WO2001093292A1 - Catalytically grown carbon fiber field emitters and field emitter cathodes made therefrom - Google Patents
Catalytically grown carbon fiber field emitters and field emitter cathodes made therefrom Download PDFInfo
- Publication number
- WO2001093292A1 WO2001093292A1 PCT/US2001/016420 US0116420W WO0193292A1 WO 2001093292 A1 WO2001093292 A1 WO 2001093292A1 US 0116420 W US0116420 W US 0116420W WO 0193292 A1 WO0193292 A1 WO 0193292A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- field emitter
- carbon fibers
- field
- carbon
- paste
- Prior art date
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J1/00—Details of electrodes, of magnetic control means, of screens, or of the mounting or spacing thereof, common to two or more basic types of discharge tubes or lamps
- H01J1/02—Main electrodes
- H01J1/30—Cold cathodes, e.g. field-emissive cathode
- H01J1/304—Field-emissive cathodes
Definitions
- This invention relates to the use of carbon fibers grown from the catalytic decomposition of carbon-containing gases over small metal particles as an electron field emitter and particularly to their use in a field emitter cathode in display screens.
- Field emission electron sources often referred to as field emission materials or field.emitters, can be used in a variety of electronic applications, e.g., vacuum electronic devices, flat panel computer and television displays, emission gate amplifiers, and klystrons and in lighting.
- Display screens are used in a wide variety of applications such as home and commercial televisions, laptop and desktop computers and indoor and outdoor advertising and information presentations.
- Flat panel displays are only a few inches thick in contrast to the deep cathode ray tube monitors found on most televisions and desktop computers.
- Flat panel displays are a necessity for laptop computers, but also provide advantages in weight and size for many of the other applications.
- Currently laptop computer flat panel displays use liquid crystals, which can be switched from a transparent state to an opaque one by the application of small electrical signals. It is difficult to reliably produce these displays in sizes larger than that suitable for laptop computers.
- Plasma displays have been proposed as an alternative to liquid crystal displays.
- a plasma display uses tiny pixel cells of electrically charged gases to produce an image and requires relatively large electrical power to operate.
- A-tubelites Two types of tube-like molecules are formed; the A-tubelites whose structure includes single-layer graphite-like tubules forming filaments-bundles 10-30 nm in diameter and the B-tubelites, including mostly multilayer graphite-like tubes 10-30 nm in diameter with conoid or dome-like caps. They report considerable field electron emission from the surface of these structures and attribute it to the high concentration of the field at the nanodimensional tips.
- B. H. Fishbine et al., Mat. Res. Soc. Symp. Proc. Vol. 359, 93 (1995) discuss experiments and theory directed towards the development of a buckytube (i.e., a carbon nanotube) cold field emitter array cathode.
- This invention provides an electron field emitter comprised of carbon fibers grown from the catalytic decomposition of carbon-containing gases over small metal particles.
- Each carbon fibers has graphene platelets arranged at an angle with respect to the fiber axis so that the periphery of the carbon fiber consists essentially of the edges of the graphene platelets.
- This invention also provides a field emitter cathode comprised of catalytically grown carbon fibers, i.e., carbon fibers grown from the catalytic decomposition of carbon-containing gases over small metal particles, attached to the surface of a substrate.
- field emitters and field emitter cathodes are useful in flat panel computer, television and other types of displays, vacuum electronic devices, emission gate amplifiers, klystrons and in lighting devices.
- the flat panel displays can be planar or curved.
- This invention provides a novel electron field emitter, carbon fibers grown from the catalytic decomposition of carbon-containing gases over small metal particles, and an electron field emitter cathode comprised of these catalytically grown carbon fibers.
- These carbon fibers can be made as described in N. M. Rodriguez et al., J. Catal. 144, 93 (1993) and N. M. Rodriguez, J. Mater, Res. 8, 3233 (1993). Briefly, the powdered metal catalyst is reduced in a 10% hydrogen-helium stream at 600°C and then brought to the desired reaction temperature. A pre-determined mixture of hydrogen, hydrocarbon and inert gas is introduced into the system and the reaction proceeds. For example, a CO-H2 (4:1) mixture can be reacted over iron at 600°C.
- catalytically grown carbon fibers means carbon fibers grown from the catalytic decomposition of carbon-containing gases over small metal particles, each of which carbon fibers has graphene platelets arranged at an angle with respect to the fiber axis so that the periphery of the carbon fiber consists essentially of the edges of the graphene platelets.
- the angle may be an acute angle or 90°.
- the catalytically grown carbon fibers are good electron filed emitters and are most useful as a electron field emitter cathode when attached to a substrate.
- Various processes can be used to attach catalytically grown carbon fibers to a substrate.
- the means of attachment must withstand and maintain its integrity under the conditions of manufacturing the apparatus into which the field emitter cathode is placed and under the conditions surrounding its use, e.g., typically vacuum conditions and temperatures up to about 450°C.
- organic materials are not generally applicable for attaching the particles to the substrate and the poor adhesion of many inorganic materials to carbon further limits the choice of materials that can be used.
- a preferred method is to screen print a paste comprised of catalytically grown carbon fibers and glass frit, metallic powder or metallic paint or a mixture thereof onto a substrate in the desired pattern and to then fire the dried patterned paste.
- the preferred process comprises screen printing a paste which further comprises a photoinitiator and a photohardenable monomer, photopatterning the dried paste and firing the patterned paste.
- the substrate can be any material to which the paste composition will adhere.
- the paste is non-conducting and a non-conducting substrate is used, a film of an electrical conductor to serve as the cathode electrode and provide means to apply a voltage to and supply electrons to the catalytically grown carbon fibers will be needed.
- Silicon, a glass, a metal or a refractory material such as alumina can serve as the substrate.
- the preferable substrate is glass and soda lime glass is especially preferred.
- silver paste can be pre-fired onto the glass at 500-550°C in air or nitrogen. The conducting layer so-formed can then be over-printed with the emitter paste.
- the emitter paste used for screen printing typically contains catalytically grown carbon fibers, an organic medium, solvent, surfactant and either low softening point glass frit, metallic powder or metallic paint or a mixture thereof.
- the role of the medium and solvent is to suspend and disperse the particulate constituents, i.e., the solids, in the paste with a proper rheology for typical patterning processes such as screen printing.
- resins that can be used are cellulosic resins such as ethyl cellulose and alkyd resins of various molecular weights.
- Butyl carbitol, butyl carbitol acetate, dibutyl carbitol, dibutyl phthalate and terpineol are examples of useful solvents. These and other solvents are formulated to obtain the desired viscosity and volatility requirements.
- a surfactant can be used to improve the dispersion of the particles. Organic acids such oleic and stearic acids and organic phosphates such as lecithin or Gafac® phosphates are typical surfactants.
- a glass frit that softens sufficiently at the firing temperature to adhere to the substrate and to the catalytically grown carbon fibers is required.
- a lead glass frit can be used as well as other glasses with low softening points such as calcium or zinc borosilicates.
- the paste also contains a metal, for example, silver or gold.
- the paste typically contains about 40 wt % to about 60 wt % solids based on the total weight of the paste. These solids comprise catalytically grown carbon fibers and glass frit and/or metallic components. Variations in the composition can be used to adjust the viscosity and the final thickness of the printed material.
- the emitter paste is typically prepared by milling a mixture of catalytically grown carbon fibers, organic medium, surfactant, a solvent and and either low softening point glass frit, metallic powder or metallic paint or a mixture thereof.
- the paste mixture can be screen printed using well-known screen printing techniques, e.g., by using a 165-400-mesh stainless steel screen.
- the paste can be deposited as a continuous film or in the form of a desired pattern.
- the paste is then fired at a temperature of about 350°C to about 500°C, preferably at about 450°C, for about 10 minutes in nitrogen. Higher firing temperatures can be used with substrates which can endure them provided the atmosphere is free of oxygen.
- the organic constituents in the paste are effectively volatilized at 350-450°C, leaving the layer of composite comprised of catalytically grown carbon fibers and glass and/or metallic conductor.
- the catalytically grown carbon fibers undergo no appreciable oxidation or other chemical or physical change during the firing in nitrogen.
- the paste contains a photoinitiator and a photohardenable monomer comprised, for example, of at least one addition polymerizable ethylenically unsaturated compound having at least one polymerizable ethylenic group.
- the cathode consists of a copper block mounted in a polytetrafiuoroethylene (PTFE) holder.
- the copper block is recessed in a 1 inch by 1 inch (2.5 cm x 2.5 cm) area of PTFE and the sample substrate is mounted to the copper block with electrical contact being made between the copper block and the sample substrate by means of copper tape.
- a high voltage lead is attached to the copper block.
- the anode is held parallel to the sample at a distance, which can be varied, but once chosen it was held fixed for a given set of measurements on a sample.
- the anode consists of a glass plate coated with indium tin oxide deposited by chemical vapor deposition. It is then coated with a standard ZnS-based white phosphor, Phosphor P-31, Type 139 obtained from
- An electrode is attached to the indium tin oxide coating.
- test apparatus is inserted into a vacuum system, and the system was evacuated to a base pressure below 1 x 10" 6 torr (1.3 x 10" 4 Pa). A negative voltage was applied to the cathode and the emission current was measured as a function of the applied voltage.
- Catalytically grown carbon fibers were obtained as a powder from Catalytic Materials Ltd, 12 Old Stable Drive, Mansfield, MA. 0.1513 grams of these catalytically grown carbon fibers were added to 0.1502 grams of glass, Bayer PK 8701 (CAS Registry No. 65997-18-4), and 1.5012 grams of a typical organic medium composed primarily of ethylcellulose in terpineol. These ingredients were mixed on a glass plate muller for 75 rotations to form the emitter paste.
- a pre-fired silvered glass substrate was prepared by screen printing a mixture of silver powder and a low melting glass frit in a typical organic ethylcellulose-based medium, followed by firing at 525°C.
- the 1 cm 2 square pattern of emitter paste was then screen printed onto the pre-fired silvered glass substrate using a 325 mesh screen and the sample was subsequently dried at 120°C for 10 minutes. The dried sample was then fired in nitrogen for 10 minutes at 450°C. After firing the paste forms an adherent coating on the substrate. The fired sample was tested for field emission as described in the specification. The emission current was in excess of 10 ⁇ 9 amp at an applied voltage of 4500 V.
Landscapes
- Cold Cathode And The Manufacture (AREA)
- Carbon And Carbon Compounds (AREA)
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2002500415A JP2004519066A (ja) | 2000-05-26 | 2001-05-22 | 触媒的に成長させた炭素繊維フィールドエミッターおよびそれから作製されたフィールドエミッターカソード |
EP01939226A EP1285450A1 (en) | 2000-05-26 | 2001-05-22 | Catalytically grown carbon fiber field emitters and field emitter cathodes made therefrom |
US10/258,252 US20030222560A1 (en) | 2001-05-22 | 2001-05-22 | Catalytically grown carbon fiber field emitters and field emitter cathodes made therefrom |
AU2001264766A AU2001264766A1 (en) | 2000-05-26 | 2001-05-22 | Catalytically grown carbon fiber field emitters and field emitter cathodes made therefrom |
CN01809733A CN1465086A (zh) | 2000-05-26 | 2001-05-22 | 催化生成的碳纤维场致发射体和由此制得的场致发射体阴极 |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US20771700P | 2000-05-26 | 2000-05-26 | |
US60/207,717 | 2000-05-26 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2001093292A1 true WO2001093292A1 (en) | 2001-12-06 |
Family
ID=22771709
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US2001/016420 WO2001093292A1 (en) | 2000-05-26 | 2001-05-22 | Catalytically grown carbon fiber field emitters and field emitter cathodes made therefrom |
Country Status (6)
Country | Link |
---|---|
EP (1) | EP1285450A1 (ko) |
JP (1) | JP2004519066A (ko) |
KR (1) | KR20030047888A (ko) |
CN (1) | CN1465086A (ko) |
AU (1) | AU2001264766A1 (ko) |
WO (1) | WO2001093292A1 (ko) |
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1244129A2 (en) * | 2001-03-21 | 2002-09-25 | GSI Creos Corporation | Carbon fiber for field electron emitter and method for manufacturing field electron emitter |
EP1187161A3 (en) * | 2000-09-01 | 2003-04-16 | Canon Kabushiki Kaisha | Electron-emitting device, electron-emitting apparatus, image display apparatus, and light-emitting apparatus |
US6843696B2 (en) | 2001-09-10 | 2005-01-18 | Canon Kabushiki Kaisha | Method of producing fiber, and methods of producing electron-emitting device, electron source, and image display device each using the fiber |
US6933664B2 (en) | 2000-05-30 | 2005-08-23 | Canon Kabushiki Kaisha | Electron emitting device, electron source, and image forming apparatus |
US7074380B2 (en) | 2002-09-26 | 2006-07-11 | Canon Kabushiki Kaisha | Method for manufacturing carbon fibers and electron emitting device using the same |
US7094123B2 (en) | 2001-09-10 | 2006-08-22 | Canon Kabushiki Kaisha | Method of manufacturing an electron emitting device with carbon nanotubes |
US7147533B2 (en) | 2002-09-26 | 2006-12-12 | Canon Kabushiki Kaisha | Method of producing electron emitting device using carbon fiber, electron source and image forming apparatus, and ink for producing carbon fiber |
US7276844B2 (en) | 2001-06-15 | 2007-10-02 | E. I. Du Pont De Nemours And Company | Process for improving the emission of electron field emitters |
US7449081B2 (en) | 2000-06-21 | 2008-11-11 | E. I. Du Pont De Nemours And Company | Process for improving the emission of electron field emitters |
US7819718B2 (en) | 2001-03-27 | 2010-10-26 | Canon Kabushiki Kaisha | Electronic device having catalyst used to form carbon fiber according to Raman spectrum characteristics |
US11778717B2 (en) | 2020-06-30 | 2023-10-03 | VEC Imaging GmbH & Co. KG | X-ray source with multiple grids |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP3880595B2 (ja) * | 2000-09-01 | 2007-02-14 | キヤノン株式会社 | 電子放出素子の製造方法、画像表示装置の製造方法 |
JP4382311B2 (ja) * | 2001-03-21 | 2009-12-09 | 守信 遠藤 | 気相成長法による炭素繊維の製造方法 |
KR101142525B1 (ko) * | 2011-03-17 | 2012-05-07 | 한국전기연구원 | 그래핀을 이용한 플렉시블 디스플레이의 제조방법 그리고 이를 이용한 디스플레이 |
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EP0913508A2 (en) * | 1997-10-30 | 1999-05-06 | Canon Kabushiki Kaisha | Carbon nanotube device, manufacturing method of carbon nanotube device, and electron emitting device |
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2001
- 2001-05-22 KR KR1020027015953A patent/KR20030047888A/ko not_active Application Discontinuation
- 2001-05-22 JP JP2002500415A patent/JP2004519066A/ja active Pending
- 2001-05-22 WO PCT/US2001/016420 patent/WO2001093292A1/en not_active Application Discontinuation
- 2001-05-22 AU AU2001264766A patent/AU2001264766A1/en not_active Abandoned
- 2001-05-22 CN CN01809733A patent/CN1465086A/zh active Pending
- 2001-05-22 EP EP01939226A patent/EP1285450A1/en not_active Withdrawn
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EP0913508A2 (en) * | 1997-10-30 | 1999-05-06 | Canon Kabushiki Kaisha | Carbon nanotube device, manufacturing method of carbon nanotube device, and electron emitting device |
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Cited By (20)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6933664B2 (en) | 2000-05-30 | 2005-08-23 | Canon Kabushiki Kaisha | Electron emitting device, electron source, and image forming apparatus |
US7449081B2 (en) | 2000-06-21 | 2008-11-11 | E. I. Du Pont De Nemours And Company | Process for improving the emission of electron field emitters |
US8529798B2 (en) | 2000-06-21 | 2013-09-10 | E I Du Pont De Nemours And Company | Process for improving the emission of electron field emitters |
US8070906B2 (en) | 2000-06-21 | 2011-12-06 | E. I. Du Pont De Nemours And Company | Process for improving the emission of electron field emitters |
US7449082B2 (en) | 2000-06-21 | 2008-11-11 | E.I. Du Pont De Nemours And Company | Process for improving the emissions of electron field emitters |
EP1187161A3 (en) * | 2000-09-01 | 2003-04-16 | Canon Kabushiki Kaisha | Electron-emitting device, electron-emitting apparatus, image display apparatus, and light-emitting apparatus |
CN1314066C (zh) * | 2001-03-21 | 2007-05-02 | 株式会社科立思 | 电场电子发射体用碳素纤维及电场电子发射体的制造方法 |
EP1244129A3 (en) * | 2001-03-21 | 2004-12-29 | GSI Creos Corporation | Carbon fiber for field electron emitter and method for manufacturing field electron emitter |
EP1244129A2 (en) * | 2001-03-21 | 2002-09-25 | GSI Creos Corporation | Carbon fiber for field electron emitter and method for manufacturing field electron emitter |
US7018602B2 (en) | 2001-03-21 | 2006-03-28 | Gsi Creos Corporation | Carbon fiber for field electron emitter and method for manufacturing field electron emitter |
US7819718B2 (en) | 2001-03-27 | 2010-10-26 | Canon Kabushiki Kaisha | Electronic device having catalyst used to form carbon fiber according to Raman spectrum characteristics |
US7276844B2 (en) | 2001-06-15 | 2007-10-02 | E. I. Du Pont De Nemours And Company | Process for improving the emission of electron field emitters |
US6843696B2 (en) | 2001-09-10 | 2005-01-18 | Canon Kabushiki Kaisha | Method of producing fiber, and methods of producing electron-emitting device, electron source, and image display device each using the fiber |
US7131886B2 (en) | 2001-09-10 | 2006-11-07 | Canon Kabushiki Kaisha | Method of producing fiber, and methods of producing electron-emitting device, electron source, and image display device each using the fiber |
US7258590B2 (en) | 2001-09-10 | 2007-08-21 | Canon Kabushiki Kaisha | Electron emitting device using carbon fiber; electron source; image display device; method of manufacturing the electron emitting device; method of manufacturing electron source using the electron emitting device; and method of manufacturing image display device |
US7094123B2 (en) | 2001-09-10 | 2006-08-22 | Canon Kabushiki Kaisha | Method of manufacturing an electron emitting device with carbon nanotubes |
US7074380B2 (en) | 2002-09-26 | 2006-07-11 | Canon Kabushiki Kaisha | Method for manufacturing carbon fibers and electron emitting device using the same |
US7923058B2 (en) | 2002-09-26 | 2011-04-12 | Canon Kabushiki Kaisha | Method for manufacturing carbon fibers and method for manufacturing electron emitting device using the same, method for manufacturing display, and ink for producing catalyst for use in these methods |
US7147533B2 (en) | 2002-09-26 | 2006-12-12 | Canon Kabushiki Kaisha | Method of producing electron emitting device using carbon fiber, electron source and image forming apparatus, and ink for producing carbon fiber |
US11778717B2 (en) | 2020-06-30 | 2023-10-03 | VEC Imaging GmbH & Co. KG | X-ray source with multiple grids |
Also Published As
Publication number | Publication date |
---|---|
JP2004519066A (ja) | 2004-06-24 |
KR20030047888A (ko) | 2003-06-18 |
EP1285450A1 (en) | 2003-02-26 |
AU2001264766A1 (en) | 2001-12-11 |
CN1465086A (zh) | 2003-12-31 |
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