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Journal Archive

Platinum Metals Rev., 2002, 46, (2), 89

NEW PATENTS: April 2002

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ELECTROCHEMISTRY

Electrode for Water Purification

h. e. o‘donnell et al. U.S. Appl. 2001/0,042,682

An electrode (1) for H2O purification, includes an intermediate layer and a protective pre-coat layer (containing a Pt group metal,). The former decreases leakage of current from an electrolyte solution directly to the latter. A method to produce (1) is claimed. (1) has a longer service life and good current yield.

ELECTRODEPOSITION AND SURFACE COATINGS

Chemical Vapour Deposition of Ruthenium Films

applied matemals inc European Appl. 1, 178, 131

Thin Ru films are deposited on a substrate by liquid source CVD using bis(ethylcyclopentadienyl)Ru, which is at room temperature. Deposition occurs in the kinetic-limited temperature regime. The bis(ethyl-cyclopentadienyl)Ru is vaporised at 100-300°C to form a CVD source material gas (1). Deposition onto the substrate is performed in a reaction chamber using (1) and O source reactant gas at ~ 100–5000C

High-Purity Bis(ethylcyclopentadienyi)ruthenium

tanaka kuclnzoku kogyo kk World Appl. 01/42,261

High purity bis(ethylcydopentadienytyRu is produced by hydrogenating bis(acetylcyclopentadienyl)-Ru (1) without callsing corrosion. (1) is prepared by reacting bis(cyclopentadienyl)Ru (2) with acetic anhydride and H3PO4 as catalyst, While (2) is prepared by reacting cyclopentadiene with Ru chloride and Zn powder. CVD formation of thin Ru or Ru compound films is also claimed for use in capacitors for ICs.

Fabrication of X-Ray Masks

int business macfljnes corp U.S. Patent 6,287,434

An apparatus, for electroplating one side of a substrate for use in fabricating X-ray masks, has an anode positioned in an electrolyte. A Pt inhibitor electrode (1) is attached to the inner surface of the dielectric plate of the cathode. A Si substrate is attached to the inner surface of the cathode. (1) allows electroplating on one side of the substrate using a rack plating system.

Palladium Plating Solution

kojdda kagaku yakufun kk Japanese Appl. 2001/192,885

A Pd plating solution (1), for decorative and electronic uses, comprises (in g l-1, as metal equiv. amount): 0.01–40 soluble Pd salt, 0.01–10 of pyridine carboxylic acid (PCA) and/or 0.002–1 of soluble salt of Fe, Zn, Tl, Se or Te, 0.005–10 of amine group derivative of PCA, and 0.001–1.2 of aldehyde benzoic acid derivative, and anionic or amphoteric group surfactant. (1) has stable properties and corrosion resistance and the Pd film has high purity, a mirror-like gloss and plasticity. Crack generation is suppressed.

APPARATUS AND TECHNIQUE

Water Denitrification

sÜd chemie mt srl European Appl. 1,178,017

Nitrates are removed from H2O by making it flow over a transition metal catalyst, preferably 0.01–5 wt.% Pd, on a porous carrier which can activate applied H2, forming metallic hydrides (1). Denitrifying bacteria, which can survive in the presence of H2, adhere to (1). CO2 is used to adjust the pH to 4.5–7.8. O3 is fed into the tank to convert nitrites.

Detecting Nitric Oxide

univ duke U.S. Patent 6,280,604

An electrode (1) for rapid in vivo detection of NO in biological samples, such as blood, urine, synovial fluid, lymph, surgical drainage fluid, etc., has a surface made of material containing Ru and at least one oxide of Ru which complexes with NO when exposed to a NO-containing fluid. (1) exhibits maximal NO response after pre-conditioning. Direct response to NO has been observed for the Ru electrodes at potentials ≤ +675 mV vs. Ag/AgCl. While the paradoxical response of the Ru electrodes to NO occurs at potentials > +675 mV vs. Ag/AgCl.

Material for a Deflecting Colour Filter

natl nsist adv dod sci technol Japanese Appl. 2001/147,326

Material for a deflecting colour filter comprises a planar organic metal complex of Pd, Pt or Ni. Light transmittance can be changed, depending on the viewing angle. By gradually increasing the angle of incidence, light transmittance is decreased. For light hitting vertically to the film surface, transmittance is ~ 90%. Light transmittance at a specific wavelength depends on the incident angle of the light.

Gas Sensor to Measure NOx Concentration

ngksparkplugcoltd Japanese Appl. 2001/153,834

A gas sensor, for accurate measurement of NOx concentrations in ICEs, motor vehicles, aeropknes and bollers, comprises an exterior electrode and an internal electrode formed on an O ion conducting layer. The internal electrode comprises (in wt.%): 0.1–25 Pd, 0.1–30 all and remainder Pt An O pump Cell controls the O concentration in the sensor void. O pumping capability is maintained for a long time.

Ozone Generator

kl san jet plasma co ltd Korean Appl. 2001/007,966

An O3 generator using low activity pksma ion discharge effects to produce purified O3 has a discharge plate for low activity plasma ions. The discharge plate is prepared from a composite powder of Zr, Y, Ti, Al oxides and balance SiN. SiO2 gkss is added to form and sinter the synthetic ceramic sheets. Molten metal between the sheets contains 1.8–2.2 wt.% of MO and 0.3–0.7 wt.% of Pt group elements.

HETEROGENEOUS CATALYSIS

Production of Epoxycyclododecane Compound

ube ind ltd European Appl. 1,125,934

An epoxycyclododecane compound (1) for producing the resin component for paints and adhesives, is produced by hydrogenating l, 2-epoxy-5, 9-cyclodo-decadiene with H2 at 0.8–9 MPa pressure, in the presence of a long-life catalyst of Pt supported on activated C, Al2O3, SiO2, etc. (1) are produced in high yield at a high reaction rate. (1) can also be used to produce a kctam compound which is an intermediate for polyamide 12 and polyesters, useful for producing synthetic resins and fibres.

Purification of Naphthalenic Carboxylic Acid

bp corp north america bjc Worid Appl. 01/56,967

A naphthalenic carboxylic acid, especially 2, 6-naphthalene dicarboxylic acid (2, 6-NDA), is purified by contacting with a purification solvent in the presence of H2 and a Group VIII catalyst, such as Ru/C, at 520–575°F. 2, 6-NDA is useful as a monomer in the production of dimethyl-2, 6-naphthalene dicarboxy-late-based polymers for use in films and food and beverage containers. Reduced amounts of organic impurities are obtained in the purified acid.

Palladium Hydrogenation Catalyst

suedchemieag World Appl.01/58,590

A catalyst for hydrogenation of unsaturated hydrocarbons, such as selective hydrogenation of diolefins to monoolefins or of acetylenes to olefins, contains a catalytically-effective amount of Pd and optionally Ag on a support. The support comprises a moulding of trliobal cross-section with holes through the lobes. Catalysts on a trliobal support have higher activity and selectivity than usual and can be used at gas hourly spatial velocities of ~ 12,000–15,000, compared with only 3000–8000 when beads, tablets or extrudates are used. The pressure drop is also lower.

Production of Epoxide

arco chem technol lp WoHdAppl. 01/62,380

An epoxide, such as propylene oxide, is produced by reacting an olefin, H2 and O2 in the presence of a catalyst of Ti zeolite, Pd and all promoter. The Ti zeolite is impregnated with a solution of a Pd compound and all compound in a solvent, followed by solvent removal and drying. Adding the all promoter increases productivity and selectivity to epoxide.

Jet Engine Catalytic Converter

p. bourgon Canadian Appl. 2,299,746

A catalytic converter for a jet engine is bulk into the engine and uses Pt anodised onto all the metal parts of the Combustion chamber and turbine, except for any bearings used in these stages. The anodised Pt catalyses some of the air/fuel mixture in the engine. The engine becomes more responsive, smoother, gains more thmst across the power band, and lists longer as there are fewer contaminating byproducts. Fuel economy is increased.

Hydrogenation Catalyst for Anthraquinones

asahi kasel kogyo kk Japanese Appl. 2001/170,485

A highly active hydrogenation catalyst (1) for anthraquinones is formed from a Pd component on support particles of diameter < 200 μm and bulk density 0.7–1.5 g ml-1. The support is a SiO2-based composition, with Al2O3 and MgO in atomic ratio MgAl > 1/2. The Pd distribution is controlled and has surface area of 40–300 m2 g-1. (1) is almost free from Pd loss and has excellent durability. The support has superior abrasion resistance.

Hydrogenation of Carbonyl Compounds

basfag GermanAppl. 100/09,817

A catalyst (1) used in hydrogenation of carbonyl compounds to alcohols at retatively low temperature (< 140°C) contains (in part wt.): 0.0001–0.5 Re, 0.0001–0.5 Pt and 0–0.25 of Ru, Zn, Cu, Ag, all, Ni, Fe, Mn, Cr, Mo, W and V on activated C, subjected to non-oxidative pretreatment. (1) has higher total selectivity for the hydrogenation of carbonyl compounds to alcohols, without ether formation.

Catalyst Preparation by Chemical Vapour Deposition

hyosung t & c. co ltd Korean Appl. 2001/046,425

A catalyst for the dehydration of hydrocarbons comprises (in wt.%): 0.1–2.0 Pt, 0.0–1.0 K, 0.1–1.0 Sn, and 0.0–1.0 Eu or Yb on an Al2O3-Al borate support. The support is prepared by mixing Al(NO3)3 and H3BO3 with NH3 solution. The support has pore volume 0.4–1.0 cc g-1, mean pore size 200–3000 A and surface area 25–150 m2 g-1. CVD impregnates the catalyst active species onto the support by spray injection of the chemicals in the reactor at 800°C.

HOMOGENEOUS CATALYSIS

Carbonylation of Unsaturated Compounds

shell int res mij bv WorldAppl. 01/68,583

Carbonylation of 3C or more efhylenically unsaturated compounds used in the preparation of detergents, involves reacting CO and hydroxyl-group-containing compounds in the presence of a catalyst system (1) in an aprotic solvent. (1) comprises a source of Pd cations, bidentate diphosphine and a source of anions derived from an acid having pKa < 3 at 18°C in an aqueous solution. High regioselec-tivity towards a linear product is obtained.

Manufacture of Cyclic Polyether Compounds

kagaku gijutsu shinkojigyodan Japanese Appl. 2001/199,987

The manufacture of a cyclic polyether compound used as starting material for the synthesis of natural substances, such as ciguatoxin, comprises cross-coupling an abryl borane and cyclic enol phosphate, in the presence of a basic aqueous solution containing a Pd(O) compound which has a phosphine ligand, as the catalyst. The method can be used to manufacture cyclic polyether product, which is suitable for the synthesis of cyclic compounds larger than six-membered rings.

FUEL CellS

electrode Catalyst for Fuel Cells

nechemcatcorp EuwpeanAppLi, 156, 543

A highly active electtode catalyst (1) for a fuel Cell electrode, such as for SPEFCs, comprises 20–70 wt.% Pt on conductive C, which has O chemically bonded to it, at an atomic ratio of 0.7–3 to the Pt. Also daimed is an alloy catalyst prepared by depositing a metal component which alloys with Pt in a Pt precursor, which is then reduced to form the alloy. (1) is also used in a membrane electrode assembly.

Proton Conducting Polymer Membrane

johnson matthey plc WotM Appl. 01/69,706

A proton conducting polymer membrane of thickness < 100 μn, for a membrane electrode assembly (MEA) and a fuel Cell, comprises channels and/or capiliaries (< 50 μm) arranged in the z-direction of the membrane. Tow or yam or Pt or Nb wires are placed or inserted into the membrane during its formation. The tow or yarn is subsequently removed to form channels; and/or the Pt or Nb is left in situ to form capiliaries. The membrane allows the supply of additional H2O to the system to sustain H2O electrolysis during Cell reversal in a MEA or fuel Cell. The MFA exhibits improved performance at low reactant gas pressure.

Generation of a Hydrogen-Rich Fuel Gas Stream

uop llc U.S. Patent 699,995

A Η-rich fuel gas stream (1) is generated by passing a fuel stream over an O-containing preferential oxidation catalyst at 70–160°C. The catalyst comprises Ru metal dispersed on an Al2O3 carrier with apparent bulk density of 0.2–0.4 g cm-3 and high porosity (average pore size 800–1500 A). (1) containing < 50 ppm of CO is passed to a fuel Cell for electric power generation for a motor vehicle. CO is converted and high selectivity to CO2 is maintained.

Platinum-Ruthenium Alloy Electrodes for Fuel Cells

ishifuku kdjzoku kogyo kk Japanese Appl. 2001/2005,086

Catalysts loaded with Pt-Ru alloys, for fuel Cell electrodes, are prepared by reducing Pt ammine type complexes and Ru salts (not containing Cl) to a state where Ru bonds to C. powder. Very fine Pt-Ru alloy particles are dispersed uniformly on the C. powder support, and poisoning by CO is inhibited.

Selective Oxidation Catalyst for Fuel CeII

matsushita electric works ltd Japanese Appl. 2001/212,458

A selective oxidation catalyst (1) used for fuel Cells, particularly SPFCs, contains Ru and Pt on a porous carrier, such as α-AL2O3, at a Ru:Pt weight ratio of 0.1–9.5. The Ru and/or Pt are locaused in a layer < 100 μm under the outer surface of the porous carrier. (1) selectively oxidises CO in a reformed gas, at low temperature, by an O2-containing gas. rmproved fuel and electricity generation efficiencies are obtained.

ELECTRICALAND ELECTRONIC ENGINEERING

Ceramic Capacitor Electrode-Forming Paste

ngladslsulatorsltd European Appl. 1,178,493

A paste to form a ceramic capacitor electrode contains (in wt.%): 10–14 of an organic vehicle and 86–90 of Pt powder. The Pt powder contains powders of spherical, flaky and indefinitely-shaped particles. The electrode layer film formed with the paste has density of > 80%, surface roughness of 0.4–0.6 μηα and adhesion strength of > 2 kg. There is improved adhesion to the dielectric layer and small through-holes can be made in the electrode layer.

Oxidation Stabilisation of Semicondutors

micron technology inc U.S. Patent 691,364

A catalyst matrix is used in high pressure, high temperature oxidation in N2O of a gate dielectric layer or Cell dielectric layer on Si to stabilise the semiconductor. Oxidation at 5–250 atm pressure and 600–7500C occurs in the presence of a catalyst selected from Pt, Ir, Pd, Rh, Pb, Ni or Ag and their oxides. The method and apparatus prevent N2O from becoming supercritical; temperature and pressure spikes are prevented. The exposure of semiconducting wafers to high temperature is minimised and undesirable diffusion prevented.

Chip-Type Multilayer Electronic Part

tdk corp U.S. Patent 6,342,732

A chip-type laminated electronic part, for a multi-layered ceramic capacitor, comprises internal metal electrodes and terrninal electrodes (1), which contain Ag and Pd as their main ingredients (Ag:Pd = 7:3 to 3:7 wt. ratio). (1) also contain 0.1–1.0 wt% B. (1) are prevented from oxidising when the electrical part is joined to the substrate, so that improved electrical bonding to the internal electrodes is attained.

High Output Piezoelectric Ceramic

nec hyogo ltd Japanese Appl. 2001/146,470

A high output piezoelectric ceramic composition for oscillators, piezoelectric actuators, and ultrasonic motors, consists of ternary composite oxide system of Pb-Mn-Sb, Pb-Zr, and Pb-Ti. Piezoelectric ceramics with a high exothermic threshold of oscillating velocity can be manufactured by sintering at low temperature together with Ag-Pd electrodes.

Reflecting FiIm for Liquid Crystal Display Elements

furuya ktnzoku kk Japanese Appl. 2001/226,765

A heat-resistant reflecting film (1) for a LCD element, consists of Ag alloy material containing 0.1–3.0 wt.% Pd. Also claimed are: a laminate of one or more layers of (1); a LCD element using the laminate; and a portable device which can use the LCD element as reflector, reflecting film or building gkss material. (1) has improved heat-resistance, reliability and optical reflecting rate. (1) has enhanced bonding with the substrate layer, gkss substrate or resin substrate. Brightness is improved, due to reduced optical loss.

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