USH721H - Production of 10 micron diameter hollow ceramic fibers - Google Patents
Production of 10 micron diameter hollow ceramic fibers Download PDFInfo
- Publication number
- USH721H USH721H US07/220,136 US22013688A USH721H US H721 H USH721 H US H721H US 22013688 A US22013688 A US 22013688A US H721 H USH721 H US H721H
- Authority
- US
- United States
- Prior art keywords
- fiber
- fibers
- carbon
- hollow
- alumina
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Abandoned
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 79
- 239000000919 ceramic Substances 0.000 title claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 title description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 15
- 239000004917 carbon fiber Substances 0.000 claims abstract description 15
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004327 boric acid Substances 0.000 claims abstract description 12
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 12
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 4
- 238000009830 intercalation Methods 0.000 claims abstract description 4
- 229910001510 metal chloride Inorganic materials 0.000 claims abstract description 3
- 239000002243 precursor Substances 0.000 claims abstract 3
- 238000000034 method Methods 0.000 claims description 22
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 16
- 238000005245 sintering Methods 0.000 claims description 11
- 238000002791 soaking Methods 0.000 claims description 7
- 238000003303 reheating Methods 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 description 8
- 239000010439 graphite Substances 0.000 description 8
- 229910018404 Al2 O3 Inorganic materials 0.000 description 7
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 5
- 229910003887 H3 BO3 Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000012510 hollow fiber Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005297 pyrex Substances 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
Classifications
-
- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
- C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
- C04B35/62236—Fibres based on aluminium oxide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/08—Hollow fibre membranes
-
- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
-
- 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
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
Definitions
- the invention relates generally to a process for making hollow ceramic fibers, and more specifically to a process for making hollow alumina fibers from intercalated graphite fibers.
- the present invention provides a novel process for making hollow metal oxide fibers.
- the unique discovery of the present invention is that soaking low density alumina fibers, which may be made according to the teachings of the referenced co-pending applications, in a boric acid solution, then briefly drying the fibers and heating at a high temperature yields hollow alumina fibers.
- the invention is directed to a method for making a hollow ceramic fiber, comprising the steps of providing a low density alumina fiber, soaking the alumina fiber in a sintering aide and reheating the fiber.
- the alumina fiber may be gamma alumina and the sintering aid may be boric acid.
- the invention is also directed to a method for making a hollow ceramic fiber, comprising the steps of providing a carbon fiber, intercalating a metal chloride inside the carbon fiber, heating the intercalated carbon fiber in air to oxidize the carbon and leave a metal oxide fiber having generally the size and structure of the previous carbon fiber, followed by soaking the metal oxide fiber in a sintering aide and reheating the fiber.
- Aluminum chloride may be used to make the intercalated carbon fiber and boric acid may be used as the sintering aid.
- the invention additionally includes heating the boric acid soaked fiber to a temperature about 1250° C. to convert the soaked fiber to a tube.
- the invention also includes heating the boric acid soaked fiber to a temperature about 800° C. to convert the soaked fiber to a flattened tube.
- the invention also includes a hollow ceramic fiber and a hollow alumina fiber made according to the disclosed methods.
- Aluminum chloride (AlCl 3 ) is first intercalated into graphite fibers by standard techniques well known in the art. For example, to intercalate (AlCl 3 ) into tows of Union Carbide P-100 fiber, the fibers are heated at ⁇ 300° C. in air to remove any sizing. The fibers are then placed inside a Pyrex tube to which the aluminum chloride and chlorine gas (Cl 2 ) are added. The Cl 2 is frozen in the tube and the tube sealed under vacuum. The sample is next heated to generate a sufficient vapor pressure of aluminum chloride. After 1-3 days, the tube is cooled and opened in a drybox. The added AlCl 3 and Cl 2 will generally be sufficient to produce C n + AlCl 4 - (n ⁇ 36) in-between the crystalline layers comprising the graphite fibers.
- AlCl 3 and Cl 2 will generally be sufficient to produce C n + AlCl 4 - (n ⁇ 36) in-between the crystalline layers comprising the graphite
- the intercalated fibers are then heated in air to 800° C. Within 1-3 hours, all the graphite burns off leaving a light and flexible oxide fiber tow.
- the individual fibers are visibly similar to the original P-100 fibers, including having a layered metal oxide microstructure along the previous layer planes.
- X-ray diffraction shows the fibers to be gamma alumina ( ⁇ -Al 2 O 3 ), with no obvious preferred orientation.
- the fiber has a lower than expected density, ⁇ 0.6 g/cc compared to ⁇ 3.9 g/cc for a fully dense material. This loss of density, or porosity, is assumed to be due to escaping CO 2 and Cl 2 as the graphite fiber is oxidized at 800° C.
- the hollow fibers are ellipsoidal, with major and minor axis of 5 and 10 ⁇ m respectively.
- the wall thickness is 1-2 ⁇ m.
- the tubes appear hollow for long distances (>100 ⁇ m). Some of the fibers are cracked open far from the points of fracture and some have holes in their walls. X-ray diffraction of hollow tubes produced by this process indicates only alpha Al 2 O 3 , with the same preferred orientation as the merely reheated fibers described in applicant's cross-referenced companion application.
- Gamma Al 2 O 3 fibers dipped in 10 -2 M H 3 BO 3 and heated to 1250° C. have the same hollow structure and Al 2 O 3 pattern as those treated with 10 -3 M H 3 BO 3 .
- Gamma Al 2 O 3 dipped in 10 -2 M H 3 BO 3 and heated to 800° C. assumes the shape of very flattened tubes. The reasons for the different morphologies with different heat treatments are unclear.
- the disclosed process successfully demonstrates making hollow alumina tubes from alumina fibers. Although the disclosed process is specialized, extension of its underlying methodology will find application in other areas where specially shaped fibers and other materials are desired. Other low density fibers, such as those taught in the cross-referenced companion applications, may be similarly densified to produce hollow fibers.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Fibers (AREA)
Abstract
Hollow ceramic fibers are made by intercalating carbon fibers with a metal chloride and then heating the intercalated fibers in air to oxidize or burn off the carbon, leaving metal oxide fibers having generally the size and structure of the carbon fiber precursors. The fibers are then soaked in boric acid solution, briefly dried and heated at a high temperature to make hollow alumina fibers. The temperatures at which the boric acid soaked fibers are heated can be varied to produce different tube morphologies.
Description
The invention described herein may be manufactured and used by or for the Government of the United States for all governmental purposes without the payment of any royalty.
This application relates to two companion applications titled PROCESS FOR MAKING COATINGS ON GRAPHITE USING INTERCALATED SPECIES, application Ser. No. 07/220,135, now U.S. Statutory Invention Registration H614, and PREPARATION OF METAL OXIDE FIBERS FROM INTERCALATED GRAPHITE FIBERS, U.S. application Ser. No. 07/217,991, both filed on the same date as this application and hereby incorporated by reference as if fully rewritten herein.
The invention relates generally to a process for making hollow ceramic fibers, and more specifically to a process for making hollow alumina fibers from intercalated graphite fibers.
Processes for making hollow ceramic fibers are not well known in the prior art. Such fibers will, however, by very valuable in such applications as ceramic capillaries, wicks in heat pipes, gas diffusion separators, high temperature filters and battery compartment separators. Combining the traditional high heat resistance and high modulus of elasticity of ceramic fibers with a hollow configuration will stimulate those in the art to develop a variety of many other new and valuable uses for these fibers.
It is, therefore, a principal object of the present invention to provide a process for making hollow metal oxide fibers.
It is an advantage of the present invention that the process is simple to understand and to perform.
In accordance with the foregoing principles, objects and advantages the present invention provides a novel process for making hollow metal oxide fibers. The unique discovery of the present invention is that soaking low density alumina fibers, which may be made according to the teachings of the referenced co-pending applications, in a boric acid solution, then briefly drying the fibers and heating at a high temperature yields hollow alumina fibers.
Accordingly, the invention is directed to a method for making a hollow ceramic fiber, comprising the steps of providing a low density alumina fiber, soaking the alumina fiber in a sintering aide and reheating the fiber. The alumina fiber may be gamma alumina and the sintering aid may be boric acid.
The invention is also directed to a method for making a hollow ceramic fiber, comprising the steps of providing a carbon fiber, intercalating a metal chloride inside the carbon fiber, heating the intercalated carbon fiber in air to oxidize the carbon and leave a metal oxide fiber having generally the size and structure of the previous carbon fiber, followed by soaking the metal oxide fiber in a sintering aide and reheating the fiber. Aluminum chloride may be used to make the intercalated carbon fiber and boric acid may be used as the sintering aid.
The invention additionally includes heating the boric acid soaked fiber to a temperature about 1250° C. to convert the soaked fiber to a tube.
The invention also includes heating the boric acid soaked fiber to a temperature about 800° C. to convert the soaked fiber to a flattened tube.
The invention also includes a hollow ceramic fiber and a hollow alumina fiber made according to the disclosed methods.
Aluminum chloride (AlCl3) is first intercalated into graphite fibers by standard techniques well known in the art. For example, to intercalate (AlCl3) into tows of Union Carbide P-100 fiber, the fibers are heated at ˜300° C. in air to remove any sizing. The fibers are then placed inside a Pyrex tube to which the aluminum chloride and chlorine gas (Cl2) are added. The Cl2 is frozen in the tube and the tube sealed under vacuum. The sample is next heated to generate a sufficient vapor pressure of aluminum chloride. After 1-3 days, the tube is cooled and opened in a drybox. The added AlCl3 and Cl2 will generally be sufficient to produce Cn + AlCl4 - (n˜36) in-between the crystalline layers comprising the graphite fibers.
The intercalated fibers are then heated in air to 800° C. Within 1-3 hours, all the graphite burns off leaving a light and flexible oxide fiber tow. The individual fibers are visibly similar to the original P-100 fibers, including having a layered metal oxide microstructure along the previous layer planes. X-ray diffraction shows the fibers to be gamma alumina (γ-Al2 O3), with no obvious preferred orientation. The fiber has a lower than expected density, ˜0.6 g/cc compared to ˜3.9 g/cc for a fully dense material. This loss of density, or porosity, is assumed to be due to escaping CO2 and Cl2 as the graphite fiber is oxidized at 800° C.
Cross-referenced companion application Ser. No. 07/217,991, Preparation of Metal Oxide Fibers from Intercalated Graphite Fibers, describes densifying the fibers by heating to achieve a phase change. Another means for densifying materials is sintering. Applicants have discovered that, surprisingly, using boric acid as a sintering aide to densify thus made alumina fibers results in the production of alumina tubes. Soaking the gamma Al2 O3 tows in 10-3 M H3 BO3 for ˜12 hours, briefly drying at 150° C. and then heating the tows to 1250° C. for ˜12 hours converts the gamma fibers to alpha Al2 O3 tubes. The hollow fibers are ellipsoidal, with major and minor axis of 5 and 10 μm respectively. The wall thickness is 1-2 μm. The tubes appear hollow for long distances (>100 μm). Some of the fibers are cracked open far from the points of fracture and some have holes in their walls. X-ray diffraction of hollow tubes produced by this process indicates only alpha Al2 O3, with the same preferred orientation as the merely reheated fibers described in applicant's cross-referenced companion application.
Gamma Al2 O3 fibers dipped in 10-2 M H3 BO3 and heated to 1250° C. have the same hollow structure and Al2 O3 pattern as those treated with 10-3 M H3 BO3. Gamma Al2 O3 dipped in 10-2 M H3 BO3 and heated to 800° C. assumes the shape of very flattened tubes. The reasons for the different morphologies with different heat treatments are unclear.
Those with skill in the art will also see that further experimentation with different pressures and temperatures will lead to a variety of other morphologies and structures.
The disclosed process successfully demonstrates making hollow alumina tubes from alumina fibers. Although the disclosed process is specialized, extension of its underlying methodology will find application in other areas where specially shaped fibers and other materials are desired. Other low density fibers, such as those taught in the cross-referenced companion applications, may be similarly densified to produce hollow fibers.
It is understood that other modifications to the invention as described may be made, as might occur to one with skill in the field of the invention. Therefore, all embodiments contemplated have not been shown in complete detail. Other embodiments may be developed without departing from the spirit of the invention or from the scope of the claims.
Claims (8)
1. A method for making a hollow ceramic fiber, comprising the steps of:
(a) providing a low density ceramic fiber;
(b) soaking the ceramic fiber in a sintering aide; and,
(c) heating the fiber to make a hollow ceramic fiber.
2. The method according to claim 1, wherein the ceramic fiber is gamma alumina.
3. The method according to claim 1, wherein the sintering aid is boric acid.
4. A method for making a hollow metal oxide fiber, comprising the steps of:
(a) providing a graphitic carbon fiber;
(b) intercalating a metal chloride inside the carbon fiber;
(c) heating the intercalated carbon fiber to oxidize the carbon and leave a low density metal oxide fiber having generally the size and structure of the carbon fiber precursor;
(d) soaking the metal oxide fiber in a sintering aide; and,
(e) reheating the fiber to make a hollow metal oxide fiber.
5. A method for making a hollow alumina fiber, comprising the steps of:
(a) providing a carbon fiber;
(b) intercalating aluminum chloride inside the carbon fiber;
(c) heating the intercalated carbon fiber to oxidize the carbon and leave a low density alumina fiber having generally the size and structure of the carbon fiber precursor;
(d) soaking the alumina fiber in a sintering aide; and
(e) reheating the fiber to make a hollow alumina oxide fiber.
6. The method according to claim 5, wherein the sintering aid is boric acid.
7. The method according to claim 6, wherein the boric acid soaked fiber is heated to a temperature about 1250° C. to convert the soaked fiber to a tube.
8. The method according to claim 6, wherein the boric acid soaked fiber is heated to a temperature about 800° C. to convert the soaked fiber to a flattened tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US07/220,136 USH721H (en) | 1988-07-05 | 1988-07-05 | Production of 10 micron diameter hollow ceramic fibers |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US07/220,136 USH721H (en) | 1988-07-05 | 1988-07-05 | Production of 10 micron diameter hollow ceramic fibers |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| USH721H true USH721H (en) | 1990-01-02 |
Family
ID=22822223
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US07/220,136 Abandoned USH721H (en) | 1988-07-05 | 1988-07-05 | Production of 10 micron diameter hollow ceramic fibers |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | USH721H (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4948763A (en) | 1988-06-30 | 1990-08-14 | Shin-Etsu Chemical Co., Ltd. | Preparation of hollow ceramic fibers |
| US5774779A (en) * | 1996-11-06 | 1998-06-30 | Materials And Electrochemical Research (Mer) Corporation | Multi-channel structures and processes for making such structures |
| US6368713B1 (en) * | 1997-07-18 | 2002-04-09 | Japan Science And Technology Corporation | Hollow microfibers and process for producing the same |
| US6573208B1 (en) * | 1998-03-20 | 2003-06-03 | Societe Des Ceramiques Techniques | Homogeneous bulky porous ceramic material |
Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3385915A (en) | 1966-09-02 | 1968-05-28 | Union Carbide Corp | Process for producing metal oxide fibers, textiles and shapes |
| US3760049A (en) | 1971-03-01 | 1973-09-18 | Minnesota Mining & Mfg | Method of firing dry spun refractory oxide fibers |
| US3795524A (en) | 1971-03-01 | 1974-03-05 | Minnesota Mining & Mfg | Aluminum borate and aluminum borosilicate articles |
| US3950478A (en) | 1972-03-15 | 1976-04-13 | Imperial Chemical Industries Limited | Process for producing alumina fiber |
| US3982955A (en) | 1971-12-22 | 1976-09-28 | Bayer Aktiengesellschaft | Aluminum oxide fibers and their production |
| US4047965A (en) | 1976-05-04 | 1977-09-13 | Minnesota Mining And Manufacturing Company | Non-frangible alumina-silica fibers |
| US4102937A (en) | 1976-12-03 | 1978-07-25 | Phillips Petroleum Company | Cycloparaffin isomerization using a catalytically active aluminum halide intercalated in graphite |
| US4110252A (en) | 1976-12-06 | 1978-08-29 | Phillips Petroleum Company | Catalytically active AlCl3 -graphite intercalate |
| US4175153A (en) | 1978-05-16 | 1979-11-20 | Monsanto Company | Inorganic anisotropic hollow fibers |
| US4267211A (en) | 1978-11-13 | 1981-05-12 | The Foundation: The Research Institute For Special Inorganic Materials | Process for producing corrosion-, heat- and oxidation-resistant shaped article |
| US4267210A (en) | 1978-07-28 | 1981-05-12 | The Foundation: The Research Institute For Special Inorganic Materials | Method for producing corrosion-, heat- and oxidation-resistant materials |
| US4268278A (en) | 1978-05-16 | 1981-05-19 | Monsanto Company | Inorganic anisotropic hollow fibers |
| US4440571A (en) | 1981-07-10 | 1984-04-03 | Nippon Carbon Co., Ltd. | Process for the surface treatment of inorganic fibers for reinforcing titanium or nickel and product |
| US4533508A (en) | 1983-08-22 | 1985-08-06 | The Dow Chemical Company | Metal oxide fibers from acrylate salts |
| US4605588A (en) | 1985-03-14 | 1986-08-12 | The Boeing Company | Barrier coated ceramic fiber and coating method |
| US4642271A (en) | 1985-02-11 | 1987-02-10 | The United States Of America As Represented By The Secretary Of The Navy | BN coating of ceramic fibers for ceramic fiber composites |
-
1988
- 1988-07-05 US US07/220,136 patent/USH721H/en not_active Abandoned
Patent Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3385915A (en) | 1966-09-02 | 1968-05-28 | Union Carbide Corp | Process for producing metal oxide fibers, textiles and shapes |
| US3760049A (en) | 1971-03-01 | 1973-09-18 | Minnesota Mining & Mfg | Method of firing dry spun refractory oxide fibers |
| US3795524A (en) | 1971-03-01 | 1974-03-05 | Minnesota Mining & Mfg | Aluminum borate and aluminum borosilicate articles |
| US3982955A (en) | 1971-12-22 | 1976-09-28 | Bayer Aktiengesellschaft | Aluminum oxide fibers and their production |
| US3950478A (en) | 1972-03-15 | 1976-04-13 | Imperial Chemical Industries Limited | Process for producing alumina fiber |
| US4047965A (en) | 1976-05-04 | 1977-09-13 | Minnesota Mining And Manufacturing Company | Non-frangible alumina-silica fibers |
| US4102937A (en) | 1976-12-03 | 1978-07-25 | Phillips Petroleum Company | Cycloparaffin isomerization using a catalytically active aluminum halide intercalated in graphite |
| US4110252A (en) | 1976-12-06 | 1978-08-29 | Phillips Petroleum Company | Catalytically active AlCl3 -graphite intercalate |
| US4175153A (en) | 1978-05-16 | 1979-11-20 | Monsanto Company | Inorganic anisotropic hollow fibers |
| US4268278A (en) | 1978-05-16 | 1981-05-19 | Monsanto Company | Inorganic anisotropic hollow fibers |
| US4267210A (en) | 1978-07-28 | 1981-05-12 | The Foundation: The Research Institute For Special Inorganic Materials | Method for producing corrosion-, heat- and oxidation-resistant materials |
| US4267211A (en) | 1978-11-13 | 1981-05-12 | The Foundation: The Research Institute For Special Inorganic Materials | Process for producing corrosion-, heat- and oxidation-resistant shaped article |
| US4440571A (en) | 1981-07-10 | 1984-04-03 | Nippon Carbon Co., Ltd. | Process for the surface treatment of inorganic fibers for reinforcing titanium or nickel and product |
| US4533508A (en) | 1983-08-22 | 1985-08-06 | The Dow Chemical Company | Metal oxide fibers from acrylate salts |
| US4642271A (en) | 1985-02-11 | 1987-02-10 | The United States Of America As Represented By The Secretary Of The Navy | BN coating of ceramic fibers for ceramic fiber composites |
| US4605588A (en) | 1985-03-14 | 1986-08-12 | The Boeing Company | Barrier coated ceramic fiber and coating method |
Non-Patent Citations (4)
| Title |
|---|
| "Deintercalation Reactions to Form Ceramic Coatings on Graphite Fibers" by B. W. McQuillan and G. H. Reynolds, Abstract, Boston, Mass., Dec. 1986. |
| "Growth of Alumina Fibers from Intercalated Graphite Precursor Fibers" B. W. McQuillan and G. H. Reynolds, Abstract, San Diego, Calif., Jan. 1987. |
| "Preparation of Ceramic Fibers by Conversion Intercalated Graphite Fibers" by B. W. McQuillan and G. H. Reynolds, Abstract, Pittsburgh, Pa., Apr. 1987. |
| "Synthesis of Refractory Ceramic Fibers from Intercalated Graphite Fiber Precursors:" B. W. McQuillan and G. H. Reynolds, Abstract, Apr. 1987. |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4948763A (en) | 1988-06-30 | 1990-08-14 | Shin-Etsu Chemical Co., Ltd. | Preparation of hollow ceramic fibers |
| US5774779A (en) * | 1996-11-06 | 1998-06-30 | Materials And Electrochemical Research (Mer) Corporation | Multi-channel structures and processes for making such structures |
| US6368713B1 (en) * | 1997-07-18 | 2002-04-09 | Japan Science And Technology Corporation | Hollow microfibers and process for producing the same |
| US6573208B1 (en) * | 1998-03-20 | 2003-06-03 | Societe Des Ceramiques Techniques | Homogeneous bulky porous ceramic material |
| US20030166449A1 (en) * | 1998-03-20 | 2003-09-04 | Exekia | Homogeneous bulky porous ceramic material |
| US7199067B2 (en) | 1998-03-20 | 2007-04-03 | Pall Corporation | Homogeneous bulky porous ceramic material |
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