Fabrication commercial quartz glass and articles thereof
However, a paramount challenge still exists to fabricate glasses with a higher strength and greater depth of ion-exchange layer DOL. Herein, aluminosilicate glasses with different contents of P 2 O 5 were prepared, and the influence of P 2 O 5 on the increased compressive stress CS and DOL was investigated by micro-Raman technique. The obtained micro-Raman spectra confirmed the formation of relatively depolymerized silicate anions that accelerated the ion exchange. Phosphorus-containing aluminosilicate glasses with a lower polymerization degree exhibited a higher strength and deeper DOL, which suggests that the phosphorus-containing aluminosilicate glasses have promising applications in flat panel displays, windshields, and wafer sealing substrates. The development of ultrathin, high strength, and damage resistance glasses for flat panel displays, windshields, and wafer sealing substrates is an ongoing challenge Wondraczek et al.
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- Chapter-70 Glass and glassware
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- Circuit materials, circuits laminates, and method of manufacture thereof
Chapter-70 Glass and glassware
A circuit substrate laminate, comprising a conductive metal layer; and a dielectric composite material having a dielectric constant of less than about 3. This application claims the benefit of U. Provisional Application Ser. This invention generally relates to circuit materials, methods for the manufacture of the circuit materials, and articles formed therefrom, including circuits and circuit laminates.
As used herein, a circuit material is an article used in the manufacture of circuits and multi-layer circuits, and includes circuit subassemblies, bond plies, resin coated conductive layers, unclad dielectric layers, and cover films. A circuit laminate is a type of circuit subassembly that has a conductive layer, e. Double clad circuit laminates have two conductive layers, one on each side of the dielectric layer.
Patterning a conductive layer of a laminate, for example by etching, provides a circuit. Multilayer circuits comprise a plurality of conductive layers, at least one of which contains a conductive wiring pattern. Typically, multilayer circuits are formed by laminating one or more circuits together using bond plies, by building up additional layers with resin coated conductive layers that are subsequently etched, or by building up additional layers by adding unclad dielectric layers followed by additive metallization.
After forming the multilayer circuit, known hole-forming and plating technologies can be used to produce useful electrical pathways between conductive layers. Mineral and ceramic particulate fillers are widely used to control the dielectric and physical properties of polymeric dielectric composite materials used in dielectric layers. Particularly where a low dielectric constant is desired, hollow glass or ceramic microspheres can be used.
For example, in U. Okada and Fujino, in U. While the synthetic microspheres described above are used for purposes of improving electrical properties in dielectric circuit substrates, there remains a need in the art for low dielectric constant, low loss circuit materials that are suitable for use in demanding applications such as high frequency applications. The above-described drawbacks and disadvantages are alleviated by a circuit subassembly comprising a conductive layer disposed on a dielectric substrate layer, wherein the dielectric layer comprises, based on the volume of the dielectric layer, about 30 to about 90 volume percent of a polymer matrix, and about 10 to about 70 volume percent of filler component comprising a plurality of cenospheres having a ferric oxide content of about 3 weight percent or less based on the weight of the cenospheres; wherein the circuit laminate has a dielectric constant of less than about 3.
A method of manufacture of the dielectric composite material is described, comprising combining the polymer matrix material and the cenosphere filler. Also described are circuit materials, circuit subassemblies, circuits, and multilayer circuits comprising the dielectric composition, and their methods of manufacture. The invention is further illustrated by the following drawings, detailed description, and examples. Referring now to the exemplary drawings wherein like elements are numbered alike in the figure:.
Circuits and multilayer circuits based on the dielectric composite material have properties equal to or superior to those made with more costly synthetic glass hollow microspheres of the prior art.
Cenospheres are hollow, alumino-silicate microspheres that are a byproduct of coal combustion. The hollow microspheres are collected by flotation of fly ash from power plants and purified and classified into controlled particle size distributions. The compositions of these cenospheres are listed in Table 1, showing weight percent ranges of the major components for the various cenosphere products.
As seen in Table 1, aluminum oxide and silicon oxide are the major components of the cenospheres, with ferric oxide making up a smaller portion. As will be described in greater detail in the Examples below, it was unexpectedly found that acceptable high frequency properties could be obtained by controlling the amount of ferric oxide in the cenospheres used in the dielectric composite material.
In one embodiment, the dielectric material has a dissipation factor of less than about 0. In another embodiment, the dielectric material has a dissipation factor of less than about 0. In still another embodiment, the dielectric material has a dissipation factor of less than about 0. The size and the size distribution of the filler particles can vary, depending on the desired characteristics of the dielectric composite material. In an exemplary embodiment, the cenospheres of the particulate filler exhibit a median particle diameter of about 20 to about micrometers, specifically about 20 to about micrometers.
The size distribution can be bimodal, trimodal, or the like. The cenospheres are present in the dielectric composite material in an amount effective to lower the dissipation factor and the dielectric constant of the composition to the desired level, in particular, a level suitable for high frequency circuit substrate applications. In some cases, it is desirable to fine-tune the dielectric constant of a high frequency circuit substrate to a predetermined value, while maintaining a high overall volume loading of filler to achieve a low coefficient of thermal expansion.
In such cases, the desired effect may be obtained by loading levels of the cenospheres as low as about 10 volume percent. In one embodiment, the cenospheres are present in the dielectric composite material in an amount of about 10 to about 70 volume percent vol. In a specific embodiment, the cenospheres are present in the dielectric composite material in an amount of about 20 to about 70 vol.
The dielectric composite material can optionally include an additional particulate filler other than the cenospheres. Use of additional types of fillers allows the dielectric constant, dissipation factor, coefficient of thermal expansion, and other properties of the dielectric composite material to be fine-tuned.
Examples of secondary particulate fillers include, without limitation, titanium dioxide rutile and anatase , barium titanate, strontium titanate, silica including fused amorphous silica , corundum, wollastonite, Ba 2 Ti 9 O 20 , solid glass spheres, synthetic glass or ceramic hollow spheres, quartz, boron nitride, aluminum nitride, silicon carbide, beryllia, alumina, alumina trihydrate, magnesia, mica, talcs, nanoclays, and magnesium hydroxide.
A combination comprising one or more secondary fillers can be used. The fillers can be surface treated with an organofunctional alkoxy silane, zirconate, or titanate coupling agent to improve the dispersion of the filler in the polymeric matrix and reduce water absorption of the finished composite circuit substrate.
The filler component used to manufacture the dielectric composite material can accordingly comprise from 1 to 99 vol. In one embodiment, the filler component comprises 30 to 50 vol. The cenospheres are dispersed in a dielectric polymer matrix material to form the dielectric composite material. Exemplary dielectric polymer matrix materials include low polarity, low dielectric constant and low loss polymer resins, including those based on thermosetting and thermoplastic resins such as 1,2-polybutadiene PBD , polyisoprene, polybutadiene-polyisoprene copolymers, polyetherimide PEI , fluoropolymers such as polytetrafluoroethylene PTFE , polyimide, polyetheretherketone PEEK , polyamidimide, polyethylene terephthalate PET , polyethylene naphthalate, polycyclohexylene terephthalate, polybutadiene-polyisoprene copolymers, polyphenylene ether resins, and those based on allylated polyphenylene ether resins.
These materials exhibit the desirable features of low dielectric constant that can be further improved i. Combinations of low polarity resins with higher polarity resins can also be used, non-limiting examples including epoxy and poly phenylene ether , epoxy and poly ether imide , cyanate ester and poly phenylene ether , and 1,2-polybutadiene and polyethylene. Suitable fluoropolymer matrix materials for the dielectric layer include fluorinated homopolymers, e.
Blends of these fluoropolymers and terpolymers formed from the above listed monomers can also be used as the polymer matrix material.
Units derived from other copolymerizable monomers can also be present in the resin, for example in the form of grafts. Exemplary copolymerizable monomers include, but are not limited to, vinylaromatic monomers, for example substituted and unsubstituted monovinylaromatic monomers such as styrene, 3-methylstyrene, 3,5-diethylstyrene, 4-n-propylstyrene, alpha-methylstyrene, alpha-methyl vinyltoluene, para-hydroxystyrene, para-methoxystyrene, alpha-chlorostyrene, alpha-bromostyrene, dichlorostyrene, dibromostyrene, tetra-chlorostyrene, and the like; and substituted and unsubstituted divinylaromatic monomers such as divinylbenzene, divinyltoluene, and the like.
Combinations comprising at least one of the foregoing copolymerizable monomers can also be used. Post-reacted resins can be used, such as such as epoxy-, maleic anhydride-, or urethane-modified butadiene or isoprene resins. The resins can also be crosslinked, for example by divinylaromatic compounds such as divinyl benzene, e. Mixtures of resins can also be used, for example, a mixture of a polybutadiene homopolymer and a poly butadiene-isoprene copolymer.
Combinations comprising a syndiotactic polybutadiene can also be useful. Suitable liquid resins can have a number average molecular weight greater than about 5, but generally have a number average molecular weight of less than about 5, most preferably about 1, to about 3, For example, in order to improve the stability of the dielectric strength and mechanical properties of the electrical substrate material over time, a lower molecular weight ethylene propylene elastomer can be used in the resin systems.
An ethylene propylene elastomer as used herein is a copolymer, terpolymer, or other polymer comprising primarily ethylene and propylene. Ethylene propylene elastomers can be further classified as EPM copolymers i. Ethylene propylene diene terpolymer rubbers, in particular, have saturated main chains, with unsaturation available off the main chain for facile cross-linking.
Liquid ethylene propylene diene terpolymer rubbers, in which the diene is dicyclopentadiene, are preferred. Useful molecular weights of the ethylene propylene rubbers are less than 10, viscosity average molecular weight. Suitable ethylene propylene rubbers include an ethylene propylene rubber having a viscosity average molecular weight MV of about 7,, which is available from Uniroyal Chemical Co.
The ethylene propylene rubber is preferably present in an amount effective to maintain the stability of the properties of the substrate material over time, in particular the dielectric strength and mechanical properties.
Typically, such amounts are up to about 20 wt. Another type of co-curable polymer is an unsaturated polybutadiene- or polyisoprene-containing elastomer. This component can be a random or block copolymer of primarily 1,3-addition butadiene or isoprene with an ethylenically unsaturated monomer, for example a vinylaromatic compound such as styrene or alpha-methyl styrene, an acrylate or methacrylate such a methyl methacrylate, or acrylonitrile. The elastomer is preferably a solid, thermoplastic elastomer comprising a linear or graft-type block copolymer having a polybutadiene or polyisoprene block, and a thermoplastic block that preferably is derived from a monovinylaromatic monomer such as styrene or alpha-methyl styrene.
Suitable block copolymers of this type include styrene-butadiene-styrene triblock copolymers, for example those available from Dexco Polymers, Houston, Tex. The optional polybutadiene- or polyisoprene-containing elastomer can further comprise a second block copolymer similar to that described above, except that the polybutadiene or polyisoprene block is hydrogenated, thereby forming a polyethylene block in the case of polybutadiene or an ethylene-propylene copolymer block in the case of polyisoprene.
When used in conjunction with the above-described copolymer, materials with greater toughness can be produced. Typically, the unsaturated polybutadiene- or polyisoprene-containing elastomer component is present in the resin system in an amount of about 10 to about 60 wt. Still other co-curable polymers that can be added for specific property or processing modifications include, but are not limited to, homopolymers or copolymers of ethylene such as polyethylene and ethylene oxide copolymers; natural rubber; norbornene polymers such as polydicyclopentadiene; hydrogenated styrene-isoprene-styrene copolymers and butadiene-acrylonitrile copolymers; unsaturated polyesters; and the like.
Levels of these copolymers are generally less than 50 wt. Free radical-curable monomers can also be added for specific property or processing modifications, for example to increase the crosslink density of the resin system after cure. Exemplary monomers that can be suitable crosslinking agents include, for example, di, tri-, or higher ethylenically unsaturated monomers such as divinyl benzene, triallyl cyanurate, diallyl phthalate, and multifunctional acrylate monomers e.
The crosslinking agent, when used, is present in the resin system in an amount of up to about 20 wt. A curing agent can be added to the resin system to accelerate the curing reaction of the polyenes having olefinic reactive sites. They can be used alone or in combination.
Typical amounts of curing agent are from about 1. In another embodiment, the polymer matrix material comprises a poly arylene ether ; optionally, a polybutadiene or polyisoprene polymer, specifically a carboxylated polybutadiene or polyisoprene polymer; and optionally, an elastomeric block copolymer comprising units derived from an alkenyl aromatic compound and a conjugated diene.
The poly arylene ether can also optionally be carboxy-functionalized. The poly arylene ether can be in the form of a homopolymer or a copolymer, including a graft or a block copolymer. Combinations of various forms can be used. Poly arylene ether s comprise a plurality of structural units of formula 1 :.
Exemplary poly arylene ether s include poly 2,6-dimethyl-1,4-phenylene ether , poly 2,6-diethyl-1,4-phenylene ether , poly 2,6-dipropyl-1,4-phenylene ether , poly 2-methylallyl-1,4-phenylene ether , poly di-tert-butyl-dimethoxy-1,4-phenylene ether , poly 2,6-dichloromethyl-1,4-phenylene ether , poly 2,6-dibromomethyl-1,4-phenylene ether , poly 2,6-di 2-chloroethyl -1,4-phenylene ether , poly 2,6-ditolyl-1,4-phenylene ether , poly 2,6-dichloro-1,4-phenylene ether , poly 2,6-diphenyl-1,4-phenylene ether , and poly 2,5-dimethyl-1,4-phenylene ether.
A useful poly arylene ether comprises 2,6-dimethyl-1,4-phenylene ether units, optionally in combination with 2,3,6-trimethyl-1,4-phenylene ether units.
The poly arylene ether can be functionalized so as to provide a functional group that enhances adhesion between a conductive metal layer and the dielectric layer. Functionalization can be accomplished using a polyfunctional compound having in the molecule both i a carbon-carbon double bond or a carbon-carbon triple bond, and ii one or more of a carboxy group, including a carboxylic acid, anhydride, amide, ester, or acid halide.
In one embodiment the functional group is a carboxylic acid or ester group. Examples of polyfunctional compounds that can provide a carboxylic acid functional group include maleic acid, maleic anhydride, fumaric acid, and citric acid. In particular, suitable functionalized poly arylene ether s include the reaction product of a poly arylene ether and a cyclic carboxylic acid anhydride. Examples of suitable cyclic anhydrides are maleic anhydride, succinic anhydride, glutaric anhydride, adipic anhydride, and phthalic anhydride, more specifically, maleic anhydride.
Modified poly arylene ethers such as maleinized poly arylene ethers can be produced by methods as described in U. Examples of commercially available suitable modified and unmodified poly arylene ethers include PPE-MA from Asahi a maleinized poly arylene ether , and Blendex HPP from Chemtura an unmodified poly arylene ether.
In one embodiment, the polybutadiene or polyisoprene polymer is carboxy-functionalized.
US5043002A - Method of making fused silica by decomposing siloxanes - Google Patents
The term annealing is not used in the ordinary sense, i. There is forvevery type of glass an annealing range of temperature. The upper limit of the annealingrangesis Ireferredto in "ordinary practice as the an' nealing temperature, and theprocess of annealing glass as heretofore practiced consists in heating the glass objects momentarily to this high temperature at which all, the internal stress and strain disappear practically instantaneously, and then cooling the lobjectsvery slowly to a temperature at which they can be handled.
By the combination of a three-axis system to move the glass sample and a fast 3D system to move the laser focus, the SLE process is now suitable to produce more complex structures in a shorter time. Here we present investigations which enabled the new possibilities. We started with investigations of the optimum laser parameters to enable high selective laser-induced etching: surprisingly, not the shortest pulse duration is best suited for the SLE process. Secondly we investigated the scaling of the writing velocity: a faster writing speed results in higher selectivity and thus higher precision of the resulting structures, so the SLE process is now even suitable for the mass production of 3D structures.
All 2,493 US products targeted by China’s new 25% tariffs
The use of hazardous or toxic waste to make a glass material a useful product is provided for herein, however, vitrification of hazardous waste for purposes of containment is excluded, see References to Other Classes below. Included within the scope of the class definition are:. Search notes relating to a processes and apparatus and b products will be identified appropriately. Although silicon and silicon dioxide are arbitrarily considered to be glass materials for Class 65, a process of growing these polycrystalline materials is proper for Class 23, even though a rod is used as a bait, unless the shape formed is not a result of crystallization or deposition on the rod. Processes of growing single-crystal of all types of materials, including silicon or silicon dioxide, are proper for Class Although silicon and silicon dioxide are arbitrarily considered to be glass for Class 65, a process of, or apparatus for, growing crystals of these materials is placed in Class 23 for a process exception, see 5 Note in Class , subclasses 1. A patent claiming a Class 23 species of crystallization and a Class 65 species or having a multiple disclosure with generic claims only is classified in Class Class , Semiconductor Device Manufacturing: Process, for the combination of Class unit coating operation or Class unit etching operation with glass melting, shaping or forming, joining, or heat treating.
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Various processes are known in the art that involve the production of metal oxides from vaporous reactants. The most basic requirements of such processes necessitate a feedstock solution, a means of generating and transporting vapors of the feedstock solution hereafter called vaporous reactants and an oxidant to a reaction site, and a means of catalyzing oxidation and combustion coincidentally, producing finely divided, spherical aggregates, called soot. This soot may be collected in any number of ways, ranging from a collection chamber to a rotating mandrel, and simultaneously or subsequently heat treated to form a non-porous, transparent, high purity glass article. The means for executing these reactions is usually a specialized piece of equipment with a unique arrangement of nozzles and burners. Much of the initial research that led to the development, and thus patent protection, of a plethora of such processes focused on the production of fused silica.
Applications include the semiconductor industry. I and II, including Vol. A typical photomask or reticle used in conventional deep-UV optical lithography comprises an optically transparent substrate containing thereon a mask layer which is an optically opaque pattern. Light passes through the non-opaque regions only, generating a pattern below the photomask.
EP0888398A1 - Germanium doped silica forming feedstock and method - Google Patents
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On January 20, Auburn Manufacturing, Inc. The first step in the investigation is the U. International Trade Commission's preliminary injury investigation. Following that affirmative determination, on June 28, the Department of Commerce announced its affirmative preliminary determination in the countervailing duty investigation. On August 25, , the Department of Commerce announced its affirmative preliminary determination in the anti-dumping duty investigation.
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The U. CVD law imposes special tariffs to counteract imports that are sold in the United States with the benefit of foreign government subsidies. Quartz surface products consist of slabs and other surfaces created from a mixture of materials that includes predominately silica e.
Circuit materials, circuits laminates, and method of manufacture thereof
It has been the largest market for Apple iPhones since Since the escalation of tariffs, though, China has stopped buying soybeans and lobsters , and Apple warned it would miss its expected Christmas holiday sales figures because of trade tensions. Skip to navigation Skip to content.
This application is a continuation-in-part of application Ser. The present invention relates to the use of cristobalite in refractory quartz glass articles and in high temperature processes such as are used in the semiconductor industry and in the investment casting industry. It involves the manufacture or fabrication of a wide variety of refractory articles.
This invention relates to a method of economically manufacturing thin silica flakes and novel silica flakes produced by that method. In another aspect, the invention also relates to chromatographic articles made with the silica flakes as well the use of the silica flakes in protective coatings. S Pat. Such a solution or dispersion is often called an "organosol" or a "sol-gel". To make flakes, the organosol is coated onto a non-adhering smooth inert substrate and dried to form a film which may tend to crack and form flakes.
We report a method for fabricating optical quality silica and silica-titania glasses by additive manufacturing, or 3D printing. Key to this success was the combination of sol-gel derived silica and silica-titania colloidal feedstocks, 3D direct ink writing DIW technology, and conventional glass thermal processing methods. Printable silica and silica-titania sol inks were prepared directly from molecular precursors by a simple one-pot method, which was optimized to yield viscous, shear-thinning colloidal suspensions with tuned rheology ideal for DIW. After printing, the parts were dried and sintered under optimized thermal conditions to ensure complete organic removal and uniform densification without crystallization. More specifically they exhibit comparable chemical composition, SiO2 network structure, refractive index, dispersion, optical transmission, and coefficient of thermal expansion. This method establishes 3D printing as a viable tool to create optical glasses with compositional and geometric configurations that are inaccessible by conventional optical fabrication methods.
More particularly, the present invention relates to silica forming feedstocks, and the manufacturing of optical waveguide preforms. Such processes require a feedstock and a means of catalyzing oxidation and combustion of the feedstock to convert the feedstock into finely divided aggregates called soot. This soot can be collected on deposition surfaces, ranging from a collection chamber to a rotating mandrel.