Battelle Memorial Institute

Delphi Technologies, Inc.

Pacific Northwest Division

Suresh Baskaran

Jun Liu

Glen E Fryxell

Christopher Andrew Coyle

Jerome C Birnbaum

Gordon Lee Graff

Mark David Hemingway

David Emil Nelson

Darrell R Herling

Bob Xiaobin Li

Karel Domansky

Jagannadha R Bontha

Glen C Dunham

Paul J Bruinsma

Nathan J Kohler

William J LaBarge

Joachim Kupe

Walter Thomas Symons

Xiaohong Shari Li

Zhenguo Yang

Kaius Kiiren Polikarpus

Timothy Robert Armstrong

Lawrence Andrew Chick

Carl Elmer Miller

Craig F Habeger

Delbert L Lessor

Kerry Gross

Gary D Maupin

Ralph E Williford

John David Vienna

Gregory Stephen Sims

Lin Song

Suntharampillai Thevuthasan

Jarrod Vincent Crum

John Gerard Darab

Shari Li Xiaohong

Porous ceramic and hybrid ceramic films are useful as low dielectric constant interlayers in semiconductor interconnects. (Hybrid ceramic films are defined as films that contain organic and ceramic molecular components in the structure, as, for example, organosilicates). This invention describes the usefulness of humidity treatments (using specific temperature/humidity treatments as illustrative examples) in increasing mechanical integrity of porous dielectric films with minimal detrimental effect on film porosity or dielectric constant and with no adverse impact on film quality. The efficacy of such treatments is illustrated using surfactant-templated mesoporous silicate films as an example. This invention also describes a specific family of additives to be used with highly pure alkali-metal-free ceramic and hybrid precursors for such dielectric films that will enable better control of the film porosity and quality and lower dielectric constants with the required mechanical integrity. The efficacy of such additives is illustrated using surfactant-templated mesoporous silicate films as a model example. The invention should be broadly applicable to any cross-linked ceramic or hybrid ceramic films (including silicate and organosilicate films, and especially highly porous forms of the films for low-dielectric constant applications). The invention has been found to be particularly effective with surfactant-templated silicate films with nanometer-scale porosity. The invention in either embodiment should also be applicable to evaporation-induced formation of other cross-linked shapes such as fibers and powders.

Method for producing high purity low dielectric constant ceramic and hybrid ceramic films

This invention pertains to surfactant-templated nanometer-scale porosity of a silica precursor solution and forming a mesoporous material by first forming the silica precursor solution into a preform having a high surface area to volume ratio, then rapid drying or evaporating a solvent from the silica precursor solution. The mesoporous material may be in any geometric form, but is preferably in the form of a film, fiber, powder or combinations thereof. The rapid drying or evaporation of solvent from the solution is accomplished by layer thinning, for example spin casting, liquid drawing, and liquid spraying respectively. Production of a film is by layer thinning, wherein a layer of the silica precursor solution is formed on a surface followed by removal of an amount of the silica precursor solution and leaving a geometrically thinner layer of the silica precursor solution from which the solvent quickly escapes via evaporation. Layer thinning may be by any method including but not limited to squeegeeing and/or spin casting. In powder formation by spray drying, the same conditions of fast drying exists as in spin-casting (as well as in fiber spinning) because of the high surface-area to volume ratio of the product. When a powder is produced by liquid spraying, the particles or micro-bubbles within the powder are hollow spheres with walls composed of mesoporous silica. Mesoporous fiber formation starts with a similar silica precursor solution but with an added pre-polymer making a pituitous mixture that is drawn into a thin strand from which solvent is evaporated leaving the mesoporous fiber(s).

Mesoporous-silica films, fibers, and powders by evaporation

Disclosed herein is a ceramic part, gas sensor, and method for making the gas sensor. The ceramic part comprises: an insulating layer affixed to a substrate wherein the insulating layer comprising AlOparticles; and a glass comprising about 45 to about 69 mole percent SiO, 0 to about 9 mole percent BO, 0 to about 26 mole percent AlO, 0 and 25 mole percent SrO, and about 10 to about 26 mole percent REO, where REOis selected from the group consisting of YO, three valent rare earth oxides, and combinations comprising at least one of the foregoing. In one embodiment of a ceramic part, a gas sensor comprises: an electrolyte layer having disposed on opposite sides thereof a first electrode and a second electrode; and an insulating layer that is in intimate contact with the second electrode, wherein the insulating layer comprises alumina and frit. The method of making the gas sensor comprises: disposing a first electrode and a second electrode on opposite sides of an electrolyte layer; forming an insulating layer comprising alumina and frit; disposing the insulating layer adjacent to the second electrode to form a green sensor; and heating the green sensor to a temperature sufficient to sinter the electrolyte layer and the insulating layer.

Gas sensor having an insulating layer

A method of joining metal and metal, or metal and ceramic parts, wherein a first metal part is selected and then processed to form a bond coat that will effectively bond to a sealing material which in turn bonds to a second metal or ceramic part without degrading under the operating conditions of electrochemical devices. Preferred first metal parts include alumina forming alloys from the group consisting of ferritic stainless steels (such as Fecralloys), austinetic stainless steels, and superalloys, and chromia forming alloys formed of ferritic stainless steels. In the case of chromia forming ferritic stainless steels, this bond coat consists of a thin layer of alumina formed on the surface, with a diffusion layer between the first metal part and this thin layer. The bond coat provides a good bonding surface for a sealing layer of glass, braze or combinations thereof, while at the same time the diffusion layer provides a durable bond between the thin alumina layer and the first metal part. In the case of alumina forming alloys, the bond coat consists of cauliflower-like growths of an aluminum oxide nodules embedded in the surface of the alumina forming alloys.

Gas-tight metal/ceramic or metal/metal seals for applications in high temperature electrochemical devices and method of making

A non-thermal plasma (NTP) reactor structural conductor element includes a base conductor support and a high dielectric constant (&ldquo;high k&rdquo;) barrier layer supported by and substantially surrounding the base conductor support to form a structural conductor NTP reactor element. The structural conductor element may comprise a variety of shapes such as plates, sheets, half-box, I shapes, C shapes, or comb shapes, among others. In one embodiment, the dielectric barrier layer includes a coating applied to the base conductor support. In another embodiment, the dielectric barrier layer includes a high k film laminated to the base conductor support. In yet another embodiment, the base conductor support integrally forms the dielectric barrier layer via conversion of surfaces of the base conductor using electrochemical, thermal or chemical means to form the dielectric barrier layer.

Non-thermal plasma reactor and method-structural conductor

Vacuum/gas phase reactor embodiments used in gas phase dehydroxylation and alkylation reactions are described in which the substrate could be subjected to high vacuum, heated to target temperature, and treated with silane as quickly and efficiently as possible. To better facilitate the silylation and to increase the efficiency of the process, the reactor is designed to contain quasi-catalytic surfaces which can act both as an &ldquo;activator&rdquo; to put species in a higher energy state or a highly activated state, and as a &ldquo;scrubber&rdquo; to eliminate possible poisons or reactive by-products generated in the silylation reactions. One described embodiment is a hot filament reactor having hot, preferably metallic, solid surfaces within the reactor's chamber in which wafers having mesoporous silicate films are treated. Another is an IR reactor having upper and lower quartz windows sealing the upper and lower periphery of an aluminum annulus to form a heated chamber. Finally, a flange reactor is described that includes a flange base and lid forming a tiny chamber therein for a wafer, the reactor being heated by conduction from a hot sand bath. The dehydroxylation and alkylation treatment of mesoporous silica films produces treated films exhibiting low dielectric constant and high elastic modulus.

Vacuum/gas phase reactor for dehydroxylation and alkylation of porous silica

A non-thermal plasma reactor element is provided comprising a multi-cell stack prepared from a plurality of formed building blocks of dielectric material, the walls of the building blocks defining a cell having an exhaust passage for flowing gas to be treated therethrough. A conductive print forming an electrode and connector is disposed on at least one wall of each of the cells and outer insulative plates, disposed on opposite ends of the multi-cell stack, are provided to protect the conductive print. The non-thermal plasma reactor element includes cells defined by a single structural dielectric barrier comprising a &ldquo;conductor-single structural dielectric barrier-exhaust passage-conductor&rdquo; arrangement, wherein individual cells of the reactor element are defined by a single structural dielectric barrier.

Non-thermal plasma reactor design and single structural dielectric barrier

The present invention is a method of dehydroxylating a silica surface that is hydroxylated having the steps of exposing the silica surface separately to a silicon organic compound and a dehydroxylating gas. Exposure to the silicon organic compound can be in liquid, gas or solution phase, and exposure to a dehydroxylating gas is typically at elevated temperatures. In one embodiment, the improvement of the dehydroxylation procedure is the repetition of the soaking and dehydroxylating gas exposure. In another embodiment, the improvement is the use of an inert gas that is substantially free of hydrogen. In yet another embodiment, the present invention is the combination of the two-step dehydroxylation method with a surfactant templating method of making a mesoporous film.

Method of dehydroxylating a hydroxylated material and method of making a mesoporous film

The present invention is a mesoporous silica film having a low dielectric constant and method of making having the steps of combining a surfactant in a silica precursor solution, spin-coating a film from this solution mixture, forming a partially hydroxylated mesoporous film, and dehydroxylating the hydroxylated film to obtain the mesoporous film. It is advantageous that the small polyoxyethylene ether surfactants used in spin-coated films as described in the present invention will result in fine pores smaller on average than about 20 nm. The resulting mesoporous film has a dielectric constant less than 3, which is stable in moist air with a specific humidity. The present invention provides a method for superior control of film thickness and thickness uniformity over a coated wafer, and films with low dielectric constant.

Mesoporous silica film from a solution containing a surfactant and methods of making same

The invention provides a method for synthesizing a titanium oxide-containing film comprising the following steps: (a) preparing an aqueous solution of a titanium chelate with a titanium molarity in the range of 0.01M to 0.6M. (b) immersing a substrate in the prepared solution, (c) decomposing the titanium chelate to deposit a film on the substrate. The titanium chelate maybe decomposed acid, base, temperature or other means. A preferred method provides for the deposit of adherent titanium oxide films from C2 to C5 hydroxy carboxylic acids. In another aspect the invention is a novel article of manufacture having a titanium coating which protects the substrate against ultraviolet damage. In another aspect the invention provides novel semipermeable gas separation membranes, and a method for producing them.

Thin films and uses

The present invention is a novel method for freeform fabrication. Specifically, the method of solid freeform fabrication has the steps of:

Method of freeform fabrication by selective gelation of powder

Growing community of inventors

Kennewick, WA, United States of America

Suresh Baskaran