CN101866794A - New application of conductive polyurethane foam plastic of carbon-doped nanotube in vacuum electronic component - Google Patents
New application of conductive polyurethane foam plastic of carbon-doped nanotube in vacuum electronic component Download PDFInfo
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Abstract
The invention belongs to new application of conductive polyurethane foam plastic of a carbon-doped nanotube in a vacuum electronic component. The conductive polyurethane foam plastic is used as a cold cathode of a field emission vacuum electronic component and has a honeycomb cell network structure, wherein the carbon nanotube content is 0.5 to 5.0 percent by weight, and the carbon nanotubes are evenly distributed on the honeycomb wall and in a honeycomb column; the open electric field is not more than 1.2V/mu m under the condition that the emission current density is 10mu A/cm<2>; the threshold electric field is not more than 2.0V/mu m under the condition that the emission current density is 1mu A/cm<2>, and the field enhancement factor can reach 2.5*104. The invention has the characteristics of taking a material for producing an anti-static package material as the cold cathode of the field emission vacuum electronic component, improving the application value and the economic benefit by a large extent, finding the cold cathode material with low price, easy industrial production, excellent performance and large production area for the cold cathode of the field emission vacuum electronic component, simplifying the production process of a nano-graphite planar field emission cathode, effectively improving the production rate, reducing the production cost by a large extent, and the like.
Description
Technical field
The invention belongs to the new purposes of conductive polyurethane foam plastic in vacuum electronic unit, device production field of carbon-doped nanometer tube, particularly a kind of conductive polyurethane foam plastic that will be conventionally used as doping (filling) carbon nano-tube of antistatic packaging material is used as the cold cathode in the field emission vacuum electronic element; Such conductive polyurethane foam plastic can be widely used as the field emission cold-cathode in the flat-panel screens (FED).
Background technology
Traditional microwave vacuum electronic device negative electrode generally adopts the associated materials of tungsten oxide or tungsten to make, and belongs to the hot cathode emission; Traditional used electron emitting cathode of projection tube electron-like device also is to rely on thermionic emission, thereby has the working temperature height and need preheating, and defectives such as volume is big, power consumption height; The employing carbon nanomaterial of developing at these defectives is as the field emission cold-cathode technology, generally prepare, promptly utilize the way of chemical vapor deposition growth system film to obtain the carbon nanometer film, for the field emission cold-cathode of Diagonal Dimension as the field emission electron cold cathode of flat thin membranous type shape by the chemical vapor carbon deposition nanotube less than the small size of 5-in; Though the sub-cold cathode of this type of generating has advantages such as threshold field is lower, current density is bigger, but exist complex manufacturing, production efficiency and output extremely low and be difficult to prepare large tracts of land cold cathode, production cost height, can not form disadvantages such as large-scale industrialized production; Then adopt spraying, ink-jet or print process preparation for the larger area field emission cold-cathode, technology is relatively simple though these class methods have, the relatively low characteristics of production cost, and existing in emission is 10 μ A/cm
2Under the condition, its required unlatching electric field is about 1.7V/ μ m, and is 1mA/cm in emission
2Under the condition, its threshold field is about 2.1V/ μ m, field enhancement factor 5000-8000, disadvantages such as effect difference.
And the conductive polyurethane foam plastic of conventional carbon-doped nanometer tube then as the packaging material to explosive, the fragile goods of electrostatic sensitive, works the mischief to packed article to avoid static.Publication number is CN1970598A, name is called " preparation of hard polyurethane conductive foam plastic for carbon nanotube filling " and publication number is CN101250321A, and the disclosed technology of patent documentation that name is called " preparation of light electric polyurethane foam plastic " just belongs to this type of doped carbon nanometer pipe conductive polyurethane foam plastic method of production.Production technology is simple, production efficiency is high though the conductive polyurethane foam plastic of this type of doped carbon nanometer pipe has, and is extremely low as doped carbon nanotubes consumption few (only needing 0.5-4.0%), production cost, easily realizes characteristics such as large-scale industrialized production; Use defective such as its value and economic benefit are extremely low but exist as packaging material.
Summary of the invention
The objective of the invention is defective at the background technology existence, the new purposes of conductive polyurethane foam plastic in vacuum electronic component of research and development carbon-doped nanometer tube, with routine only as the material of low gear purposes such as Production and Packaging thing, use as the cold-cathode material in the field emission vacuum electronic element, increase substantially the using value and the economic benefit of the conductive polyurethane foam plastic of carbon-doped nanometer tube, and the production technology of simplifying nano-graphite class flat field emitting electrons negative electrode, effectively improve the productivity ratio of nano-graphite class flat field emitting electrons negative electrode, reduce its production cost, realize purposes such as industrialization.
Solution of the present invention be with routine as the conductive polyurethane foam plastic of the carbon-doped nanometer tube of antistatic packaging material as the cold cathode in the field emission vacuum electronic element.The above-mentioned cold cathode that is used as in the field emission vacuum electronic element is the field emission cold-cathode in the flat-panel screens (FED).(percentage by weight) content of carbon nano-tube is 0.5-5.0wt% in the described conductive polyurethane foam plastic cold cathode, and the diameter of carbon nano-tube is Φ 1～40nm, pipe range 0.5～100 μ m.Described conductive polyurethane foam plastic cold cathode is for having honey comb like cellular network structure, and even carbon nanotube is distributed in hard polyurethane conductive foam plastic or the flexibel polyurethane conductive foam plastic in cell walls and the honeycomb post.Described carbon-doped nanometer tube conductive polyurethane foam plastic cold cathode is 10 μ A/cm in emission
2Under the condition, its required unlatching electric field≤1.2V/ μ m, and be 1mA/cm in emission
2Under the condition, its threshold field≤2.0V/ μ m.The production method of the conductive polyurethane foam plastic cold cathode of described carbon-doped nanometer tube comprises:
A. get the raw materials ready: the weight portion with PPG is a benchmark, press 100 parts of PPGs, 0.5～10 part of carbon nano-tube, 10～200 parts of isocyanates, 0.01～1.2 part of deionized water or distilled water (blowing agent), 0.01～1 part of organotin, 0.01～1 part of triethylene diamine, 10～100 parts in 0.1～3 part of silicone oil and potassium permanganate, 100～1000 parts of the concentrated sulfuric acid or red fuming nitric acid (RFNA)s, weighing is stand-by respectively;
B. prepare the mixed liquor of carbon nano-tube and PPG: after the solution (oxidant) that at first adopts the potassium permanganate and the concentrated sulfuric acid or red fuming nitric acid (RFNA) carries out oxidation processes to carbon nano-tube, clean to remove impurity with distilled water, again the carbon nano-tube after the removal of impurities is distributed in deionized water or acetone, the ethanol class polarity non-active solvent, makes the carbon nano-tube mixed liquor; Then that weighing is stand-by PPG adds in this mixed liquor, mix after, place 80～120 ℃ removing non-active solvent, the mixed liquor of gained carbon nano-tube and PPG, the cooling back is stand-by;
C. preparation raw material mixed liquor: organotin that weighing is stand-by and triethylene diamine, silicone oil (stabilizer) and as the deionized water or the distilled water of blowing agent, in the carbon nano-tube that adding is made by step B and the mixed liquor of PPG, stir, make the raw material mixed liquor;
D. polymerization foaming: the isocyanates that weighing is stand-by adds rapidly in the raw material mixed liquor that is made by step C, and brute force stirs after 10～60 seconds, mixed liquor is injected mould and rapid closing die cap, carries out the polymerization foaming and handles;
E. later stage maturation process: will place baking oven in the lump together with mould through the material after the step D polymerization foaming, after 80～120 ℃ of following maturation process 3～5 hours, cooling the conductive polyurethane foam plastic of carbon-doped nanometer tube;
F. section: will cut into slices, promptly get the field emission cold-cathode goods by the specification of field emission cold-cathode requirement by the conductive polyurethane foam plastic of step e gained carbon-doped nanometer tube.
Powerful stirring, its mixing speed are 1000～3000 rev/mins described in the said method.
The present invention only as the carbon-doped nanometer tube conductive polyurethane foam plastic of producing antistatic packaging material, as the cold-cathode material usefulness in the field emission vacuum electronic element, is 10 μ A/cm in emission with routine
2The time, its required unlatching electric field can be low to moderate 0.6v/ μ m, and is 1mA/cm in emission
2The time, its threshold field can be low to moderate 1.2V/ μ m, field enhancement factor can reach 2.5 * 10
4, cost is the greatly amplitude reduction [conductive polyurethane foam plastic of carbon-doped nanometer tube of the present invention (about 2～5m per ton at present, then
3) about 50,000 yuan]; Thereby, the present invention has increased substantially the using value and the economic benefit of carbon-doped nanometer tube conductive polyurethane foam plastic, for the cold cathode in the field emission vacuum electronic element seek and developed a kind of inexpensive, easily realize industrialization production, function admirable and can produce the big field emission cold-cathode material of area, simplified the production technology of nano-graphite class flat field emitting electrons negative electrode, effectively improved nano-graphite class flat field emitting electrons negative electrode productivity ratio, reduced characteristics such as production cost.
Description of drawings
Fig. 1 is embodiment 1 gained (conductive polyurethane foam plastic of carbon-doped nanometer tube) cold cathode goods stereoscan photographs;
Fig. 2 is embodiment 2 gained (conductive polyurethane foam plastic of carbon-doped nanometer tube) cold cathode goods stereoscan photographs;
Fig. 3 is that the current density-electric field strength of embodiment 1, embodiment 2 and embodiment 3 field emission cold-cathode goods concerns coordinate curve contrast schematic diagram.
Embodiment
Embodiment 1: with preparation hard carbon-doped nanometer tube conductive polyurethane foam plastic cold cathode is example:
A. get the raw materials ready: density is the PPG 100ml of 1.1g/ml, carbon nano-tube 5g, density is the isocyanates 140ml of 1.23g/ml, deionized water 1ml, density is the dibutyl tin laurate 0.05ml of 1.05g/ml, density is the triethylene diamine 0.05ml of 1.122g/ml, density is the silicone oil 0.3ml of 0.96g/ml, potassium permanganate 50g, density is the concentrated sulfuric acid 500ml of 1.84g/ml, weighing is stand-by respectively;
B. prepare the mixed liquor of carbon nano-tube and PPG: after the solution (oxidant) that at first adopts potassium permanganate 50g and concentrated sulfuric acid 500ml carries out oxidation processes to carbon nano-tube 5g, clean with deacidification and impurity with deionized water 5000ml, again the carbon nano-tube after the removal of impurities is distributed among the deionized water 500ml, makes the carbon nano-tube mixed liquor; Then that weighing is stand-by PPG 100ml adds in this mixed liquor, mix after, place 110 ℃ removing moisture content, the mixed liquor of gained carbon nano-tube and PPG, the cooling back is stand-by;
C. preparation raw material mixed liquor: the dibutyl tin laurate 0.05ml that weighing is stand-by, triethylene diamine 0.05, silicone oil 0.3ml and deionized water 1ml add in the mixed liquor of the carbon nano-tube that made by step B and PPG, stir under 1000 rev/mins of conditions, make the raw material mixed liquor;
D. polymerization foaming: the isocyanates that weighing is stand-by joins rapidly in the raw material mixed liquor that is made by step C, under 2500 rev/mins the condition powerful stir 30 seconds after, mixed liquor is injected mould and rapid closing die cap, carry out the polymerization foaming and handle;
E. later stage maturation process: will place baking oven in the lump together with mould through the material after the step D polymerization foaming, after 100 ℃ of following maturation process 4 hours, cooling density be 0.2g/cm
3The carbon-doped nanometer tube hard polyurethane conductive foam plastic;
F. section: will cut into slices, promptly get sheet field emission cold-cathode goods by the specification of (long * wide * thick) 10 * 10 * 1mm by the conductive polyurethane foam plastic of step e gained carbon-doped nanometer tube.
These cold cathode goods are through high vacuum field transmitting station, and vacuum degree is less than 1 * 10
-6Holder, anode is the stainless steel cylinder of diameter of phi 3.9mm, and present embodiment makes the cold cathode goods as negative electrode, and anode is 0.4mm to the spacing of negative electrode, is 10 μ A/cm in emission
2Under the condition, its required unlatching electric field is 0.6V/ μ m, and is 1mA/cm in emission
2Under the condition, its threshold field is 1.4V/ μ m, field enhancement factor is 2.5 * 10
4
Embodiment 2: with preparation density is 0.5g/cm
3Hard carbon-doped nanometer tube conductive polyurethane foam plastic cold cathode be example:
A. get the raw materials ready: the deionized water that present embodiment adds in step C is the 0.5ml, and all the other supplementary materials are all identical with embodiment 1;
B. prepare the mixed liquor of carbon nano-tube and PPG: after the solution (oxidant) that at first adopts potassium permanganate 50g and concentrated sulfuric acid 500ml carries out oxidation processes to carbon nano-tube 5g, clean with deacidification and impurity with deionized water 5000ml, again the carbon nano-tube after the removal of impurities is distributed in the deionized water 500, makes the carbon nano-tube mixed liquor; Then that weighing is stand-by PPG 100ml adds in this mixed liquor, mix after, place 110 ℃ removing moisture content, the mixed liquor of gained carbon nano-tube and PPG, the cooling back is stand-by;
C. preparation raw material mixed liquor: the dibutyl tin laurate 0.05ml that weighing is stand-by, triethylene diamine 0.05, silicone oil 0.3ml and deionized water 0.5ml add in the mixed liquor of the carbon nano-tube that made by step B and PPG, stir under 1000 rev/mins of conditions, make the raw material mixed liquor;
D. polymerization foaming: the isocyanates that weighing is stand-by joins rapidly in the raw material mixed liquor that is made by step C, under 2500 rev/mins the condition powerful stir 30 seconds after, mixed liquor is injected mould and rapid closing die cap, carry out the polymerization foaming and handle;
E. later stage maturation process: will place baking oven in the lump together with mould through the material after the step D polymerization foaming, promptly getting density after 100 ℃ of following maturation process 4 hours, cooling is 0.5g/cm
3The carbon-doped nanometer tube hard polyurethane conductive foam plastic;
F. section: will be by the conductive polyurethane foam plastic of step e gained carbon-doped nanometer tube, cutting into slices, promptly get density by the specification of (long * wide * thick) 10 * 10 * 1mm is 0.5g/cm
3Sheet field emission cold-cathode goods.
These cold cathode goods are through high vacuum field transmitting station, and vacuum degree is less than 1 * 10
-6Holder, anode is the stainless steel cylinder of diameter of phi 3.9mm, and present embodiment makes the cold cathode goods as negative electrode, and anode is 0.4mm to the spacing of negative electrode, is 10 μ A/cm in emission
2Under the condition, its required unlatching electric field is 1.2V/ μ m, and is 1mA/cm in emission
2Under the condition, its threshold field is 2.0V/ μ m, field enhancement factor is 0.67 * 10
4
Embodiment 3: with preparation density is 0.2g/cm
3Soft carbon-doped nanometer tube conductive polyurethane foam plastic cold cathode be example:
A. get the raw materials ready: density is the PPG 100ml of 1.1g/ml, carbon nano-tube 2.5g, density is the isocyanates 20ml of 1.23g/ml, distilled water 0.5ml, density is the stannous octoate 0.03ml of 1.251g/ml, density is the triethylene diamine 0.03ml of 1.122g/ml, density is the silicone oil 0.2ml of 0.96g/ml, potassium permanganate 30g, density is the concentrated sulfuric acid 300ml of 1.4g/ml, weighing is stand-by respectively;
B. prepare the mixed liquor of carbon nano-tube and PPG: after the solution (oxidant) that at first adopts potassium permanganate 30g and red fuming nitric acid (RFNA) 300ml carries out oxidation processes to carbon nano-tube 2.5g, clean with deacidification and impurity with distilled water 2500ml, again the carbon nano-tube after the removal of impurities is disperseed to make the carbon nano-tube mixed liquor among the distilled water 250ml; Then that weighing is stand-by PPG 100ml adds in this mixed liquor, mix after, place 110 ℃ removing moisture content, the mixed liquor of gained carbon nano-tube and PPG, the cooling back is stand-by;
C. preparation raw material mixed liquor: the stannous octoate 0.03ml that weighing is stand-by, triethylene diamine 0.03, silicone oil 0.2ml and distilled water 0.5ml add in the mixed liquor of the carbon nano-tube that made by step B and PPG, stir under 1000 rev/mins of conditions, make the raw material mixed liquor;
D. polymerization foaming: the isocyanates that weighing is stand-by joins rapidly in the raw material mixed liquor that is made by step C, under 2500 rev/mins the condition powerful stir 25 seconds after, mixed liquor is injected mould and rapid closing die cap, carry out the polymerization foaming and handle;
E. later stage maturation process: will place baking oven in the lump together with mould through the material after the step D polymerization foaming, obtaining density after 100 ℃ of following maturation process 4 hours, cooling is 0.2g/cm
3Carbon-doped nanometer tube flexibel polyurethane conductive foam plastic;
F. section: will be by the conductive polyurethane foam plastic of step e gained carbon-doped nanometer tube, cutting into slices, promptly get density by the specification of (long * wide * thick) 10 * 10 * 1mm is 0.2g/cm
3Sheet field emission cold-cathode goods.
These cold cathode goods are through high vacuum field transmitting station, and vacuum degree is less than 1 * 10
-6Holder, anode is the stainless steel cylinder of diameter of phi 3.9mm, and present embodiment makes the cold cathode goods as negative electrode, and anode is 0.4mm to the spacing of negative electrode, is 10 μ A/cm in emission
2Under the condition, its required unlatching electric field is 0.6V/ μ m, and is 1mA/cm in emission
2Under the condition, its threshold field is 1.2V/ μ m, field enhancement factor is 2.5 * 10
4
Claims (7)
1. the conductive polyurethane foam plastic of carbon-doped nanometer tube is used as the cold cathode in the field emission vacuum electronic element.
By the conductive polyurethane foam plastic of the described carbon-doped nanometer tube of claim 1 as the cold cathode in the field emission vacuum electronic element, it is characterized in that cold cathode in the described field emission vacuum electronic element is the field emission cold-cathode in the flat-panel screens.
3. the conductive polyurethane foam plastic of pressing the described carbon-doped nanometer tube of claim 1 is as the cold cathode in the field emission vacuum electronic element, the content that it is characterized in that carbon nano-tube in the described conductive polyurethane foam plastic cold cathode is 0.5～5.0wt%, and the diameter of carbon nano-tube is Φ 1～40nm, pipe range 0.5～100 μ m.
4. the conductive polyurethane foam plastic of pressing the described carbon-doped nanometer tube of claim 1 is as the cold cathode in the field emission vacuum electronic element, it is characterized in that described conductive polyurethane foam plastic cold cathode for having honey comb like cellular network structure, even carbon nanotube is distributed in hard polyurethane conductive foam plastic or the flexibel polyurethane conductive foam plastic in cell walls and the honeycomb post.
5. the conductive polyurethane foam plastic of pressing the described carbon-doped nanometer tube of claim 1 is characterized in that as the cold cathode in the field emission vacuum electronic element conductive polyurethane foam plastic cold cathode of described carbon-doped nanometer tube is 10 μ A/cm in emission
2Under the condition, its required unlatching electric field≤1.2V/ μ m, and be 1mA/cm in emission
2Under the condition, its threshold field≤2.0V/ μ m.
6. be used as the production method of the cold cathode in the field emission vacuum electronic element by the conductive polyurethane foam plastic of the described carbon-doped nanometer tube of claim 1, comprise:
A. get the raw materials ready: the weight portion with PPG is a benchmark, press 100 parts of PPGs, 0.5～10 part of carbon nano-tube, 10～200 parts of isocyanates, 0.01～1.2 part of deionized water or distilled water, 0.01～1 part of organotin, 0.01～1 part of triethylene diamine, 10～100 parts in 0.1～3 part of silicone oil and potassium permanganate, 100～1000 parts of the concentrated sulfuric acid or red fuming nitric acid (RFNA)s, weighing is stand-by respectively;
B. prepare the mixed liquor of carbon nano-tube and PPG: after the solution that at first adopts the potassium permanganate and the concentrated sulfuric acid or red fuming nitric acid (RFNA) carries out oxidation processes to carbon nano-tube, clean to remove impurity with distilled water, again the carbon nano-tube after the removal of impurities is distributed in deionized water or acetone, the ethanol class polarity non-active solvent, makes the carbon nano-tube mixed liquor; Then that weighing is stand-by PPG adds in this mixed liquor, mix after, place 80～120 ℃ removing non-active solvent, the mixed liquor of gained carbon nano-tube and PPG, the cooling back is stand-by;
C. preparation raw material mixed liquor: organotin that weighing is stand-by and triethylene diamine, silicone oil and as the deionized water or the distilled water of blowing agent, add in the mixed liquor of the carbon nano-tube that makes by step B and PPG, stir, make the raw material mixed liquor;
D. polymerization foaming: the isocyanates that weighing is stand-by adds rapidly in the raw material mixed liquor that is made by step C, and powerful the stirring after 10～60 seconds injected mould and rapid closing die cap with mixed liquor, carries out the polymerization foaming and handles;
E. later stage maturation process: will place baking oven in the lump together with mould through the material after the step D polymerization foaming, after 80～120 ℃ of following maturation process 3～5 hours, cooling the conductive polyurethane foam plastic of carbon-doped nanometer tube;
F. section: will cut into slices, promptly get the field emission cold-cathode goods by the specification of field emission cold-cathode requirement by the conductive polyurethane foam plastic of step e gained carbon-doped nanometer tube.
7. by the production method of the described cold cathode of claim 6, it is characterized in that the described powerful speed that stirs is 1000～3000 rev/mins.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201010133313 CN101866794B (en) | 2010-03-26 | 2010-03-26 | New application of conductive polyurethane foam plastic of carbon-doped nanotube in vacuum electronic component |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201010133313 CN101866794B (en) | 2010-03-26 | 2010-03-26 | New application of conductive polyurethane foam plastic of carbon-doped nanotube in vacuum electronic component |
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| CN101866794A true CN101866794A (en) | 2010-10-20 |
| CN101866794B CN101866794B (en) | 2013-04-03 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106832177A (en) * | 2017-02-24 | 2017-06-13 | 耿佃勇 | polyurethane electronic sponge and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1788994A (en) * | 2004-11-22 | 2006-06-21 | 日信工业株式会社 | Method of manufacturing thin film, substrate having thin-film, electron emission material |
| CN1884373A (en) * | 2006-06-28 | 2006-12-27 | 四川大学 | Preparation of low density(0.03-0.2g/cm3)conductive polyurethane foam material containing carbon nanometer tube |
| CN1970598A (en) * | 2005-11-23 | 2007-05-30 | 四川大学 | Preparation of hard polyurethane conductive foam plastic for carbon nanotube filling |
| CN101250321A (en) * | 2008-03-18 | 2008-08-27 | 四川大学 | Preparation of light electric polyurethane foam plastic |
-
2010
- 2010-03-26 CN CN 201010133313 patent/CN101866794B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1788994A (en) * | 2004-11-22 | 2006-06-21 | 日信工业株式会社 | Method of manufacturing thin film, substrate having thin-film, electron emission material |
| CN1970598A (en) * | 2005-11-23 | 2007-05-30 | 四川大学 | Preparation of hard polyurethane conductive foam plastic for carbon nanotube filling |
| CN1884373A (en) * | 2006-06-28 | 2006-12-27 | 四川大学 | Preparation of low density(0.03-0.2g/cm3)conductive polyurethane foam material containing carbon nanometer tube |
| CN101250321A (en) * | 2008-03-18 | 2008-08-27 | 四川大学 | Preparation of light electric polyurethane foam plastic |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106832177A (en) * | 2017-02-24 | 2017-06-13 | 耿佃勇 | polyurethane electronic sponge and preparation method thereof |
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