm were formed on homogeneously crystalline Si nanoparticles. Incase of Si-C nanoparticles, there were 30~40 layers of C with a number of defects. Li-ion batteries were fabricated with the above-mentioned nanoparticles, and their electrochemical properties were measured. Pristine Si shows a high IRC (initial reversible capacity) of 2,517 mAh/g and ICE (initial columbic efficiency) of 87%, but low capacity retention of 22%, respectively. SiOx shells decreased IRC (1,534 mAh/g) and ICE (54%), while the retention increased up to 65%, which can be explained by irreversible phases such as LiO2 and Li2SiO3. C shells exhibited no differences in IRC and ICE compared to the pristine Si but an enhanced retention of 54%, which might be from proper defect structures.

Silicon-carbon (Si-C) composites with various weight ratios were prepared through heat treatment of water-soluble carboxymethyl cellulose (CMC) with Si nanoparticles synthesized by using an inductively-coupled plasma. Microstructures of the Si-C composites were thoroughly investigated by using X-ray diffraction (XRD), scanning electron microscopy (SEM) and Raman spectroscopy. The results indicate that we obtained a micro-sized Si-C composite with homogeneously-distributed crystalline Si nanoparticles in an amorphous C-matrix. Pores, which were due to the volatilization of CO2 from CMC during heat treatment, was detected when the concentration of carbon was increased. The electrochemical properties of those Si-C composites for use as anode materials in lithium-ion batteries (LIBs) were also investigated. The C-matrix enhanced the capacity retention, as well as the rate capability of Si nanoparticles, due to the dense and homogeneous microstructures of the composite. The Si-C composites (7:3 weight ratio) retained a reversible capacity of > 1,000 mAh/g with a capacity retention of 88.9% even after 100 cycles. The reversible capacity ratio at a 1.5 C-rate was about 80% as compared with that at a 0.1 C-rate.

Si nanoparticles were synthesized by inductively coupled plasma and a specially designed double tube reactor. By injection of large amount of PH3 during the synthesis, the effects of phosphorous incorporation on their microstructures and chemical binding environments were investigated. Injection of PH3 gas during the synthesis resulted in a change from crystalline to amorphous phase, a reduction of particle size as well as a process yield. All of the above results were attributed to a lower plasma density when higher amount of PH3 was injected. From energy-dispersive X-ray spectroscopy, secondary ion mass spectrometry, and X-ray photoelectron spectroscopy analysis, it was revealed that P was doped in Si nanoparticles. However, secondary phases such as P4 and P2O5 were formed as amorphous ones in nano-scale when a relatively large amount of PH3 was injected. In addition, those nanoparticles were applied as an active material in the lithium-ion battery's anode. Unexpectedly, amorphous Si nanoparticles with secondary phases showed improved electrochemical properties. P-doping in Si nanoparticles could not directly advance cycling performance by improvement of electrical conductivity of Si nanoparticles. It was rather assumed that a secondary phase influenced and enhanced electrochemical properties by additional capacity due to a formation of Li3P and forming an effective buffer against large volumetric change of Si nanoparticles during the charge/discharge. The initial reversible capacity of amorphous Si nanoparticles synthesized with 100 sccm of PH3 flow rate was 2113 mAh g− 1, and that at the 100th cycle was still about 1000 mAh g− 1, which was twice as high as that of Si nanoparticles synthesized without PH3 injection.

Phosphorous (P) incorporated silicon nanoparticles (Si NPs) were synthesized by using inductive coupled plasma (ICP) and a specially designed double tube reactor.Their microstructures were investigated by injecting various amounts of PH3 gas during the synthesis. Injection of PH3 gas during the synthesis resulted in a change from crystalline to amorphous phase, a reduction of particle size as well as process yield. These results were attributed to a lower plasma density when higher amount of PH3 was injected.From EDS, SIMS and XPS analysis, it was revealed that P was successively incorporated in Si NPs.However, secondary phases such as P4 (red P) and P2O5were formed as amorphous ones in nanoscale when a relatively large amount of PH3 was injected.

The autothermal reforming of methane to syngas has been carried out in a reactor charged with both a Ni (15 wt%)-Ru (1 wt%)/-MgO metallic monolith catalyst and an electrically-heated convertor (EHC). The standalone type reactor has a start-up time of less than 2 min with the reactant gas of fed to the autothermal reactor. The and ratio governed the methane conversion and temperature profile of reactor. The reactor temperature increased as the reaction shifted from endothermic to exothermic reaction with decreasing ratio. Also the amount of in the products increases with increasing ratio due to water gas shift reaction. The 97% of conversion was obtained and the reactor temperature was maintained at the condition of $GHSV

In this study, for recovery of renewable noble metal from used stack of fuel cell, synthesis of platinum nano particle is established through effect of platinum solution concentration, pH value, reducing agent and dispersing agent at a volume ratio of 1 mM :10 mM :8 mM Cl4TABr

Carbon-templated mesoporous ZSM-5 zeolites were synthesized directly avoiding a drying process. Carbon nanoparticles were simply mixed into synthesis precursor of ZSM-5 and hydrothermally treated by microwave irradiation. The amount of mesopores formed inside the ZSM-5 single crystals was controllable by adjusting the amount of carbon used. For comparison, mesoporous ZSM-5 zeolites have also been synthesized under hydrothermal conditions. The influence of microwave irradiation on mesoporous ZSM-5 materials was thoroughly investigated by using nitrogen adsorption/desorption studies and 27Al MAS NMR. The nature of acid sites both in the micropores (internal) and on the surface of mesopores (external) was investigated by in situ FTIR spectroscopy using pyridine (Py) and 2′,6′-di-tert-butylpyridine (DTBPy) as a probe molecules. Mesoporous ZSM-5 prepared by microwave synthesis showed higher catalytic activity in the bulky molecular reaction of 2′,4′-dimethoxyacetophenone (2′,4′-DMAP) with 4-methoxybenzaldehyde as a model reaction in comparison with the results obtained over hydrothermally prepared ZSM-5. The further catalytic behavior has been studied in condensation reaction and cracking of substituted benzene.

The trace polymer and additives in used stripper solutions were analyzed by a combination of Py-GC/MS and ESI-MS. In the comparison of the pyrolysates produced by the pyrolysis of the pure stripper and photoresist at 500 o C, the presence of novolac polymer in the used stripper was confirmed by the presence of the characteristic peaks of its pyrolysates, such as those of the methylphenol, di-methylphenol and methylenebis(methylphenol) isomers. The intact trace polymer was measured by ESI-MS, which showed the distribution of oligomers at intervals of 120 Da, indicating di-methylphenol to be the repeat unit. Additional MS/MS measurements demonstrated that the end group is methylphenol and the repeat groups are di-methylphenol. Some modified oligomers caused by the methylation or di-methylation of the repeat unit were also identified. Although the polymer is only present at a trace level in the used stripper, these combined analytical methods provided the means to qualify the stripper solution through the identification and structural determination of the polymer.

Metal incorporation into nanoporous materials could give Lewis acid sites through the framework substitution of silica matrix, which are supposed to be in tetrahedral substitution of silica. In this work, Zr- and Sn-incorporated SBA-16 were directly synthesized by the microwave synthesis method. These microwave synthesized Zr- and Sn-incorporated mesoporous silica materials were applied in activation of ketones by Lewis acid sites to catalyze Meerwein-Ponndorf-Verly reduction of cyclohexanone and Baeyer-Villiger oxidation of adamantanone, respectively. Optimum incorporated Zr- and Sn-species gave almost 100% selectivity with high activity onto corresponding alcohol and lactone, respectively.

The amino-functionalized SBA-15 (NH2-SBA-15) catalysts have been synthesized by different approaches such as direct co-condensation, prehydrolysis of sodium metasilicate, and post synthetic-grafting methods in order to get different morphologies by using the amphiphilic triblock copolymer, pluronic P123 as a surfactant and 3-aminopropyltriethoxysilane (APTES) as a precursor of functional groups under a strong acidic condition. The functionalized materials were confirmed with X-ray diffraction (XRD), N2 gas adsorption/desorption studies, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and the amount of amino-groups was evaluated by TGA analyses. Catalytic transesterification reactions of diethylmalonate with various aliphatic and aromatic alcohols were investigated over the amino-functionalized SBA-15 catalysts. Among the functionalized catalysts, the material synthesized via direct co-condensation method which had short channeled hexagonal platelet morphology exhibited enhanced catalytic activities with normal aliphatic alcohols than other fibrous type catalysts. The activities of the catalysts were found to be very much dependent on morphologies, dispersion of amino groups and molecular shape of alcohols.

MnO 2 -ZrO 2 binary oxide catalytic system was applied for the effective utilization of CO 2 as an oxidant in the ethylbenzene dehydrogenation (EBD) to styrene monomer (SM). MnO 2 -ZrO 2 oxides were prepared by co-precipitation method and characterized as solid solution mixture having surface area more than 100 2 g −1 . 10% MnO 2 -ZrO 2 mixed oxide catalyst exhibited conversion of 73% with the selectivity of 98% at 650 °C. The MnO 2 -ZrO 2 binary oxides were X-ray amorphous whereas the individual oxides (MnO 2 and ZrO 2 ) having much lower surface areas were crystalline in nature. As a result, MnO 2 -ZrO 2 binary oxides exhibited greatly elevated catalytic activity for the conversion of ethylbenzene (EB) than those of individual oxides in the presence of CO 2 . However, in the absence of CO 2 poor catalytic activity and stabilities were observed. Gradual enhancement of activities were demonstrated in the higher CO 2 to EB ratios. Hence, CO 2 had a profound role as a soft oxidant by improving both activity and stability in the EBD over MnO 2 -ZrO 2 mixed oxide catalysts.

Iron-substituted SBA-16 materials have been synthesized by using direct microwave synthesis method under weak acidic conditions. Different iron species including isolated framework iron species, iron cluster and iron oxides were formed by adjusting the pH value and Si/Fe molar ratios. All the materials has been characterized by XRD, N 2 sorption and SEM. Lewis acid catalyzed Friedel-Crafts type alkylation reaction of benzene with benzylchloride has been investigated over Fe catalysts prepared with different pH values and iron contents.

Zr incorporated and pure SBA-16 were prepared by microwave synthesis method. These microwave synthesized Zr-SBA-16 played a role as Lewis acid sites for the Meerwein-Ponndorf-Verly reduction of ketones giving almost 100 % selectivities with high activities.

Silicon nanoparticles (Si NPs) were simply mixed with carbon nanofibers (CNFs) without any chemical process at various weight ratios, and the electrochemical properties of these nanoparticles as anode materials were investigated in lithium-ion batteries (LIBs). To study the effects of the physical incorporation of CNFs on the volumetric variations in Si NPs, the dilations of full cells were measured. The measured volumetric change of the anode using a mixture of Si NPs and CNFs was smaller than that calculated from the theoretical volumetric changes of Si and graphite. Although the reversible capacity of Si NPs faded sharply, the fading was mitigated by increasing the mixing ratio of CNFs. In particular, the Si NP/CNF mixture prepared at weight ratio retained a reversible capacity of >800 mAh/g with a capacity retention of 53.2% even after 100 cycles. CNFs alleviated stress and strain during the charge–discharge process even though there was no tight chemical bonding with Si NPs.