CN103409138A - Preparation method of CNTs (Carbon Nano Tubes) used on PDP (Plasma Display Panel) and mixed with fluorescent powder - Google Patents
Preparation method of CNTs (Carbon Nano Tubes) used on PDP (Plasma Display Panel) and mixed with fluorescent powder Download PDFInfo
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- CN103409138A CN103409138A CN2013103393686A CN201310339368A CN103409138A CN 103409138 A CN103409138 A CN 103409138A CN 2013103393686 A CN2013103393686 A CN 2013103393686A CN 201310339368 A CN201310339368 A CN 201310339368A CN 103409138 A CN103409138 A CN 103409138A
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Abstract
The invention provides a preparation method of CNTs (Carbon Nano Tubes) used on a PDP (Plasma Display Panel) and mixed with fluorescent powder and belongs to the technical field of function materials. The preparation method comprises two steps of purifying and dispersing the CNTs; uniformly mixing the fluorescent powder with the CNTs. The first step is that impurities in the CNTs are removed through high-temperature burning and a reflux method; the surfaces of the CNTs are modified; then the monodispersion of the CNTs in solution is realized through activator addition and mechanical treatment. The second step is that the dispersed CNTs are mixed with the fluorescent powder; the mixture is stirred until the mixture is uniform; the mixture is subjected to high-temperature burning; finally the uniform mixing between the CNTs and the fluorescent powder is realized through a ball mill. According to the preparation method, the local clustering of the CNTs in the fluorescent powder is avoided, and the complete uniform mixing is realized. Through the adoption of the preparation method, the addressing time of the PDP is effectively shortened, the addressing speed of the PDP is improved, difficulty in controlling the mixing amount of the CNTs is lowered, and the improvement on the luminance and luminescence efficiency of the PDP is facilitated.
Description
Technical field
The invention belongs to technical field of function materials, relate to PDP preparation method, the especially PDP of the fluorescent material preparation method with carbon nano tube-doped fluorescent material.
Background technology
Since the nineties colour plasma display board in last century (PDP) was pushed to the market, its technical development reached its maturity.Because PDP has the characteristics such as big area, high brightness, high-contrast and wide visual angle, become gradually giant-screen main flow display device.
In the PDP working process, geseous discharge is a significant process, and geseous discharge can be divided into self-maintained discharge and non-self-maintained discharge according to its volt-ampere characteristic (as Fig. 1), and self-maintained discharge can be divided into selfsustaining dark discharge, glow discharge and arc discharge.And the glow discharge stage can select minimum one section of voltage wherein as normal glow discharge district (as the E-F section of Fig. 1), the needed voltage of this section is namely the stable operating voltage of PDP.The stable operating voltage that reduces PDP can reduce the power consumption in the PDP discharge process effectively.
Addressing and display separation ADS (Address and Display Separation) type of drive is one of type of drive commonly used of PDP work.It mainly contains three processes: initial phase, addressing stage and maintenance stage.At initial phase and institute's time spent addressing stage, be wherein namely addressing time (as Fig. 2), the addressing time of reducing PDP can effectively reduce its power consumption and improve its luminous efficiency.The fast development of HDTV (High-Definition Television) was at present had higher requirement to the addressing time of reducing PDP.Because address period is longer, the time of leaving maintenance phase for is just shorter, and the brightness of image is just lower, and picture quality is just lower.
Carbon nanotube (CNTs) is the very active nano material of Recent study, due to itself minimum size and symmetry structure highly, has given its significant quantum effect and excellent electric property, and conduction electrons has less electron affinity.Carbon nanotube has very high current capacity, in current density up to 6 * 10
6A/cm
2Situation under, the structure of its pipe does not still have destroyed.In addition, its physical strength is high, and its intensity is 100～1000 times of steel.Verified the interpolation in PDP fluorescent material the addressing time that the CNTs material can shorten PDP effectively, improve addressing speed.Yet because carbon nanotube has very high length-to-diameter ratio, high-specific surface area makes it very easily reunite and be wound around, surface presents chemical inert, therefore in matrix, be difficult to dispersed, easily form larger coacervate, because carbon nano-tube material has strong absorption to visible light, its content is very big on luminosity and the luminous efficiency impact of PDP screen simultaneously, and it is most important that the control of addition just becomes.Therefore, must process it before utilizing carbon nanotube: remove impurity, enhanced property, dispersed, make it to meet requirement of experiment.How improving the dispersing property of carbon nanotube, eliminate its reunion in the fluorescent material matrix, realize evenly mixing, is the important prerequisite condition of carbon nanotube in the application of PDP field, is significant.
Summary of the invention
The invention provides the preparation method of a kind of PDP with carbon nano tube-doped fluorescent material, this preparation method can be doped to even carbon nanotube in PDP fluorescent material, assemble the part of avoiding forming carbon nanotube, can effectively shorten the addressing time of PDP and improve addressing speed, and reduced the control difficulty of carbon nano tube-doped amount, helped to improve luminosity and the luminous efficiency of screen.
Technical solution of the present invention is as follows:
A kind of PDP by the preparation method of carbon nano tube-doped fluorescent material, as shown in Figure 3, comprises the following steps:
Step 1 a: calcination.Self-control or commercially available carbon nanotube are being no more than to fully calcination under the temperature condition of 400 ℃, with removal, are being attached to the organic impurity of carbon nano tube surface.
Step 2: ultrasonic backflow.It is 50% concentrated nitric acid solution sonic oscillation 1～2 hour that carbon nanotube after step 1 is processed is put into to mass percent concentration, then put into reflux abundant magnetic agitation under 80 ℃ of water bath condition, with the inorganic impurity of removing carbon nano tube surface and be with upper oxygen-containing functional group.
Step 3: centrifuge washing.Carbon nanotube after step 2 is processed is carried out to centrifugal treating, then adopt deionized water wash to pH value of solution to being neutral.
Step 4: ultrasonic dispersion.Carbon nanotube after step 3 is processed is added in the acetone organic solvent, and magnetic agitation after sonic oscillation, form set aside for use after homodisperse carbon nano tube dispersion liquid.For improving the dispersing uniformity of carbon nanotube in the acetone organic solvent, can add in right amount tensio-active agent (preferably nonionic surface active agent, wherein preferred Triton).
Step 5: mix.PDP is added in the acetone organic solvent with fluorescent material, after magnetic agitation, mix with step 4 gained carbon nano tube dispersion liquid, obtain the blending dispersion liquid system of PDP with fluorescent material and carbon nanotube, during mixing, should control PDP and make final target product PDP meet design requirement by the doping of carbon nanotube in carbon nano tube-doped fluorescent material by the ratio of fluorescent material and carbon nanotube.
Step 6: secondary calcination.By step 5 gained PDP by the blending dispersion liquid system of fluorescent material and carbon nanotube being no more than fully calcination under the temperature condition of 400 ℃, to remove acetone solvent and other organic residual impurity.
Step 7: ball milling.PDP after step 6 is processed is carried out to ball-milling processing with the mixture of fluorescent material and carbon nanotube, obtain the final carbon nano tube-doped fluorescent material of target product PDP.
Further, carbon nanotube described in step 1 can be single wall or multi-walled carbon nano-tubes, and its length-to-diameter ratio is 500～5000; PDP described in step 5 can be redness, green or blue colour fluorescent powder with fluorescent material;
The beneficial effect that the present invention compared with prior art has:
The invention provides the preparation method of a kind of PDP with carbon nano tube-doped fluorescent material, its operating process is simple, easily control, even carbon nanotube can be doped in PDP fluorescent material, assemble the part of avoiding forming carbon nanotube, can effectively shorten the addressing time of PDP and improve addressing speed, and reduced the control difficulty of carbon nano tube-doped amount, helped to improve luminosity and the luminous efficiency of screen.The present invention is that carbon nanotube really is applied to the PDP field and has created condition, can the structure generation of fluorescent material and carbon nanotube itself not destroyed simultaneously, and the preparation technology of itself and PDP screen has fine compatibility, Decrease production cost effectively.
The accompanying drawing explanation
The current voltage characteristic of Fig. 1 geseous discharge, can be divided into two stages of self-maintained discharge and non-self-maintained discharge.The E-F section normal glow discharge district of self-maintained discharge wherein, the needed voltage of this section is namely the stabilized voltage of PDP.
Fig. 2 means the three phases of addressing and display separation ADS (Address and Display Separation) type of drive: initial phase, addressing stage, maintenance stage.Initialize as seen from the figure, (addressing) stage that writes is address period.Addressing time very during this period of time.
Fig. 3 is schematic flow sheet of the present invention.
Fig. 4 is the setting drawing in reflow step, by round-bottomed flask, spherical condensation tube, U-shaped pipe drying tube, and tank, the hot type magnetic stirrer assembles.Wherein 1 is cooling water outlet, and 2 is tank, and 3 is the U-shaped drying tube, and 4 is soda-lime, and 5 is spherical condensation tube, and 6 is round-bottomed flask, and 7 is CNTs and concentrated nitric acid, and 8 is magneton, and 9 is cooling water inlet, and 10 is heating in water bath, and 11 is the hot type magnetic stirrer.
The centrifugal schematic diagram of Fig. 5.Wherein 12 is centrifuge tube, and 13 is whizzer.In centrifuge tube, filling CNTs and salpeter solution.
Fig. 6 is the calcination schematic diagram.Wherein 14 is retort furnace, and 15 is beaker, and 16 is the mixing solutions of CNTs and water.
Fig. 7 is the SEM figure of the CNTS sample of dispersion.
Embodiment:
Embodiment 1
A kind of PDP by the preparation method of carbon nano tube-doped fluorescent material, comprises the following steps:
1) calcination.To make by oneself or commercially available carbon nanotube is put into retort furnace, 400 ℃ of lower calcinations 2 hours, with removal, be attached to the organic impurity of carbon nano tube surface.
2) ultrasonic backflow.Weigh the carbon nanotube of 2.00g after a calcination is processed and put into round-bottomed flask, with graduated cylinder, measuring the 80.0ml mass percent concentration is that 50% salpeter solution injects round-bottomed flask, flask is put into to sonic oscillation machine sonic oscillation and processed 2 hours.Magneton is put into to round-bottomed flask, then round-bottomed flask, spherical condensation tube, U-shaped pipe such as Fig. 4 are coupled together, then device is placed in to magnetic stirrer, 80 ℃ of heating in water bath, stir 12h.
3) centrifuge washing.From the mixing solutions that takes out 10ml CNTs and concentrated nitric acid flask, inject centrifuge tube, use whizzer centrifugal 5min under 3000R/min, supernatant liquid is poured in waste liquid bottle, the CNTs of centrifuge tube bottom still stays in centrifuge tube, in centrifuge tube, injecting appropriate amount of deionized water, repeated centrifugation operation after stirring until the pH in centrifuge tube near 7.
4) ultrasonic dispersion.The carbon nanotube washed is put into to sample bottle, add and inject 100ml acetone, it is inserted to oscillation treatment in the sonic oscillation machine, in process, dropwise splash into the 1ml Triton, processed 2 hours, then in sample bottle, put into magneton, continue to stir 2h, finally sample bottle is placed in to standing 24h on platform.
5) mix.Get 2.0g green light fluorescent powder (Zn
2SiO
4: Mn
2+) add in 50ml acetone soln round-bottomed flask and carry out magnetic agitation, with syringe, get the 1ml carbon nano tube dispersion liquid subsequently and dropwise inject beaker, continue to stir 2 hours.
6) secondary calcination.The fluorescent material and the carbon nano-tube solution that mix are put into to quartz crucible, insert retort furnace, 400 ℃ of lower calcinations 2 hours, to remove acetone solvent and other organic residual impurity.
7) ball milling.The fluorescent material that to process through calcination and carbon nanotube mixture are put into mortar and are ground 0.5h and put into subsequently the planetary ball mill ball-milling processing 24 hours, take out sample, obtain the final carbon nano tube-doped fluorescent material of target product PDP.
A kind of PDP by the preparation method of carbon nano tube-doped fluorescent material, comprises the following steps:
1) calcination.To make by oneself or commercially available carbon nanotube is put into retort furnace, 400 ℃ of lower calcinations 2 hours, with removal, be attached to the organic impurity of carbon nano tube surface.
2) ultrasonic backflow.Weigh the carbon nanotube of 1.00g after a calcination is processed and put into round-bottomed flask, with graduated cylinder, measuring the 40.0ml mass percent concentration is that 50% salpeter solution injects round-bottomed flask, flask is put into to sonic oscillation machine sonic oscillation and processed 2 hours.Magneton is put into to round-bottomed flask, then round-bottomed flask, spherical condensation tube, U-shaped pipe such as Fig. 4 are coupled together, then device is placed in to magnetic stirrer, 80 ℃ of heating in water bath, stir 12h.
3) centrifuge washing.From the mixing solutions that takes out 5ml CNTs and concentrated nitric acid flask, inject centrifuge tube, use whizzer centrifugal 5min under 3000R/min, supernatant liquid is poured in waste liquid bottle, the CNTs of centrifuge tube bottom still stays in centrifuge tube, in centrifuge tube, injecting appropriate amount of deionized water, repeated centrifugation operation after stirring until the pH in centrifuge tube near 7.
4) ultrasonic dispersion.The carbon nanotube washed is put into to sample bottle, add and inject 50ml acetone, it is inserted to oscillation treatment in the sonic oscillation machine, in process, dropwise splash into the 1ml Triton, processed 2 hours, then in sample bottle, put into magneton, continue to stir 2h, finally sample bottle is placed in to standing 24h on platform.
5) mix.Get 1.0g red light fluorescent powder ((Y, Gd) BO
3: Eu
3+) add in 50ml acetone soln round-bottomed flask and carry out magnetic agitation, with syringe, get the 0.5ml carbon nano tube dispersion liquid subsequently and dropwise inject beaker, continue to stir 2 hours.
6) secondary calcination.The fluorescent material and the carbon nano-tube solution that mix are put into to quartz crucible, insert retort furnace, 400 ℃ of lower calcinations 2 hours, to remove acetone solvent and other organic residual impurity.
7) ball milling.The fluorescent material that to process through calcination and carbon nanotube mixture are put into mortar and are ground 0.5h and put into subsequently the planetary ball mill ball-milling processing 24 hours, take out sample, obtain the final carbon nano tube-doped fluorescent material of target product PDP.
Embodiment 3
A kind of PDP by the preparation method of carbon nano tube-doped fluorescent material, comprises the following steps:
1) calcination.To make by oneself or commercially available carbon nanotube is put into retort furnace, 400 ℃ of lower calcinations 2 hours, with removal, be attached to the organic impurity of carbon nano tube surface.
2) ultrasonic backflow.Weigh the carbon nanotube of 4.00g after a calcination is processed and put into round-bottomed flask, with graduated cylinder, measuring the 100.0ml mass percent concentration is that 50% salpeter solution injects round-bottomed flask, flask is put into to sonic oscillation machine sonic oscillation and processed 2 hours.Magneton is put into to round-bottomed flask, then round-bottomed flask, spherical condensation tube, U-shaped pipe such as Fig. 4 are coupled together, then device is placed in to magnetic stirrer, 80 ℃ of heating in water bath, stir 12h.
3) centrifuge washing.From the mixing solutions that takes out 10ml CNTs and concentrated nitric acid flask, inject centrifuge tube, use whizzer centrifugal 5min under 3000R/min, supernatant liquid is poured in waste liquid bottle, the CNTs of centrifuge tube bottom still stays in centrifuge tube, in centrifuge tube, injecting appropriate amount of deionized water, repeated centrifugation operation after stirring until the pH in centrifuge tube near 7.
4) ultrasonic dispersion.The carbon nanotube washed is put into to sample bottle, add and inject 200ml acetone, it is inserted to oscillation treatment in the sonic oscillation machine, in process, dropwise splash into the 2ml Triton, processed 2 hours, then in sample bottle, put into magneton, continue to stir 2h, finally sample bottle is placed in to standing 24h on platform.
5) mix.Get 4.0g blue light fluorescent powder (BaMgAl
10O
17: Eu
2+) add in 50ml acetone soln round-bottomed flask and carry out magnetic agitation, with syringe, get the 0.5ml carbon nano tube dispersion liquid subsequently and dropwise inject beaker, continue to stir 2 hours.
6) secondary calcination.The fluorescent material and the carbon nano-tube solution that mix are put into to quartz crucible, insert retort furnace, 400 ℃ of lower calcinations 2 hours, to remove acetone solvent and other organic residual impurity.
7) ball milling.The fluorescent material that to process through calcination and carbon nanotube mixture are put into mortar and are ground 0.5h and put into subsequently the planetary ball mill ball-milling processing 24 hours, take out sample, obtain the final carbon nano tube-doped fluorescent material of target product PDP.
Claims (6)
1. a PDP by the preparation method of carbon nano tube-doped fluorescent material, comprises the following steps:
Step 1 a: calcination; Self-control or commercially available carbon nanotube are being no more than to fully calcination under the temperature condition of 400 ℃, with removal, are being attached to the organic impurity of carbon nano tube surface;
Step 2: ultrasonic backflow; It is 50% concentrated nitric acid solution sonic oscillation 1～2 hour that carbon nanotube after step 1 is processed is put into to mass percent concentration, then put into reflux abundant magnetic agitation under 80 ℃ of water bath condition, with the inorganic impurity of removing carbon nano tube surface and be with upper oxygen-containing functional group;
Step 3: centrifuge washing; Carbon nanotube after step 2 is processed is carried out to centrifugal treating, then adopt deionized water wash to pH value of solution to being neutral;
Step 4: ultrasonic dispersion; Carbon nanotube after step 3 is processed is added in the acetone organic solvent, and magnetic agitation after sonic oscillation, form set aside for use after homodisperse carbon nano tube dispersion liquid;
Step 5: mix; PDP is added in the acetone organic solvent with fluorescent material, after magnetic agitation, mix with step 4 gained carbon nano tube dispersion liquid, obtain the blending dispersion liquid system of PDP with fluorescent material and carbon nanotube, during mixing, should control PDP and make final target product PDP meet design requirement by the doping of carbon nanotube in carbon nano tube-doped fluorescent material by the ratio of fluorescent material and carbon nanotube;
Step 6: secondary calcination; By step 5 gained PDP by the blending dispersion liquid system of fluorescent material and carbon nanotube being no more than fully calcination under the temperature condition of 400 ℃, to remove acetone solvent and other organic residual impurity;
Step 7: ball milling; PDP after step 6 is processed is carried out to ball-milling processing with the mixture of fluorescent material and carbon nanotube, obtain the final carbon nano tube-doped fluorescent material of target product PDP.
2. PDP according to claim 1, by the preparation method of carbon nano tube-doped fluorescent material, is characterized in that, carbon nanotube described in step 1 is single wall or multi-walled carbon nano-tubes, and its length-to-diameter ratio is 500～5000.
3. PDP according to claim 1, by the preparation method of carbon nano tube-doped fluorescent material, is characterized in that, the fluorescent material of PDP described in step 5 is redness, green or blue colour fluorescent powder.
4. according to right, to go any one PDP in 1 to 3 by the preparation method of carbon nano tube-doped fluorescent material, to it is characterized in that, in order to improve the dispersing uniformity of carbon nanotube in the acetone organic solvent, add in right amount tensio-active agent during the ultrasonic dispersion of step 4.
5. PDP according to claim 4, by the preparation method of carbon nano tube-doped fluorescent material, is characterized in that, described tensio-active agent is nonionic surface active agent.
6. PDP according to claim 5, by the preparation method of carbon nano tube-doped fluorescent material, is characterized in that, described nonionic surface active agent is Triton.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104597113A (en) * | 2015-01-21 | 2015-05-06 | 华中师范大学 | Image acquisition semiconductor film for high-resolution mass-spectral imaging system, and preparation method and application of image acquisition semiconductor film |
| CN106006601A (en) * | 2016-05-11 | 2016-10-12 | 赵社涛 | Pretreatment method of carbon nano tube for chemical power supply |
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| CN102115668A (en) * | 2010-12-17 | 2011-07-06 | 西北师范大学 | Novel temperature-sensitive fluorescent nano composite material and preparation method thereof |
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- 2013-08-06 CN CN2013103393686A patent/CN103409138A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102115668A (en) * | 2010-12-17 | 2011-07-06 | 西北师范大学 | Novel temperature-sensitive fluorescent nano composite material and preparation method thereof |
Non-Patent Citations (1)
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| 李锋: "碳纳米管的活化和碳纳米管_镍复合材料的制备", 《鞍山科技大学 硕士学位论文》, 15 September 2008 (2008-09-15), pages 23 - 24 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104597113A (en) * | 2015-01-21 | 2015-05-06 | 华中师范大学 | Image acquisition semiconductor film for high-resolution mass-spectral imaging system, and preparation method and application of image acquisition semiconductor film |
| CN104597113B (en) * | 2015-01-21 | 2015-12-09 | 华中师范大学 | A kind of high resolution mass spectrum imaging system image acquisition semiconductive thin film, preparation method and application |
| CN106006601A (en) * | 2016-05-11 | 2016-10-12 | 赵社涛 | Pretreatment method of carbon nano tube for chemical power supply |
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Inventor after: Yin Yi Inventor after: Xu Zhicai Inventor after: Lin Zulun Inventor after: Qi Kangcheng Inventor after: Cao Guichuan Inventor after: Wang Xiaoju Inventor after: Yan Qun Inventor after: Zhou Hui Inventor before: Yin Yi Inventor before: Xu Zhicai Inventor before: Lin Zulun Inventor before: Qi Kangcheng Inventor before: Cao Guichuan Inventor before: Wang Xiaoju |
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Application publication date: 20131127 |