• 한국입자에어로졸학회지
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• 제10권2호
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• pp.53-59
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• 2014

Palladium (Pd) nanoparticles attached graphene (GR) composite was synthesized for an enhanced glucose biosensor. Aerosol spray pyrolysis (ASP) was employed to synthesize the GR-Pd composite using a colloidal mixture of graphene oxide (GO) and palladium chloride ($PdCl_2$) precursor. The effects of the weight ratio of the Pd/GR on the particle properties including the morphology and crystal structure were investigated. The morphology of GR-Pd composites was generally the shape of a crumpled paper ball, and the average composite size was about $1{\mu}m$. Pd nanoparticles less than 20 nm in diameter were deposited on GR sheets and the Pd nanoparticles showed clear crystallinity. The characteristic of the glucose biosensor fabricated with the as-prepared GR-Pd composite was tested through cyclic voltammetry measurements. The biosensor exhibited a high current flow as well as clear redox peaks, which resulted in a superior ability of the catalyst in terms of an electrochemical reaction. The highest sensitivity obtained from the amperometric response of the glucose biosensor was $14.4{\mu}A/mM{\cdot}cm^2$.

• 대한화학회지
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• 제35권6호
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• pp.667-672
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• 1991

팔라듐(Ⅱ) 이온의 존재하에서 isonitrosobenzoylacetone(IBA)과 diamine (ethylenediamine(en) 또는 trimethylenediamine(tn))으로부터 새로운 착물들인 N-(2-aminoethylisonitrosobenzoylacetone imino) chloropalladium(Ⅱ), PdCl(IBA)-en, 및 N-(3-aminopropylisonitrosobenzoylacetone imino) chloropalladium(Ⅱ), PdCl (IBA)-tn을 합성하고 이들 착물의 구조를 조사하였다. 그 결과 이들 착물은 모두 사각평면구조를 가지며 하나의 디이민리간드와 염소이온이 금속에 배위되어 있음을 알 수 있었다. 여기서 디이민리간드는 isonitrosobenzoylacetone과 diamine이 1:1로 반응하여 생성되었으며, isonitroso (=N-O), C=N 및 $NH_2$기의 세개의 질소원자들을 통하여 금속에 결합하고 있는 세자리 리간드임을 알 수 있었다.

• 한국표면공학회지
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• 제48권6호
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• pp.253-259
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• 2015

The test equipment becomes more important with the development of semiconductor industry. MEMS probe is an important testing component to detect the defects from the generated electric signal when it contacts the metal pad of semiconductor devices. Ni-Pd alloy has been paid attention to as a candidate of MEMS probe material because of its high surface hardness and relatively low resistivity. In this study, electroplated Ni-Pd alloy has been prepared by using ethylene diamine as a complexing agent. Solid solution alloy coating could be formed when concentration of palladium chloride and current density were in the ranges of 1~5 mM and $0.2{\sim}1.5A/dm^2$, respectively. The increase of current density brought about an decrease in palladium content, which made both of lattice parameter and grain size smaller. As a result of grain refinement, high hardness could be obtained. However, surface cracking was observed due to residual stress when the current density was above $1.3A/dm^2$. When effects of heat treatment temperature on hardness and sheet resistance were investigated, the accompanied grain growth decreased both of them. The decrease of hardness remained stable at a temperature of $200^{\circ}C$. The sheet resistance was drastically reduced at $100^{\circ}C$. After that, it was found to become constant.

• Macromolecular Research
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• 제13권6호
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• pp.491-498
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• 2005

Fluorene-containing, spiro-type, conjugated polymers were synthesized via the cyclopolymerization of dipropargylfluorenes (2-substituted, X=H, Br, Ac, $ NO_{2}$) with various transition metal catalysts. The polymerization of dipropargylfluorenes proceeded well using Mo-based catalysts to give a high polymer yield. The catalytic activities of the Mo-based catalysts were found to be more effective than those of W-based catalysts. The palladium (II) chloride also increased the polymer yield of the polymerization. The polymer structure of poly(dipropargylfluorene)s was characterized by such instrumental methods as NMR ($^{1}H_{-}$, $^{13}C_{-}$), IR, UV-visible spectroscopies, and elemental analysis as having the conjugated polymer backbone bearing fluorene moieties. The $^{13}C_{-}$NMR spectral data on the quaternary carbon atoms in polymers indicated that the conjugated cyclopolymers have the six-membered rings majorly. The poly(dipropargylfluorene) derivatives were completely soluble in halogenated and aromatic hydrocarbons such as methylene chloride, chloroform, benzene, toluene, and chlorobenzene. The poly(dipropargylfluorene) derivatives were thermally more stable than poly(dipropargylfluorene) itself, and X-ray diffraction analyses revealed that the polymers are mostly amorphous. The photoluminescence peaks of the polymers were observed at about 457-491 nm, depending on the substituents of fluorene moieties.

• Bulletin of the Korean Chemical Society
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• 제18권12호
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• pp.1269-1273
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• 1997

The system which employs iron, palladium, molecular oxygen and hydrogen as a model mono-oxygenase, has been investigated to develop a new method for selective cyclohexane oxidation uner mild conditions. This system provides much higher yield and selectivity for the formation of cyclohexanol and cyclohexanone compared to that of the existing industrial method. When the catalytic system, FeCl2-Pd/alumina, was employed, the oxidation system required acetone as a solvent to be efficient and acidifying the solvent by a little addition of acetic acid or HCl made the system more efficient. The Pd catalyst was recyclable without a significant deactivation but the recycling of ferrous chloride showed the decrease in the activity. On the other hand, the heterogeneous catalytic system, Pd/Fe2O3 could be recovered easily and reused after drying treatment.

• Bulletin of the Korean Chemical Society
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• 제20권6호
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• pp.643-647
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• 1999

Hydropalladium carboxylates, formed from π-allylpalladium chloride dimer plus carboxylic acids, have been shown to catalyze cyclization of structurally diverse enediynes to form the corresponding six- or five-membered rings depending upon the reaction conditions. Some enediynes having an Oxygen linker in an appropriate position under the similar condition yielded the corresponding cyclopropanation products in highly stereoselective manner. A study using deuterated formic acid has proven that the alkylpalladium intermediates formed in our conditions were reduced by the pendant formate ligand. The dienediyne 10 yielded only the tricyclic product 12 in 67% yield, although it was expected to frrm the cyclic product 11. All these cyclizations seemed to occur via the corresponding alkylpalladium intermediates I. which could proceed to the corresponding cyclic products depending on the reaction conditions and the substrates. The study using ceuterated formic acid could provide an important information to understand the present cyclization mechanism. Overall the present study could play an important role in developing new synthetic methodologies for constructing complex polycyclic compounds.

• Bulletin of the Korean Chemical Society
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• 제7권3호
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• pp.235-237
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• 1986

Reaction of $(E)-{\beta}-chloro-{\gamma}$-hydroxyvinylmercurials, prepared by mercuration of propargyl alcohol and 2-methyl-3-butyne-2-ol, with olefins in the presence of a catalytic amount of $Li_2PdCl_4$ and 2 equiv of cupric chloride in methanol at $50^{\circ}C$ gave the corresponding (E,E)-2,4-dienols in moderate yields. However, addition of 1 equiv of inorganic bases such as magnesium oxide to the reaction mixture brings a rapid and clean vinylation and gave high yields of the dienols at room temperature. In the case of hindered (E)-2-chloro-3-chloromercuri-2-buten-1,4-diol prepared from 2-butyne-1,4-diol, reaction with olefins gave the dienols only in low yields even in the presence of 2 equiv of magnesium oxide.

• Bulletin of the Korean Chemical Society
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• 제8권4호
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• pp.246-250
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• 1987

The reaction of aryl iodides or bromides with olefins in the presence of 1 mol % of $PdCl_2(PPh_3)_2$ and 3 equiv. of $n-Bu_3N\; at\; 100^{\circ}C$ in carbon monoxide atmosphere gave the corresponding aryl vinyl ketones in good yields with small amount of vinylated 1-aryl olefins. But, when the reaction was proceeded under the 10 atm of carbon monoxide, aryl vinyl ${\alpha}$-diketones and aryl vinyl ketones were obtained in moderate to good yields. The reaction was tolerant of a wide variety of functional groups on either the aryl halides or olefin compounds. Reactivity of aryl halide decrease in the order; aryl iodide > aryl bromide ${\gg}$aryl chloride. In general, the reaction proceeded well and gave good yields of aryl vinyl ketones and aryl vinyl ${\alpha}$-diketones when reactants are substituted with electron withdrawing groups.

• The Journal of Advanced Prosthodontics
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• 제7권1호
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• pp.56-61
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• 2015

PURPOSE. The purpose of this study was to evaluate the effects of the surface treatment and shape of the dental alloy on the composition of the prosthetic work and its metallic ion release in a corrosive medium after casting. MATERIALS AND METHODS. Orion Argos (Pd-Ag) and Orion Vesta (Pd-Cu) were used to cast two crowns and two disks. One of each was polished while the other was not. Two as-received alloys were also studied making a total of 5 specimens per alloy type. The specimens were submersed for 7 days in a lactic acid/sodium chloride solution (ISO standard 10271) and evaluated for surface structure characterization using SEM/EDAX. The solutions were quantitatively analysed for the presence of metal ions using ICP-MS and the results were statistically analysed with one-way ANOVA and a Tukey post-hoc test. RESULTS. Palladium is released from all specimens studied (range $0.06-7.08{\mu}g{\cdot}cm^{-2}{\cdot}week^{-1}$), with the Pd-Cu alloy releasing the highest amounts. For both types of alloys, ion release of both disk and crown pairs were statistically different from the as-received alloy except for the Pd-Ag polished crown (P>.05). For both alloy type, disk-shaped pairs and unpolished specimens released the highest amounts of Pd ions (range $0.34-7.08{\mu}g{\cdot}cm^{-2}{\cdot}week^{-1}$). Interestingly, in solutions submerged with cast alloys trace amounts of unexpected elements were measured. CONCLUSION. Shape and surface treatment influence ion release from dental alloys; polishing is a determinant factor. The release rate of cast and polished Pd alloys is between $0.06-0.69{\mu}g{\cdot}cm^{-2}{\cdot}week^{-1}$, which is close to or exceeding the EU Nickel Directive 94/27/EC compensated for the molecular mass of Pd ($0.4{\mu}g{\cdot}cm^{-2}{\cdot}week^{-1}$). The composition of the alloy does not represent the element release, therefore we recommend manufacturers to report element release after ISO standard corrosion tests beside the original composition.

• 센서학회지
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• 제27권5호
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• pp.345-351
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• 2018

We employed an unprecedented technique to synthesize porous $WO_3@SnO_2$ nanofibers exhibiting core-shell and fiber-in-tube configurations. Firstly, 2-methylimidazole was uniformly incorporated in as-spun nanofibers containing ammonium metatungstate hydrate and the sacrificial polymer (polyacrylonitrile). Secondly, the 2-methylimidazole on the surfaces of nanofibers was complexed with tin(II) chloride ($SnCl_2$) via simple impregnation of the as-spun nanofibers in ethanol containing tin(II) chloride dihydrate ($SnCl_2{\cdot}2H_2O$). The presence of vacant p-orbitals in tin (Sn) and the nucleophilic nitrogen on the imidazole ring allowed for the reaction between $SnCl_2$ and 2-methylimidazole, forming adducts on the surfaces of the as-spun nanofibers. The calcination of these nanofibers resulted in porous $WO_3@SnO_2$ nanofibers with a higher surface area ($55.3m^2{\cdot}g^{-1}$) and a better response to 1-5 ppm of acetone than pristine $SnO_2$ NFs synthesized using a similar method. An improved response to acetone was achieved upon functionalization of the $WO_3@SnO_2$ nanofibers with catalytic palladium nanoparticles. This work demonstrates the potential application of $WO_3@SnO_2$ nanofibers as sensing layers for chemiresistive sensory devices for the detection of acetone in exhaled breath.