CN101866794B - 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 benefitby 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 exists working temperature high and need preheating, and the defective such as volume is large, power consumption is high; The employing carbon nanomaterial of developing for these defectives is as the field emission cold-cathode technology, generally prepare, namely utilize the way of chemical vapor deposition growth masking to obtain the carbon nanometer film, as the field emission electron cold cathode of flat thin membranous type shape by the chemical vapor carbon deposition nanotube for the field emission cold-cathode of Diagonal Dimension less than the small size of 5-in; Although the sub-cold cathode of this type of generating has the advantages such as threshold field is lower, current density is larger, but exist complex manufacturing, production efficiency and output extremely low and to be difficult to prepare large tracts of land cold cathode, production cost high, can not form the disadvantages such as large-scale industrialized production; Then adopt spraying, ink-jet or print process preparation for the larger area field emission cold-cathode, technique is relatively simple although 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, the disadvantage such as effect is poor.
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 although the conductive polyurethane foam plastic of this type of doped carbon nanometer pipe has, carbon nano-tube consumption few (only needing 0.5-4.0%), production cost as doping are extremely low, easily realize the characteristics such as large-scale industrialized production; Use the 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 the defective for 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 the low gear purposes such as Production and Packaging thing, use as the cold-cathode material in the field emission vacuum electronic element, increase substantially 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 electron emission negative electrode, the productivity ratio of Effective Raise nano-graphite class flat field electron emission negative electrode, reduce its production cost, realize the 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: take the weight portion of PPG as 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 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 with the carbon nanotube dispersed after the removal of impurities in deionized water or acetone, ethanol class polarity non-active solvent, make the carbon nano-tube mixed liquor; Then after the PPG that weighing is stand-by adds in this mixed liquor, mixes, place 80～120 ℃ removing non-active solvent, the mixed liquor of gained carbon nano-tube and PPG, stand-by after the cooling;
C. preparation raw material mixed liquor: the organotin that weighing is stand-by and triethylene diamine, silicone oil (stabilizer) and as 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, strong stirring after 10～60 seconds, mixed liquor is injected mould and rapid closing die cap, carries out the polymerization foaming and processes;
E. later stage maturation process: the material after step D polymerization foaming is placed baking oven in the lump together with mould, after 80～120 ℃ of lower maturation process 3～5 hours, cooling the conductive polyurethane foam plastic of carbon-doped nanometer tube;
F. section: will by the conductive polyurethane foam plastic of step e gained carbon-doped nanometer tube, cut into slices, namely get the field emission cold-cathode goods by the specification of field emission cold-cathode requirement.
Strong stirring described in the said method, its mixing speed are 1000～3000 rev/mins.
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 greatly amplitude reduction [at present, the conductive polyurethane foam plastic of carbon-doped nanometer tube of the present invention (about 2～5m per ton then
3) about 50,000 yuan]; Thereby, the present invention has increased substantially 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 large field emission cold-cathode material of area, simplified the production technology of nano-graphite class flat field electron emission negative electrode, Effective Raise the productivity ratio of nano-graphite class flat field electron emission negative electrode, reduced the 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: take preparation hard carbon-doped nanometer tube conductive polyurethane foam plastic cold cathode as 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 to deacidify and impurity with deionized water 5000ml, again with the carbon nanotube dispersed after the removal of impurities in deionized water 500ml, make the carbon nano-tube mixed liquor; Then after the PPG 100ml that weighing is stand-by adds in this mixed liquor, mixes, place 110 ℃ removing moisture content, the mixed liquor of gained carbon nano-tube and PPG, stand-by after the cooling;
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, at strong stirring under 2500 rev/mins the condition after 30 seconds, mixed liquor is injected mould and rapid closing die cap, carries out the polymerization foaming and processes;
E. later stage maturation process: the material after step D polymerization foaming is placed baking oven in the lump together with mould, after 100 ℃ of lower maturation process 4 hours, cooling density be 0.2g/cm
3The carbon-doped nanometer tube hard polyurethane conductive foam plastic;
F. section: will by the conductive polyurethane foam plastic of step e gained carbon-doped nanometer tube, cut into slices, namely get sheet field emission cold-cathode goods by the specification of (long * wide * thick) 10 * 10 * 1mm.
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: take preparation density as 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 to deacidify and impurity with deionized water 5000ml, again with the carbon nanotube dispersed after the removal of impurities in deionized water 500, make the carbon nano-tube mixed liquor; Then after the PPG 100ml that weighing is stand-by adds in this mixed liquor, mixes, place 110 ℃ with except moisture content, the mixed liquor of gained carbon nano-tube and PPG, stand-by after the cooling;
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, at strong stirring under 2500 rev/mins the condition after 30 seconds, mixed liquor is injected mould and rapid closing die cap, carries out the polymerization foaming and processes;
E. later stage maturation process: the material after step D polymerization foaming is placed baking oven in the lump together with mould, and namely getting density after 100 ℃ of lower 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, namely 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: take preparation density as 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 to deacidify and impurity with distilled water 2500ml, with among the carbon nanotube dispersed distilled water 250ml after the removal of impurities, make the carbon nano-tube mixed liquor again; Then after the PPG 100ml that weighing is stand-by adds in this mixed liquor, mixes, place 110 ℃ with except moisture content, the mixed liquor of gained carbon nano-tube and PPG, stand-by after the cooling;
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, at strong stirring under 2500 rev/mins the condition after 25 seconds, mixed liquor is injected mould and rapid closing die cap, carries out the polymerization foaming and processes;
E. later stage maturation process: the material after step D polymerization foaming is placed baking oven in the lump together with mould, and obtaining density after 100 ℃ of lower 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, namely 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 (6)
1. the cold cathode in the field emission vacuum electronic element; The material that it is characterized in that cold cathode is the conductive polyurethane foam plastic of carbon-doped nanometer tube, and the content of carbon nano-tube is 0.5～5.0wt% in the conductive polyurethane foam plastic, and the diameter of carbon nano-tube is Φ 1～40nm, pipe range 0.5～100 μ m.
2. by the cold cathode in the described field emission vacuum electronic element of claim 1, 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. by the cold cathode in the described field emission vacuum electronic element of claim 1, 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.
4. by the cold cathode in the described field emission vacuum electronic element of claim 1, it is characterized in that the 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.
5. by the production method of the cold cathode in the described field emission vacuum electronic element of claim 1, comprising:
A. get the raw materials ready: take the weight portion of PPG as 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 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 with the carbon nanotube dispersed after the removal of impurities in deionized water or acetone, ethanol class polarity non-active solvent, make the carbon nano-tube mixed liquor; Then after the PPG that weighing is stand-by adds in this mixed liquor, mixes, place 80～120 ℃ removing non-active solvent, the mixed liquor of gained carbon nano-tube and PPG, stand-by after the cooling;
C. preparation raw material mixed liquor: the organotin that weighing is stand-by and triethylene diamine, silicone oil and as deionized water or the distilled water of blowing agent, add in the mixed liquor of the carbon nano-tube that made 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 strong stirring injected mould and rapid closing die cap with mixed liquor after 10～60 seconds, carries out the polymerization foaming and processes;
E. later stage maturation process: the material after step D polymerization foaming is placed baking oven in the lump together with mould, after 80～120 ℃ of lower maturation process 3～5 hours, cooling the conductive polyurethane foam plastic of carbon-doped nanometer tube;
F. section: will by the conductive polyurethane foam plastic of step e gained carbon-doped nanometer tube, cut into slices, namely get the field emission cold-cathode goods by the specification of field emission cold-cathode requirement.
6. by the production method of the described cold cathode of claim 5, the speed that it is characterized in that described strong stirring 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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| 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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| CN101866794B true CN101866794B (en) | 2013-04-03 |
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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
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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 |
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