WO2002062723A2 - Compression molded inorganic fiber articles, and methods and compositions used in molding same - Google Patents
Compression molded inorganic fiber articles, and methods and compositions used in molding same Download PDFInfo
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- WO2002062723A2 WO2002062723A2 PCT/US2002/003906 US0203906W WO02062723A2 WO 2002062723 A2 WO2002062723 A2 WO 2002062723A2 US 0203906 W US0203906 W US 0203906W WO 02062723 A2 WO02062723 A2 WO 02062723A2
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- WIPO (PCT)
- Prior art keywords
- article
- composition
- fireplace
- molding
- inorganic
- Prior art date
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/24—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24B—DOMESTIC STOVES OR RANGES FOR SOLID FUELS; IMPLEMENTS FOR USE IN CONNECTION WITH STOVES OR RANGES
- F24B1/00—Stoves or ranges
- F24B1/18—Stoves with open fires, e.g. fireplaces
- F24B1/1808—Simulated fireplaces
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24C—DOMESTIC STOVES OR RANGES ; DETAILS OF DOMESTIC STOVES OR RANGES, OF GENERAL APPLICATION
- F24C3/00—Stoves or ranges for gaseous fuels
- F24C3/002—Stoves
- F24C3/006—Stoves simulating flames
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
Definitions
- the invention relates generally to a method of compression molding, and to articles produced using compression molding.
- the invention also relates generally to a molding composition including inorganic fibers for use in such compression 10 molding methods and compression molded articles. More specifically, the invention relates to compression molding an inorganic fiber matrix to form articles made up of inorganic fiber.
- Vacuum formed articles made of ceramic or refractory fibers are generally 15 known. For example, it is known to mix chopped dry ceramic fibers with water and various fillers to form a slurry, and then vacuum form the slurry into various articles composed mainly of chopped ceramic fibers. Such articles are often used in high temperature environments, and can withstand high temperatures without decomposition or deformation of the articles. For example, fireplace boxes and 20 artificial fireplace logs have been produced by using such vacuum forming techniques.
- Vacuum forming techniques of forming ceramic fiber articles have been very useful, but it would be desirable to provide an alternative method of forming ceramic fiber articles that does not involve vacuum forming. Vacuum forming techniques tend 25 to be slow, dirty, and relatively complicated. Additionally, it would be desirable to provide ceramic fiber articles that have increased strength, dimensional stability, and thermal conductivity properties as compared to those formed using vacuum forming techniques. Summary of the Invention
- the invention provides a method of forming articles made of an inorganic fiber material using compression molding.
- the use of compression molding to form inorganic fiber articles is distinctly different from vacuum forming techniques of making such articles. Additionally, in at least some embodiments, the use of compression molding to form inorganic fiber articles provides for an improvement over vacuum forming techniques, and in some embodiments, provides for inorganic fiber articles having desirable strength and integrity characteristics.
- the invention is directed to a method of forming an article, the method including: providing a molding composition comprising inorganic fiber and an inorganic binder, and compression molding the molding composition into the article.
- the invention is directed to a method of forming an article, the method including: providing a molding composition comprising inorganic fibers and a binder, and compression molding the molding composition into the article, wherein at least 75% by weight of the molded article is inorganic material.
- the invention is directed to a method of forming an article, the method including: providing a molding composition comprising inorganic fibers and a binder, and compression molding the molding composition into the article such that the binder cures, wherein the cured binder is capable of withstanding temperatures of at least 600° F without significant degradation or deterioration due to heat.
- the invention is directed to a method of forming an article, the method including: providing a molding composition comprising inorganic fibers and a binder, and compression molding the molding composition into the article, wherein the article is capable of withstanding temperatures of at least 600° F without significant degradation or deterioration due to heat.
- the invention is directed to articles made by the use of such methods.
- the invention is directed to a molding composition for use in compression molding an article.
- the compression molded inorganic fiber articles are intended for use in high temperature environments.
- some embodiments are contemplated for use as a component of: a fireplace assembly, a grill assembly, a campfire assembly, a burner assembly, or the like.
- Examples of such articles can include a fireplace box, a surround, a combustion chamber, a fireplace door, a log or log set, a burner, and a refractory member.
- Fig. 1A is a front perspective view of a compression-molded combustion chamber in accordance with one embodiment of the invention
- Fig. IB is a back perspective view of the compression molded combustion chamber of Fig. 1A;
- Fig. 2 is a front view of the compression molded combustion chamber of Fig. 1A;
- Fig. 3 is a top view of the compression molded combustion chamber of Fig. 1A;
- Fig. 4 is a bottom view of the compression molded combustion chamber of Fig. 1A;
- Fig. 5 is a back view of the compression molded combustion chamber of Fig. 1A;
- Fig. 6 is a side view of the compression molded combustion chamber of
- FIG. 1A Fig. 7 is cross-sectional view of the compression molded combustion chamber of Fig. 1A taken along line 7-7 of Fig. 2;
- Fig. 8 is a cross-sectional view of the compression molded combustion chamber of Fig. 1 A taken along line 8-8 of Fig. 2;
- Fig. 9 is a cross-sectional view of the compression molded combustion chamber of Fig. 1A taken along line 9-9 of Fig. 2;
- Fig. 10 is a cross-sectional view of the compression mold used to mold the combustion chamber of Fig. 1 A showing the mold in an open position with unmolded inorganic fiber composition in the bottom portion of the mold;
- Fig. 11 is a cross-sectional view of the compression mold of Fig. 10 showing the mold in a closed position and molding the inorganic fiber composition;
- Fig. 12 a cross-sectional view of the compression mold of Fig. 10 showing the mold in an open position and the compression molded combustion chamber in accordance with one embodiment of the invention.
- Fig. 13 is a schematic top view of a monolithic panel for a gas burner according to one embodiment of the invention.
- Figure 14 is a schematic cross-sectional view of the monolithic panel of Fig. 13, taken along line 14-14 of Fig. 13;
- Figure 15 is a schematic cross-sectional view of the monolithic panel of Fig. 13, taken along line 15-15 of Fig. 13.
- the invention relates to the use of compression molding techniques to mold a matrix including inorganic fibers into useful articles, hi some embodiments, methods of the invention generally include providing a molding composition including inorganic fibers and a binder, and compression molding the molding composition into the article.
- the first step involved in one embodiment of such a molding method entails providing the molding composition.
- the molding composition generally includes inorganic fibers, binder, carrier solvent, and optional additives. A more detailed discussion of some embodiments of the molding composition will be provided below.
- the next step entails compression molding the molding composition.
- Compression molding as used herein generally involves the use of a heated mold and compressive pressure produced by the mold to form the moldable composition into a desired shape.
- Many compression molding techniques may be used.
- the mold comprises a plurality of matched dies, and in some embodiments, a pair of dies, for example male and female dies, that mate with each other to form a mold cavity or mold cavities.
- the dies are attached to equipment that is designed to bring the dies together with enough compressive pressure to perform the molding. It is contemplated that in other embodiments, the weight of the dies can create enough compressive pressure to perform the molding.
- the dies are typically preheated to a molding temperature, and a measured quantity of moldable composition including inorganic fiber is placed in the heated mold.
- the moldable composition is placed in the heated mold when the mold is in the open position.
- the mold is then closed and the moldable composition, through pressure applied from the closing of the mold, fills the mold cavity.
- Continued heating at least partially cures the moldable composition within a relatively short period of time, in some embodiments within a matter of minutes, such that the molded article retains its shape. Pressure is then released, the dies are separated, and the molded article is removed from the mold.
- the moldable composition is forced into the heated mold through one or more injection ports using appropriate injection techniques when the mold is in the closed position.
- the moldable composition through pressure from the injection process, and compression from the closed mold dies, fills the mold cavity, and is formed into the desired shape. Therefore, it will be understood that as used herein, the terms "compression molding” is intended to include embodiments using all types of known compression molding, including such injection techniques.
- compression molding the moldable composition including inorganic fiber will now be described, with reference to Figs. 10-12. Referring to Fig.
- a cross section of a compression mold 120 in an open position is shown, including a top die 122 and a bottom die 124 which together define a mold cavity 126 in the desired shape of the article to be molded.
- the article to be molded is a monolithic combustion chamber for use in a fireplace assembly, for example a combustion chamber of a gas fireplace assembly.
- the mold cavity 126 includes an upper surface 135 and a lower surface 136. Typically, the mold surfaces 135 and 136 are hardened and highly polished.
- the mold may also include ejector pins (not shown), or other such structures as generally known in the art, to aid in the removal of the article when the molding process is complete.
- the dies are mounted on platens 140 and 142 of a press 144, for example a vertical hydraulic press. The press 144 is operated to open and close the mold 120, and typically is able to create the necessary compression pressure for molding.
- the dies 122 and 124 are preheated to a predetermined molding temperature.
- the molding temperature is over 400°F, preferably in the range of 425°F to 475°F, or in the range of 440°F to 460°F, and more preferably about 450°F.
- the dies 122 and 124 are preheated using heated platens 140 and 142, and heat is transferred from the platens 140 and 142 to the dies 122 and 124.
- the molding composition including inorganic fibers 150 is then introduced into the lower die 122, and the press 144 is operated to close the mold 120. (Fig. 11). As the mold 120 is closed, an appropriate amount of compression molding pressure is applied to achieve the desired molding. As will be understood by those of skill in the art and others, the necessary amount of molding pressure is dependent upon many variables, for example the size and complexity of the article being molded, the properties of the particular molding composition used, and other such parameters. In some embodiments, a compression pressure of up to 50 tons is applied. In other embodiments, a compression pressure in the range 1 to 20 tons, or in the range of 3 to 10 tons is applied.
- the moldable composition 150 through pressure applied from the closing of the mold 120, fills and is formed into the shape of the mold cavity. Continued heating of the composition in the mold at least partially cures the moldable composition within a relatively short period of time, in some embodiments within a matter of minutes, such that the molded article retains its shape.
- the amount of time necessary can vary, depending upon the size and shape of the part, the properties of the particular molding composition used, and other such parameters.
- the press is operated to separate the dies 122 and 124, and the molded article 151 is removed from the mold 120.
- the molded article can be further dried by either air drying, or in some cases, by oven drying or firing, hi some embodiments, however, the article can be dried by being held in the heated mold for a longer period of time to achieve the desired drying.
- additional drying can be achieved by oven drying after removal from the mold at a temperature in the range of 350° F and 1800° F, more preferably in the range of 650° F to 750° F for a sufficient amount of time to drive off any of the remaining excess carrier solvent, for example water, from the mold composition.
- the dry time depends greatly upon the method of drying used, and the article being formed.
- the article can be trimmed or machined to a final desirable shape, if needed, and colored as desired.
- the molding composition generally includes inorganic fibers, binder, carrier solvent, and optional additional additives.
- the inorganic fiber is generally described as fibers made of one or more inorganic materials.
- inorganic fibers include glass fibers, ceramic fibers, ref actory fibers, refractory ceramic fibers (RCF), mineral fibers, or other like inorganic fibers, or mixtures thereof.
- Such fibers can include, for example, staple fiber, spun fiber, continuous fiber, bulk fiber, filament fiber or wool fibers or the like, or mixtures thereof.
- the fibers can be in a broad variety of forms, for example, in a crystalline or polycrystalline form, or the like, or mixtures thereof.
- Refractory ceramic fibers (RCFs) along with fibrous glass and mineral wool, are often times grouped as man-made materials generally referred to as synthetic vitreous fibers (SVF).
- the fibers are selected from chopped fiber glass, alumina silicate RCF, or mixtures thereof.
- fibers that can withstand high temperatures.
- the size of the inorganic fibers can vary greatly, depending upon many variables, for example the particular article being molded, or the desired properties or characteristics of the molding composition or the finished article.
- the fibers range in length from less than 1/16 of an inch to two inches, preferably from 1/16 of an inch to 1 inch, and more preferably from 1/8 of an inch to 1/2 of an inch.
- the fibers have a diameter in the range of 1 micron to 30 microns, preferably in the range of 4 microns to 9 microns, and more preferably in the range of 5 microns to 7 microns.
- the fibers can make up a major component of the composition, for example in some envisioned embodiments, up to 80 % or more of the composition. However, in some embodiments, a significant amount of fillers, for example inorganic fillers, can be used, thereby reducing the necessary concentration of inorganic fiber.
- the binder used acts to bind the components of moldable composition together when cured during the molding process.
- the binder includes inorganic or organic binders generally known, or mixtures thereof. Examples of binders include silica, sodium, calcium, and magnesium based binders, and the like, or mixtures thereof. Other examples include polymeric materials, petroleum distillate, polyethylene oxide, and the like, or mixtures thereof.
- the binder can be hydrous, anhydrous, crystalline, or amorphous.
- the binder within the molding composition in the form of a dispersion, emulsion, slurry or solution with the carrier medium.
- binders that can withstand high temperatures.
- the preferred binders include amorphous silica.
- the carrier solvent typically acts to create a dispersion, emulsion, slurry or solution with the rest of the components.
- the moldable composition is in the form of a slurry.
- the carrier solvent is burned off or leaves due to the heat during the molding process, and little or none remains in the finished molded article.
- the preferred carrier solvent for most embodiments is water.
- the moldable composition preferably includes water as the primary carrier solvent.
- the composition preferably has a moisture content in the range of 20 to 35% , more preferably 23 to 30%, and most preferably 25 to 27% by weight of the total composition.
- additives can optionally be included within the molding composition to provide the molding composition or the final molded article with desirable properties.
- additives can be included to enhance the emulsion or dispersion of the components of the composition, to enhance the moldabihty of the composition or to enhance the appearance or physical properties of the molded article.
- Some examples of additives include inorganic or organic fillers, surfactants, diluents, thickeners, solvents, dyes or colorants, or other appearance enhancing materials, and the like, or mixtures thereof. Fillers can be used, for example, to increase the volume of the composition and reduce the necessary amount of inorganic fiber. Additionally, some fillers can be added to impart desired properties to the final molded article.
- fillers include inorganic or organic fillers that are compatible with the other components in the composition.
- Preferred fillers include inorganic fillers, for example silica compounds, such as alumina silicate, crystalline silica, and the like.
- Another example of an inorganic filler includes ceramic micro spheres, and the like.
- an example of a preferred emulsion or dispersion agent is petroleum distillate, hydrotreated light. This material can also act as a carrier in the formulation.
- Nonylphenol polyethylene oxide is another example of a dispersing or emulsifying agent that can also act as a surfactant.
- an organic polymer such as an acrylic polymer
- an organic polymer is added to the composition to act as a dispersing agent, and also to act as a molding thickener to help the composition hold shape when it is being molded.
- this type of material is burned off during the molding process.
- the organic polymer can be present in the composition in the range of about 0.1 to about 5%, more preferably in the range of 0.1 to 1%, and more preferably in the range of 0.1 to 0.5%, by weight of the total composition. It is contemplated that these, and many other additives can be used in compositions embodying the invention.
- Some embodiments of moldable compositions comprise the constituent concentrations for base components as found in Table 2, wherein the values are given in wt. % of the ingredients in reference to the total composition weight. Table 2
- the molding composition is made by mixing the inorganic fibers and any filler with a binder solution that is in aqueous form and includes any additional additives. After the combination of fibers, filler and binder solution are mixed together, they are agitated so that the fibers completely adsorb the binder solution. After the mixing and agitation occurs, a slurry or paste is formed that is of a consistency that permits the mixture to be used to fill the compression mold, and is ready to be compression molded.
- One specific example of a molding composition comprises the constituent concentrations for base components as found in Table 3, wherein the values are given in wt. % of the ingredients in reference to the total composition weight.
- Another specific example of a molding composition comprises the constituent concentrations for base components as found in Table 4, wherein the values are given in wt. % of the ingredients in reference to the total composition weight.
- One preferred moldable slurry of ceramic fibers is a product named THERMOSEAL® Moldable P244, which is commercially available from Mid- Mountain Materials Incorporated of Seattle, Washington.
- Another preferred moldable slurry of ceramic fibers is a product named THERMOSEAL® Moldable P254, which is commercially available from Mid-Mountain Materials Incorporated of Seattle, Washington.
- the molding composition or the finished article are made up of primarily inorganic materials.
- the molding composition or the finished article include at least 75% by weight inorganic material, or in other embodiments, at least 90% by weight inorganic material, and in still other embodiments, at least 95% by weight inorganic material, and sometimes at least 99%o by weight inorganic material.
- the molding composition, prior to molding includes a mixture of inorganic and organic material, but that a significant portion of the organic material will be burned off, or leave during the molding process, leaving the final compression molded article to be made up of primarily inorganic materials.
- the final compression molded article comprises materials that can withstand high temperatures.
- materials that can withstand high temperatures.
- fibers, binders, or any other optional ingredients, such as fillers that when molded into the final article can withstand temperatures of at least 600°F, or at least 800°F, or least 1000°F, or at least 1200°F, and more preferably at least 1300°F, without significant degradation or deterioration due to the heat.
- Figs. 1A, IB and 2-9 show one embodiment of a compression molded article that was molded in accordance with the invention.
- a compression molded monolithic combustion chamber enclosure 251 for use in a fireplace, for example a gas fireplace, is shown.
- the combustion chamber enclosure 251 defines an outer surface 254 and inner surface 256.
- the combustion chamber enclosure includes a bottom panel 258, side panels 260 and 262, a top panel 264, and a back panel 265.
- the combustion chamber enclosure 251 can define one or more apertures that are formed through the one or more of the panels during the compression molding process.
- the one or more apertures can be formed through one or more of the panels after the molding process .
- the top panel 264 defines an aperture 268, for example, for venting combustion products
- the back panel 265 defines an aperture 270, for example, for supplying air or gas to the combustion chamber 251
- the bottom panel 258 defines an aperture 272, for example, for supplying air or gas to the combustion chamber, as shown in Figures 1 A, IB and 2-9.
- the aperture 268 and the aperture 272 were formed in the combustion chamber in post molding operations, while the aperture 270 was formed in the combustion chamber during the molding process.
- the combustion chamber enclosure 251 includes raised portions 274 on the outer surface 254, for example, to provide a space between the combustion chamber enclosure 251 and a structure into which the combustion chamber enclosure is eventually inserted.
- the combustion chamber enclosure 251 can also include a design, such as a masonry design 276 formed into at least a portion of the inner surface 256.
- a design such as a masonry design 276 formed into at least a portion of the inner surface 256.
- Figure 2 shows a simulated brick design 276 on the back panel 265 and side panels 260 and 262 of the combustion chamber enclosure.
- the masonry design can also be formed into the bottom panel 258 and top panel 264.
- Other masonry designs include, but are not limited to, stone or concrete.
- the combustion chamber enclosure can be formed without a masonry design, or with other designs.
- Burner Panel Another particular embodiment of an article that can be molded in accordance with the invention is shown in Figs. 13-15.
- a compression molded monolithic gas burner panel 351 is shown.
- the monolithic gas burner panel 351 defines a top surface 354 and a bottom surface 356.
- the top surface 354 defines a raised upper portion 360 and a lower portion 362.
- the raised upper portion 360 is defined by one or more elevated areas 374 and 376, shown for example, in Figures 14 and 15.
- the elevated area or areas 374 and 376 can be formed into any number of generic shapes including, but not limited to, rounded, trapezoid, crescent, or any other desired shape.
- Figures 13-15 show elevated areas of a general trapezoid shape having areas of irregular shape.
- the elevated area is formed into at least one preformed log that includes contours and detail in the top surface of the burner panel that simulates a log.
- the bottom surface 356 defines at least one cavity 364 below at least one of the elevated areas 374 and 376. A portion of at least one cavities 364 extend above at least a portion of the top surface 354, as shown in Figures 14 and 15. In some embodiments, the bottom surface 356 defines a cavity 364 under each of the elevated areas 366. In other embodiments, there can be elevated areas that do not include a cavity there under that extends above the top surface 354.
- the burner panel 351 can be formed as a bottom panel of a combustion chamber enclosure, such as the combustion chamber enclosure shown in Figures 1 A, IB and 2-9. The burner panel 351 can optionally define one or more apertures, for example burner apertures that are formed into the burner panel 351 during the compression molding process. Alternatively, the one or more apertures can be formed into the burner panel after the molding process.
- the burner panel 351 can also include a masonry design 370 formed, for example, into a portion of the lower portion of the top surface.
- Figure 13 shows a simulated brick design on part of the lower portion.
- Other masonry designs include, but are not limited to, stone or concrete.
- the burner panel can be formed without a masonry design, or with another design.
Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP02707754A EP1399395A2 (en) | 2001-02-08 | 2002-01-17 | Compression molded inorganic fiber articles, and methods and compositions used in molding same. |
AU2002242143A AU2002242143B2 (en) | 2001-02-08 | 2002-01-17 | Compression molded inorganic fiber articles, and methods and compositions used in molding same |
JP2002562689A JP2004525055A (en) | 2001-02-08 | 2002-01-17 | Compression molded inorganic fiber products and methods and components used in molding the products |
CA2437191A CA2437191C (en) | 2001-02-08 | 2002-01-17 | Compression molded inorganic fiber articles, and methods and compositions used in molding same |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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US09/781,148 US7098269B2 (en) | 2001-02-08 | 2001-02-08 | Compression molded inorganic fiber articles, and methods and compositions used in molding same |
US09/781,148 | 2001-02-08 |
Publications (2)
Publication Number | Publication Date |
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WO2002062723A2 true WO2002062723A2 (en) | 2002-08-15 |
WO2002062723A3 WO2002062723A3 (en) | 2003-02-06 |
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PCT/US2002/003906 WO2002062723A2 (en) | 2001-02-08 | 2002-01-17 | Compression molded inorganic fiber articles, and methods and compositions used in molding same |
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Country | Link |
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US (4) | US7098269B2 (en) |
EP (1) | EP1399395A2 (en) |
JP (1) | JP2004525055A (en) |
AU (1) | AU2002242143B2 (en) |
CA (1) | CA2437191C (en) |
WO (1) | WO2002062723A2 (en) |
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US7470729B2 (en) | 2001-02-08 | 2008-12-30 | Hni Technologies Inc. | Compression molded inorganic fiber articles, and methods and compositions used in molding same |
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- 2002-01-17 CA CA2437191A patent/CA2437191C/en not_active Expired - Fee Related
- 2002-01-17 JP JP2002562689A patent/JP2004525055A/en active Pending
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- 2002-01-17 EP EP02707754A patent/EP1399395A2/en not_active Withdrawn
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2005
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7470729B2 (en) | 2001-02-08 | 2008-12-30 | Hni Technologies Inc. | Compression molded inorganic fiber articles, and methods and compositions used in molding same |
Also Published As
Publication number | Publication date |
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EP1399395A2 (en) | 2004-03-24 |
CA2437191C (en) | 2012-03-20 |
US20050165160A1 (en) | 2005-07-28 |
CA2437191A1 (en) | 2002-08-15 |
JP2004525055A (en) | 2004-08-19 |
US7470729B2 (en) | 2008-12-30 |
AU2002242143B2 (en) | 2008-01-03 |
WO2002062723A3 (en) | 2003-02-06 |
US20030039933A1 (en) | 2003-02-27 |
US7098269B2 (en) | 2006-08-29 |
US20050119397A1 (en) | 2005-06-02 |
US20030049575A1 (en) | 2003-03-13 |
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