CN1694207A - Method for preparing silver/carbon nanotube field emission cold cathode at low temperature - Google Patents
Method for preparing silver/carbon nanotube field emission cold cathode at low temperature Download PDFInfo
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- CN1694207A CN1694207A CN 200510013650 CN200510013650A CN1694207A CN 1694207 A CN1694207 A CN 1694207A CN 200510013650 CN200510013650 CN 200510013650 CN 200510013650 A CN200510013650 A CN 200510013650A CN 1694207 A CN1694207 A CN 1694207A
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- cathode
- field emission
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- tube
- carbon nanotube
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 20
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 14
- 239000004332 silver Substances 0.000 title claims abstract description 14
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims description 49
- 239000002041 carbon nanotube Substances 0.000 title claims description 49
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 10
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000758 substrate Substances 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000007921 spray Substances 0.000 claims abstract description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000011521 glass Substances 0.000 claims abstract description 4
- 239000010453 quartz Substances 0.000 claims abstract description 4
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 4
- 239000010703 silicon Substances 0.000 claims abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 19
- 239000002002 slurry Substances 0.000 claims description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims 1
- 238000010907 mechanical stirring Methods 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 4
- 238000013019 agitation Methods 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 abstract 1
- 230000002977 hyperthermial effect Effects 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 238000012876 topography Methods 0.000 description 6
- 230000018109 developmental process Effects 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 238000004626 scanning electron microscopy Methods 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000013528 metallic particle Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000002048 multi walled nanotube Substances 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Cold Cathode And The Manufacture (AREA)
- Electrodes For Cathode-Ray Tubes (AREA)
Abstract
The invention discloses a method for preparing silver/carbon nanometer tube field transmitting cold-cathode at low temp. This method includes mixing the nanometer silver tube and the carbon nanometer tube according to the mass ratio mixing the mixture in acetone, the ethyl alcohol, normal heptane and normal butyl alcohol solution, dispersing by the mechanical agitation and the supersonic wave forming spray size. Manufacturing field transmitting cold-cathode copper bottom electrode on glass, quartz, silicon substrate by magnetic suputtering method hyperthermic sintering in bake over, removing the mask, making the silver/carbon nanometer tube field transmitting cold-cathode. The advantages are good electric conductivity and strong adhesive the carbon nanometer tube may fully exposed on the surface of field transmitting cold-cathode.
Description
Technical field
The present invention relates to a kind of method, just belong to the technology that sintering prepares field emission cold-cathode by unordered made of carbon nanotubes field emission cold-cathode.
Background technology
Carbon nano-tube field emission display has vast market and good application prospects because of having low, the advantages such as brightness is big, resolution is high, response speed is fast, power consumption is little, good stability of the electric field of unlatching in the flat panel display field.Along with the continuous development of made of carbon nanotubes technology, more company and R﹠D institution are engaged in the development work of carbon nanotube field emission plane display.Main at present employing disordered carbon nanotube or carbon nano pipe array prepare field emission cold-cathode, because of screen effect problem between the caking property of carbon nano pipe array and substrate, the carbon nano-tube also is not well solved, the development of carbon nano pipe array Field Emission Display is subjected to certain limitation.And unordered made of carbon nanotubes is simple, output is big, cost is low, be fit to commercially produce, Korea S Samsung adopts conductive epoxy resin to mix with carbon nano-tube, method with silk screen printing prepares carbon nanotube field transmitting cold-cathode, and then produces the carbon nanotube field emission plane display suitable with the cathode-ray tube display performance; In addition, domestic scientific research personnel adopts method high temperature such as silver slurry or metal powder fusion preparation carbon nanotube field transmitting cold-cathode down.Adopt epoxy resin (mixing the conductivity that metallic particles increases resin sometimes) to have low, the easy shortcoming such as aging, poor reliability of conductivity, because carbon nano-tube usually is embedded in the epoxy resin influence emission effciency as binding agent.It is less to adopt conductive silver paste and metal powder fusion method to prepare the contact resistance of carbon nanotube field transmitting cold-cathode, but needs higher sintering temperature (500-1200 ℃), and the destructible carbon nano-tube also is unfavorable for the integrated of device; Because the particle diameter of metallic particles such as silver is (more than tens of microns) greatly, make the surface irregularity of field emission cold-cathode, influence the even distribution of carbon nano-tube, and then the control of an influence emission effciency and pixel.
Summary of the invention
The purpose of this invention is to provide a kind of method of utilizing nano-Ag particles to prepare carbon nanotube field transmitting cold-cathode, adopt this method can significantly improve conductivity and caking property between carbon nano-tube and the substrate, carbon nano-tube can be exposed to the field emission cold-cathode surface fully; Low preparation temperature can make carbon nano-tube field emission display spare and semiconductor technology compatibility, has quickened carbon nano-tube field emission display spare commercialization process.
The present invention is realized that by the following technical programs a kind of method of preparing silver/carbon nanotube field transmitting cold-cathode at low temp is characterized in that comprising following process:
1) nano-Ag particles of particle diameter 5-30nm and the carbon nano-tube of diameter 20-100nm are pressed mass ratio 10: 1-1: 3 mix, this mixture is added (4-5) by volume: (2-4): (1-3): (0.5-3) in the acetone of Hun Heing, ethanol, normal heptane and the butanol solution, adopt mechanical agitation and ultrasonic wave to combine and disperse, form the spraying slurry.
2) adopt magnetron sputtering method on glass, quartz, silicon base, to prepare the copper hearth electrode of field emission cold-cathode.
3) utilize mask to spray slurry on hearth electrode, carry out the temperature programming sintering then in baking oven, programming rate 0.1-2 ℃/min, sintering temperature arrives 140-200 ℃, and more than the insulation 1h.
4) remove mask, make the silver/carbon nanotube field transmitting cold-cathode of thickness 0.5-3 μ m.
Beneficial effect of the present invention is: adopt nano-Ag particles and carbon nano-tube to be mixed with field emission cold-cathode, promptly have caking property by force, the advantage that conducts electricity very well, its side's resistance can reach 0.007 Ω/below the.Because silver-colored particle grain size is less than the diameter of carbon nano-tube, under settlement action, the top of carbon nano-tube is exposed at the field emission cold-cathode surface, forms transmitting terminal, and the quality by nano-Ag particles and carbon nano-tube is than may command cold-cathode field emission.Because the volatility of acetone, ethanol, normal heptane and n-butanol is different, in the process that the carbon nano-tube cold cathode is shaped, it is smooth that its surface can keep.The more important thing is,, can utilize conventional semiconductor technology and printed circuit technology to produce the carbon nanotube field emission plane display, will promote commercially producing of carbon nanotube field emission plane display greatly because sintering temperature is low.
Description of drawings
Fig. 1 the present invention prepares carbon nanotube field transmitting cold-cathode method flow block diagram
High-resolution transmission electron microscope (HRTEM) photo of Fig. 2 silver nano-grain
The carbon nano-tube root is embedded in the TEM photo in the silverskin behind Fig. 3 sintering
Fig. 4 nano-Ag particles and carbon nano-tube are scanning electron microscopy (SEM) photo of the field emission cold-cathode surface topography of preparation in 5: 1 o'clock by mass ratio
Fig. 5 nano-Ag particles and carbon nano-tube by mass ratio be preparation in 2: 1 o'clock the SEM photo of field emission cold-cathode surface topography
Fig. 6 bottom nano-Ag particles and carbon nano-tube are 10: 1 o'clock by mass ratio, and second layer nano-Ag particles and carbon nano-tube are the SEM photo of the field emission cold-cathode surface topography of preparation in 1: 1 o'clock by mass ratio
Embodiment
Multi-walled carbon nano-tubes with silver nano-grain and catalystic pyrolysis preparation is that example illustrates how to implement the present invention, the invention is not restricted to these embodiment.
Embodiment 1 (as shown in Figure 1)
The nano-Ag particles of particle diameter 5-30nm and the carbon nano-tube of diameter 20-100nm are pressed mass ratio mixing in 5: 1, mixture is joined by 5: 4: 2: in the acetone of 1 mixed, ethanol, normal heptane and the butanol solution, the mode that adopts mechanical agitation and ultrasonic wave to combine is disperseed, and forms the spraying slurry.Adopting glass, quartz or silicon is substrate, and it is comprised that sulfuric acid carries out pickling, after deionized water is cleaned, cleans with acetone again, after the oven dry, will adopt magnetron sputtering method to prepare the copper hearth electrode of field emission cold-cathode in substrate.Utilize mask to spray slurry on hearth electrode, carry out the temperature programming sintering then in baking oven, 0.5 ℃/min of programming rate arrives 185 ℃ of sintering temperatures, and insulation 1.5h.Make the silver/carbon nanotube field transmitting cold-cathode of the about 1.5 μ m of average thickness behind the removal mask, carbon nano-tube bottom and substrate well bond together.The cold cathode surface topography as shown in Figure 4, cold cathode surface side resistance about 0.007 Ω/.Field emission experiment result shows that the carbon nanotube field transmitting cold-cathode emitting performance of this method preparation is better, and an emission and threshold field intensity are respectively 8mAcm
-2, 4.8V μ m
-1
Embodiment 2
Present embodiment is similar to embodiment 1, difference is that the mass ratio of nano-Ag particles and carbon nano-tube is 2: 1 in the step 1, and the sintering temperature that changes in the step 3 is 160 ℃, the cold cathode surface topography as shown in Figure 5, cold cathode surface side resistance about 0.009 Ω/, an emission and threshold field intensity are respectively 29mAcm
-2, 4.3V μ m
-1
Embodiment 3
Present embodiment is similar to embodiment 1, difference is that step 3 spraying earlier is 10: 1 slurry with the mass ratio of nano-Ag particles and carbon nano-tube, after drying by the fire 0.5h under slowly being warming up to 100 ℃, the mass ratio that sprays nano-Ag particles and carbon nano-tube again is 2: 1 a slurry, the cold cathode surface topography as shown in Figure 6 when sintering temperature was 200 ℃, cold cathode surface side resistance about 0.008 Ω/, an emission and threshold field intensity are respectively 31mAcm
-2, 3.9V μ m
-1
Embodiment 4
Present embodiment is similar to embodiment 1, difference is that the mass ratio of nano-Ag particles and carbon nano-tube is 1: 1 in the step 1, and the sintering temperature that changes in the step 3 is 140 ℃, and cold cathode surface side hinders about 0.037 Ω/, and field emission and threshold field intensity are respectively 19mAcm
-2, 5.2V μ m
-1
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510013650 CN1694207A (en) | 2005-06-01 | 2005-06-01 | Method for preparing silver/carbon nanotube field emission cold cathode at low temperature |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510013650 CN1694207A (en) | 2005-06-01 | 2005-06-01 | Method for preparing silver/carbon nanotube field emission cold cathode at low temperature |
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| Publication Number | Publication Date |
|---|---|
| CN1694207A true CN1694207A (en) | 2005-11-09 |
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| CN 200510013650 Pending CN1694207A (en) | 2005-06-01 | 2005-06-01 | Method for preparing silver/carbon nanotube field emission cold cathode at low temperature |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7887878B2 (en) | 2006-12-07 | 2011-02-15 | Electronics And Telecommunications Research Institute | Method of manufacturing a fine-patternable, carbon nano-tube emitter with high reliabilty |
| CN103871802A (en) * | 2012-12-15 | 2014-06-18 | 中国科学院深圳先进技术研究院 | Carbon nanotube composite thin film field emission cathode preparation method |
| CN106745365A (en) * | 2016-12-05 | 2017-05-31 | 南京悠谷知识产权服务有限公司 | A kind of water purification material and preparation method thereof |
| CN111128635A (en) * | 2019-12-24 | 2020-05-08 | 中国工程物理研究院应用电子学研究所 | High-current repetition frequency carbon nanotube reinforced silver cold cathode and preparation method thereof |
-
2005
- 2005-06-01 CN CN 200510013650 patent/CN1694207A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7887878B2 (en) | 2006-12-07 | 2011-02-15 | Electronics And Telecommunications Research Institute | Method of manufacturing a fine-patternable, carbon nano-tube emitter with high reliabilty |
| CN103871802A (en) * | 2012-12-15 | 2014-06-18 | 中国科学院深圳先进技术研究院 | Carbon nanotube composite thin film field emission cathode preparation method |
| CN103871802B (en) * | 2012-12-15 | 2016-09-07 | 中国科学院深圳先进技术研究院 | The preparation method of carbon nano-tube coextruded film field-transmitting cathode |
| CN106745365A (en) * | 2016-12-05 | 2017-05-31 | 南京悠谷知识产权服务有限公司 | A kind of water purification material and preparation method thereof |
| CN111128635A (en) * | 2019-12-24 | 2020-05-08 | 中国工程物理研究院应用电子学研究所 | High-current repetition frequency carbon nanotube reinforced silver cold cathode and preparation method thereof |
| CN111128635B (en) * | 2019-12-24 | 2023-04-07 | 中国工程物理研究院应用电子学研究所 | High-current repetition frequency carbon nanotube reinforced silver cold cathode and preparation method thereof |
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