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Journal Archive

Platinum Metals Rev., 2002, 46, (4), 192

NEW PATENTS: October 2002

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ELECTRODEPOSITION AND SURFACE COATINGS

FiIm Deposition on Nanometre Structures

ibm corp U.S. AppL 2002/0, 090, 458

Thin film is deposited on a nanometre structure without filling holes and trenches by coating with a aerogel material and a metal, Uc seed layer, such as Pt or Pd acetylacetonate. The coating is combined with a supercritical fluid, such as Sc-CO2, and a co-solvent, such as an alcohol. When the supercritical fluid is removed the coating Solidifies into the thin Solid fikn.

Chemical Vapour Deposition of Ruthenium Films

applied materlalsinc U.S. Patent 6, 440, 495

A method to deposit Ru fiLms via liquid source CVD uses vaporised bis(ethylcyclopentadienyi)Ru as the CVD source material gas at 100—3000C in a reaction chamber. An O2 source reactant gas is provided. The substrate comprises Ti nitride, TiAl nitride or Ta pentoxide at a temperature of ~ 100-5000C and has a seed layer of Ru, Ir, Pt, Ru oxide, Ir oxide, etc., on which the Ru films are formed. The Ru film can be used as an electrode in a MIM capacitor.

APPARATUS AND TECHNIQUE

Thin FiIm 0xygen Sensor

panametricslnc WoridAppL 02/42, 756

An O2 sensor operating at 30O—350°C, comprises a crystalline ZrO2 (1) sheet, and two porous Pt electrodes poisoned by Pb to a level that will inhibit cross sensitivity to reactive components, such as H2. The Pt electrodes are arranged to induce superionic O transport along current paths in (1) at the electrode surface. O2 concentrations of ppb can be detected.

Optical Switching Device

u.s. phlups corp U.S. AppL 2002/0, 089, 732

An optical switching device comprises a transparent substrate and a switching fiLm of a hydride of Sc and Mg, and optionally Ni, AL Cr, etc., covered with a Pd or Pt catalytically active layer, in contact with an electrolyte. When a potential or current is applied between two electrodes, a change in optical transmission is detectable. The hydride is electrochemically switched from a low-H, mirror-like composition to a high-H, transparent composition, and vice versa, by H exchange. The device can be used in an optical switching element or sunroof.

Electrochemical Light-Emitting Elements

showa denko kk Japanese Appl. 2002/075, 001

An electrochemical light-emitting element (1) uses a Ru complex for its bght-en^tting layer together with a high-polymer Solid electrolyte and an electrolyte salt (1) has a high performance and needs only a low driving voltage to produce high Light emission. (1) has superior stability, reliability, and low manufacturing costs.

Colouring Mater Sensitisation Type Solar Battery CeII

dainippon printing Japanese Appl. 2002/093, 475

A colouring matter sensitisation-type sokr battery Cell is made from kminations of a transparent substrate, a transparent electrode layer, a power generation layer, a back electrode layer and a back substrate. The back substrate is pattem-coated with a Pt paste to form the back electrode layer, then baked with a coating liquid of fine TiO2 grains to form an oxide semiconductor fikn. The fiLm is impregnated, dried, and carries a Ru complex pigment sensitiser. Highly efficient power generation is obtained.

Hydrogen Separating Membrane

mitsubishi kakoki k. Japanese Appl. 2002/119, 834

The manufacture of a highly permeable H2 separating membrane (1) for separating H2 from a H2-containing gas is claimed. (1) is made by forming a Pd-based thin film on the surface of a porous carrier, and then depositing a Pd alloy or a metal to be alloyed with Pd on the pinhole parts of the membrane. After heat treatment, when a Pd-metal, alloy is formed, the pinholes are effectively closed, and H2 yield is increased. (1) is easily made.

HETEROGENEOUS CATALYSIS

Ruthenium Perovskite Production

natl.inst.mater.sci. European Appl. 1, 233, 002

Ru perovskites of the type LaRuO3 (1) are produced by reacting an aqueous solution of La and Ru ions with a precipitate-forming liquid to coprecipitate hydroxides of La and Ru which are then heat treated. (1) may also be precipitated onto a carrier from a homogeneous solution containing La, Ru and urea. The coprecipitated hydroxides have uniform dispersion and the resulting materials are efficient catalysts.

Destruction of CO, VOC and Organic Emissions

degussa ag WorLd AppL 02/34, 371

A high performance catalyst (1) for the destruction of gaseous CO, VOC and halogenated ofganic emissions comprises a layer of Pt group metal deposited on an inert support. A washcoat into which the Pt is deposited consists of Al2O3 stabilised with La2O3, CeO2 stabilised with ZrO2 and Pr6O11. (1) is promoted by S-containing compounds selected from PtSO3, H2SO4, (NH4)2S04, TiOSO4, Ti2(SO4)3, etc.

Production of High Quality OiI Bases

Inst. francais du petrol WorL Appls. 02/48, 289-290

The simultaneous production of very high quality oil bases and middle distillates comprises successive steps of hydroisomerisation (1) and catalytic dewax-ing (2). (1) is performed in the presence of a Pt group metal catalyst deposited on an amorphous acid SiO2-Al2O3 support, with metal dispersion of ~ 20—100%. (2) occurs in the presence of a Pt or Pd catalyst and a molecular sieve selected from ZBM-30, etc.

Catalytic Converter for a Lean-Burn Engine

johnson matthey plc U.S. Patent 6, 413, 483

A catalytic converter (1) for a lean-burn engine comprises a supported two-Layer catalyst. The first Layer contains Pt, K and a Ba NOx storage component on a washcoat of a mixture of at least two of Al2O3, CeO2 and/or ZrO2. The second Layer contains Rh on a washcoat of CeO2 and ZrO2. (1) further has an interLayer of a Ba compound on a washcoat. (1) is more selective for catalyric reaction between NOx and/or nitrate with hydrocarbons and/or CO than for between hydrocarbons and/or CO with O2. NOx can be reduced to N2 under constant lean to stoichiometric conditions without the need for rich spikes.

Hydrogenation of Acetylenes

uop llc U.S. Patent 6, 417, 419

Hydrogenation of 4C acetylenes in a liquid hydrocarbon stream that contains mainly butadiene is performed by contacting H2 and the hydrocarbon stream with a catalytic composite on an inorganic oxide support. The catalytic composite has an average diameter of ≤ 800 μm, with ≥ 70 wt.% of Cu and activator metal Pt, Pd, Ni, Co, Mn, or their mixture, being finally dispersed on the outer 200 μm Layer of the support. The microsphere catalyst has much improved stability and selectivity compared to similar catalysts with particles of diameter ~ 1600 um.

Vapour Phase Carbonylation with Iridium and GoId

eastman chemical co U.S. Patent 6, 441, 222

A vapour phase carbonyLation process produces carboxyUc acids and esters from a gaseous mixture of lower allphatic alcohols, ethers, esters, CO and ester-alcohol mixtures using a Solid supported catalyst. The gaseous mixture includes a halide promoter, and also H2O and MeOH in a moLar ratio of ~ 0.01:1 to ~ 1:1. The catalyst may be C, activated C, pumice, Al2O3, etc., containing 0.01-10 wt% of Ir and all each, preferably 0.1—2 wt.%. The catalyst also comprises another metal selected from alkaline metals, alkaline earth metals, Sn, etc. The carbonylation is performed at 100-3500C and a pressure of 1-50 bar absolute.

(S)-1 -Phenylpropylamine

toyo kaseikogyo Japanese Appl. 2002/088, 031

(S )-l-PhenylpropyLamine (1) is prepared by reacting (R)-I -phenylpropyl alcohol with diphenylphosphoryl azide as an azidation agent in the presence of a base to provide (S )-l-phenylpropyl azide (2). (2) is then subjected to a hydrogenating reaction in the presence of a Pd/C catalyst. (1) is produced in high quality and high yield.

Removing Carbon Monoxide

mitsubishi heavy ind. Japanese Appl. 2002/121, 008

CO can be selectively reduced in a H2-containing gas, to ~ 10 ppm CO, by passing over a supported Ru metal catalyst at 60-350°C. Gas with an O2:CO moLar ratio of 0.01–0.5 is introduced to the catalyst. The difficulty of O2 quality control is avoided.

HOMOGENEOUS CATALYSIS

C-C Coupling Reaction

dsm nv World Appl. 02/57, l99

A C-C Coupling reaction between an optionally substituted (hetero) aromatic bromide compound (1) and a second reactant, such as an aryl boric acid is cLaimed. The process was performed in the presence of an aprotic dipoLar solvent, such as dimethylfor-mamide or N-methylpyrrolidinone, a base and a Pd salt catalyst. The ratio between the quantity of Pd present in the Pd salt and (1) is 0.00001–0.1 mol%, preferably 0.01–0.1 mol%. (1) should contain at least one heteroatom chosen from N, O and S.

Acetic Acid and Methyl Acetate Production

acetex chimie World Appl. 02/62, 739

A continuous production of acetic acid and/or methyl acetate, based on carbonyLation of MeOH, dimethylether, etc., is performed in a homogeneous liquid phase under CO. The catalytic system comprises Rh and a halogenated promoter, with H2O at > 14% concentration. The process is gradually modified by adding an Ir compound. The system shifts from being a Rh-based homogeneous catalyst on its own to a catalyst based on Rh and Ir, or even Ir alone, without stopping the installation and reducing the H2O content.

Ruthenium Alkylidene Catalysts for Olefin Metathesis

california lnst. technol. U.S. Patent 6, 426, 419

Ru allcyUdene complexes (PCy3)(L)Cl2Ru(CHPh) (1), where L is a triazolyUdene ligand, are claimed. (1) show high olefin metathesis activity, which is much higher at higher temperatures than that of the parent catalyst (PCy3)2Cl2Ru(CHPh) (2). When L is 1, 3, 4-triphenyl-4, 5-dihydro-1H-triazol-5-ylidene, (1) is able to catalyse the ring-closing metathesis of substituted dienes to give tetrasubstituted cyclic olefins in good yield. Additionally, (1) has a similar stability towards O2 and moisture as that exhibited by (2).

Living Radical Polymerisation Initiator

kuraray co ltd Japanese Appl. 2002/080, 523

A living radical polymerisation initiating system applicable to a wide range of radically polymerisable monomers comprises a halogenopentamethyl cyclo-pentadienyl bis(triarylphosphine) Ru, an α-halogeno-carbonyl compound or α-halogenocarboxylic acid ester, and an amine. The system can easily and quickly produce a polymer with narrow molecular weight distribution While controlling the molecular weight.

Allene-Substituted Carboxylic Acid Ester

denki kagaku kogyo Japanese Appl. 2002/088, 026

A pure allene derivative free from substituent on the terminal and with a malonic acid ester (with a 1–8C straight chain alkyl a branched alkyl with secondary or tertiary C, allyl, an aromatic hydrocarbon or butadi-enyl group) is produced using a Pd phosphine catalyst, and 2-chloro-1, 3-butadiene. The diene is reacted with a Na compound of a malonic acid ester.

FUEL CellS

Platinum-Ruthenium Electrocatalyst

natl. lnst. adv. ind. technol Japanese Appl. 2002/075, 384

Manufacture of an electrocatalyst (1) for an electrode catalyst joint body in a Solid polymer fuel Cell (SPFQ involves attaching a Pt-Ru catalyst layer to the surface of a polymer electrolyte membrane. (1) has superior oxidation activity for CO and alcohols. The SPFC has high performance.

Hydrogen Generating Device

matsushita electric ind. Japanese Appl. 2002/121, 006

H2 is efficiently produced in a catalyst-containing H2 generating device by suppressing catalyst deterioration due to S. The H2 is produced by contacting a feed fueL such as natural gas or LPG that might contain a S-based compound as an odorant, H2O and air, with a Pt reforming catalyst. The catalyst also contains oxides of La, Ce, AL Ga, Ti, Mg, Ca, Sr and/or Ba with Zr. The H2 can be used in a fuel Cell.

ELECTRICAL AND ELECTRONIC ENGINEERING

Surface-metallised Pigmented Optical Body

3m innovative properties co World Appl. 02/41, 045

A colour-tailorable, surface-metallised, pigmented optical body comprises Layered polymeric core(s) containing layer(s) of a thermoplastic polymer material. The thermoplastic polymer layers contain a dispersion of a particulate pigment such as C. black, Fe oxides, etc. The metallic layer (1) comprises Pt, Ag, all, AL Cu and/or Ni, etc., at the outer surface(s) of the polymeric core (2). The transmission spectrum of the optical body differs from those of (1) and (2). The tinted polymeric films are used to provide neutral or coloured tint, in display devices, mirrors or other optical equipment.

Thermoelectric Device

ibm corp World Appl. 02/47, 178

A thermoelectric device includes an electrical Pt conductor (1) thermally coupled to a cold pLate and also a thermoelement electrically coupled to (1). The thermoelement has a plurallty of tips to couple it electrically to (1). The tips provide a low resistive connection While ntinimising thermal conduction between (1) and the thermoelement. The device has improved efficiency and is used for cooLing substances, such as integrated circuit chips.

Electroless Ni/Pd/all metallisation Structure

flip chtp technologies llc World Appl. 02/58, 144

A Ni/Pd/Au metallisation stack is formed upon the connection pads of integrated circuits at the wafer level by electroless plating. The interconnection pads can be Cu or Al (1). The lower Ni layer bonds securely to (1) and the intermediate Pd layer serves as an out-diffusion barrier for Ni. The upper Au layer can receive a variety of interconnect elements.

Ruthenium Oxide FiIm Formation

general electric co U.S. Patent 6, 417, 062

RuO2 films, for the fabrication of stable thin film resistors for microcircuits, are made by forming an inorganic Ru-based film (1) on a substrate, and then thermally decomposing a portion of (1) by exposure to high-intensity radiation, preferably visible light. RuCl3nH20 and Ru(III) nitrosyl nitrate are used as the precursors. The method does not require thermal treatment which heats the bulk of the substrate, so can be used for non-ceramic substrates in printed circuit boards and flexible circuits.

Top Spin Valve Sensor

ibm corp U.S. Patent 6, 437, 950

A top spin valve sensor includes an IrMn pinning layer formed by ion beam sputter deposition. The magnetoresistive coefficient of the spin valve sensor is increased by placing an IrMnO seed layer between a free layer of the spin valve sensor and a first read gap Layer of the read head. The free layer is preferably a NiFe-free fiLm located between the first and second CoFe-free films.

Ferroelectric Capacitor with High Ferroelectricity

rohm co ltd U.S. Patent 6, 437, 966

A ferroelectric capacitor, with maintained high ferroelectricity, comprises a Si substrate on which is a Si oxide Layer, a lower electrode of an Ir-Pt alloy, a ferroelectric layer and an upper electrode. An Ir oxide layer is placed on the Si oxide layer, followed by an Ir layer on top, then the ferroelectric layer. The Ir-Pt alloy of the lower electrode can be formed to correspond to the ferroelectric layer. O vacancy in the ferroelectric layer can be prevented.

Electrically Conductive Antireflection FiIm

nippon electric glass Japanese Appl. 2002/071, 906

An electrically conductive antireflection fikn (1) consisting of two layers is cLaimed. The first Layer, of thickness 70—250 nm, contains at least one Pt group metal all and/or Ag, and their compounds, and a Co-containing inorganic pigment. The second Layer has a refractive index of 1.3—1.6. (1) is coated on a glass panel of high Light transmittance for use in a cathode ray tube. (1) reduces reflected light, enhances the contrast, and imparts superior antistatic performance and electromagnetic wave shielding.

MEDICAL USES

Microelectrode Catheter for Mapping and Ablation

c. r. bard inc World Appl. 02/47, 569

A catheter (1) for mapping and/or ablation, includes a metallic cap of Pt or all with a plurallty of apertures and electrode(s) disposed in each aperture. Electrodes may be paked, or arranged along the length or ckcumference of the cap. (1) is used to treat a heart condition by placing it inside the heart and mapping a region of the heart with the mapping electrodes on the catheter or ablation using an ablation electrode disposed about the mapping electrodes.

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