CN101428975A - Processing method for thermal sintering in producing composite nano-diamond film on electrically conducting glass substrate - Google Patents
Processing method for thermal sintering in producing composite nano-diamond film on electrically conducting glass substrate Download PDFInfo
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- CN101428975A CN101428975A CNA2008102338017A CN200810233801A CN101428975A CN 101428975 A CN101428975 A CN 101428975A CN A2008102338017 A CNA2008102338017 A CN A2008102338017A CN 200810233801 A CN200810233801 A CN 200810233801A CN 101428975 A CN101428975 A CN 101428975A
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Abstract
The invention relates to the preparation of a composite nano-diamond film through screen printing on a conductive glass substrate, in particular to a thermal sintering treatment method in preparation of the composite nano-diamond film through screen printing on the conductive glass substrate. The method is characterized by comprising the following steps: the temperature is increased to be between 313 and 323K and then is maintained for 25 to 35 minutes, then the temperature is increased to be between 373 and 393K and then is maintained for 100 to 130 minutes, then the temperature is increased to be between 603 and 613K and then is maintained for 60 to 80 minutes, and the film is naturally cooled to room temperature. The thermal sintering treatment method has two aims that on one hand, the method ensures that the film is dried and firmly adhered to the conductive glass substrate; and on the other hand, the method ensures that a pulping material on the surface of the film is decomposed and evaporated to expose a diamond emitter tip. If the pulping material can not be fully decomposed and evaporated, the material can be closely wrapped on a nano-diamond emitter after a printing layer is dried, thereby making the nano-diamond emitter fail to emit electrons.
Description
Technical field
The present invention relates to that reticulated printing prepares composite nano-diamond film on the Conducting Glass, especially silk screen printing prepares processing method for thermal sintering in the composite nano-diamond film on the Conducting Glass.
Background technology
Diamond crystal has hardness the highest in the existing material of nature, its Mohs' hardness is 10.Adamantine fusing point is 4000 ℃; It also has very high thermal conductivity, and the thermal conductivity under the natural II quasi-diamond room temperature is 26W/ (CMK), is 5 times of copper.Thermal conductivity under the natural I quasi-diamond room temperature is 9W/ (CMK), thermal conductivity under the artificial high-quality single-crystal diamond room temperature is 18～20W/ (CMK), thermal conductivity under the general defective artificial single-crystal diamond room temperature is 4.5～6.5W/ (CMK), and the thermal conductivity under the general synthetic polycrystalline diamond room temperature is 4～10W/ (CMK).Fabulous thermal conductivity makes it become the preferred material in the microwave electron source that needs the Rapid Thermal diffusion.
Diamond energy gap numerical value is 5.3～5.5eV, DIELECTRIC CONSTANT r is 5.58 ± 0.03, the resistivity of natural diamond is 1010 Ω CM, resistivity under the natural II quasi-diamond room temperature is 1～108 Ω CM, the acceptor level of its boron is positioned at about 0.37eV on the valence band, has very high saturated carrier velocity.Adamantine breaking down field strength is up to 100 * 105V/cm.Diamond has good chemical stability, and is acidproof corrosion-resistant.Even at high temperature various acid are worked hardly to diamond, in the air diamond crystal of large-size below 600～700 ℃ and the diadust crystal all be very stable below 450～500 ℃.Though adamantine work function is up to 5.8eV, diamond has negative electron affinity.Especially the Nano diamond crystals is SP
3Key makes it have very high physical strength and chemical stability has determined its good insulation performance, stability and high rigidity; Nano diamond crystal grain is more little, the SP on top layer
2Key is many more, and its field emission performance is good more.Thereby nano-diamond film becomes the focus of electron emission research field in the world as the microwave electron source, particularly those devices that need big power consumption or must work under the high corrosion environment.
The present international and domestic method for preparing nano-diamond film, explosion method cleaning than early stage High Temperature High Pressure is reliable, but and the film of depositing high-quality, the main flow processing method for preparing diamond thin at present, chemical vapour deposition (MOCVD) is arranged, hot wire process MPCVD method, radio frequency discharge method, plasma torch method etc.Which kind of source of the gas atmosphere the researchist to taking come the depositing high-quality nano-diamond film also to carry out exploring widely and studying both at home and abroad, and the source of the gas atmosphere that is common in documents and materials at present has CH
4/ H
2CH
4/ Ar, CH4/N
2Deng.
Though it is a variety of that the preparation method of diamond thin has, these growth methods all can not obtain the fine diamond thin of the uniform field emission performance of big area.
Summary of the invention
The purpose of this invention is to provide silk screen printing on a kind of Conducting Glass and prepare processing method for thermal sintering in the composite nano-diamond film, make film drying on the one hand and be bonded on the Conducting Glass securely, pulping material decomposition evaporation on the film surface is fallen, expose the diamond emission tip.
For achieving the above object, the technical solution used in the present invention is:
Silk screen printing prepares the processing method for thermal sintering in the composite nano-diamond film on a kind of Conducting Glass, and its special feature is, comprises the following steps:
Kept 25-35 minute after being warming up to 313-323K, and then kept 100-130 minute after being warming up to 373-393K, and then kept 60-80 minute after being warming up to 603-613K, naturally cool to room temperature and get final product.
In intelligent sintering oven, carry out.
Composite nano-diamond film produces Low Temperature Hydrogen Plasma by plasma generator after thermal sintering, by pressurized air with 0.70W/cm
2Hydrogen plasma is sprayed to the nano-diamond film surface that previous step obtains suddenly, and the time kept 1.3-1.5 minute, and Nano diamond emission point is evenly distributed on the film surface.
Processing method for thermal sintering of the present invention has two purposes: film drying also is bonded on the Conducting Glass securely, the pulping material decomposition evaporation on the film surface is fallen, expose the diamond emission tip.If pulping material decomposition evaporation is fully fallen, these materials can closely be wrapped on the Nano diamond radiator after the printed layers drying, making it can't emitting electrons, therefore must in the heat treatment process of back, be removed, make the Nano diamond radiator expose film surface, just help electronic field emission.
Description of drawings
Accompanying drawing 1 is the thermal sintering treatment temp curve after printing among the present invention.
Embodiment
The processing method for thermal sintering that silk screen printing prepares in the composite nano-diamond film on the Conducting Glass is as follows:
One, preparation composite nano diamond slurry
Composite nano diamond slurry preparation process: long-time ultra-sonic dispersion in the weighing → grinding of Nano diamond, nano-graphite, ethyl cellulose → adding solvent → sieve → heated and stirred → room temperature of sieving → be cooled to.
Because the Nano diamond particle is easy to reunite, formation has the larger-size coacervate of some weak linkage interfaces, this has brought very big difficulty at the uniform distribution of substrate surface for nano particle, thereby influence the homogeneity of electron emission, so before pulp preparation, respectively Nano diamond and nano-graphite are ground, its coacervate granularity of scattering are diminished.Ethyl cellulose is preferably also ground.
The time of ultra-sonic dispersion was generally 6-9 hour in the heat-processed, treated that Nano diamond, nano-graphite, ethyl cellulose get final product abundant dispersion the in the solvent Terpineol 350.Nano particle is reunited easily, preparation composite diamond slurry, and it disperseed for three steps carried out.Mix after the weighing according to a certain percentage of the first step Nano diamond, nano-graphite, ethyl cellulose and grind and stir evenly; Second step was to add the solvent post-heating to 330K ultrasonic dispersing 6-9 hour, and agglomerated composite nano-diamond together obtains partition.The 3rd step was that the screen cloth (more than 400 orders) with high order number further filters mashed prod, by mechanical external force to remove macrobead wherein, and the size of composite nano-diamond aggregate of guaranteeing not obtain good distribution makes the composite nano-diamond uniform distribution being under the mechanical external force effect on the suitable yardstick.Disperse the scattered paste shape slurry to become heavy-gravity when being cooled to room temperature.
Two, silk screen printing prepares composite nano-diamond film
The used net of screen printing composite nanometer diamond thin has wire cloth and terylene silk net on the Conducting Glass, can determine the quality and the meshcount of silk screen according to the needs of actual print.Suitable meshcount is the 300-400 order, and the printing lines are meticulous more, and needed order number is high more.Printing equipment is the screen process press of automatic or manual.
When needing the printing special pattern, prepare the silk screen version of printing usefulness earlier.The mask-making technology flow process is: draw original copy → makings positive sheet → selection screen frame → net that stretches tight → glue net → half tone pre-treatment (cleaning) → be coated with photoresists → oven dry → printing down → development → colour-separation drafting → re-expose → drying → printing.
When printing, the operating method of handpress and automatic press is slightly different, but its principle is identical, all be with scraper plate (being called imprinter in the automatic press) extruding composite nano diamond slurry, make it by bite stock surface (on the Conducting Glass) below the silk screen of silk screen version.On Conducting Glass, utilize above-mentioned method for printing screen, above-mentioned composite nano diamond slurry is printed on the Conducting Glass as the indicating meter electron emitting cathode.
Three, the thermal sintering after the printing is handled
Owing to be enclosed on the Nano diamond radiator without pulping material in the printing composite nano diamond thin film of thermal sintering processing, handle so must carry out thermal sintering to it.
Thermal sintering has two purposes: make on the one hand film drying and be bonded in securely on the Conducting Glass, make on the other hand that contained pulping material decomposition evaporation falls in the film.If pulping material (ethyl cellulose) can not be fallen its decomposition evaporation fully, these materials can closely be wrapped on the Nano diamond radiator after the printed layers drying, making it can't emitting electrons, therefore must be removed in the heat treatment process of back.Make the Nano diamond radiator expose film surface, just help electronic field emission.
The thermal sintering curve comprises 3 temperature rise periods, 3 constant temperature stages and 1 temperature-fall period.First section constant temperature mainly is the oven dry nano-diamond film, and second section constant temperature mainly is that the capillary effect by slurry itself makes Nano diamond printed layers surface more evenly and smooth, be one from the modification process.And make the printed layers thorough drying.The 3rd section thermostatic process is in order to make dried pulping material at high temperature decompose volatilization.Be the nature temperature-fall period at last.
Four, the hydrogen plasma after the thermal sintering is handled
The carry out hydrogen plasma of silk screen printing after the composite nano-diamond film cathode sample thermal sintering of Conducting Glass handled.Plasma generator produce that the high voltagehigh frequency energy is activated in the nozzle steel pipe and controlled glow discharge in produced Low Temperature Hydrogen Plasma, by pressurized air hydrogen plasma is sprayed to the nano-diamond film surface, when meet in hydrogen plasma and surface, chemical action and physical change have been produced, its surface molecular chain structure has obtained change, SP
2It is many that key becomes, make electronics wear then and emission becomes easy; And the diamond tip on composite nano-diamond film surface is evenly distributed, improve the stability of electronic field emission.
The method cost of manufacture that above-mentioned silk screen printing prepares composite nano-diamond film is low, can the uniform printing composite nano diamond thin film of big area.Utilize the present invention, introduce the composite nano-diamond film of nano-graphite, improved the high characteristics of electron emission characteristic and electronic transmitting efficiency as the preparation of conduction crystal boundary.Diamond has good chemical stability, and is acidproof corrosion-resistant.The display cathode that on Conducting Glass, prepares with the screen printing composite nanometer diamond thin.The present invention uses Nano diamond as radiator, nano-graphite is as conductive medium, prepare the uniform composite nano-diamond film of big area with method for printing screen cheaply on Conducting Glass, it is fine and can be used for the display cathode of severe environment to have prepared field emission performance.
Embodiment 1
A kind of silk screen printing prepares the method for composite nano-diamond film on the Conducting Glass, comprises the following steps:
The grinding of a, Nano diamond and nano-graphite: to be ground to granularity be 100 nanometers with grinding body will to get nano-graphite 30 gram, Nano diamond 80 grams, ethyl cellulose 60 grams before pulp preparation respectively, and thorough mixing is as solute;
B, preparation Nano diamond slurry: with the solute that mixes, by the 1:5 mass ratio solute is added in the Terpineol 350, ultra-sonic dispersion 8 hours to solute fully disperses in solvent, heated and stirred under 373K then, after crossing 400 mesh sieves, make Nano diamond and nano-graphite uniform distribution, it is stand-by to naturally cool to room temperature;
C, silk screen printing prepare composite nano-diamond film: selecting the order number is 350 purpose wire cloth or terylene silk nets, uses the Nano diamond slurry that a step obtains and carries out silk screen printing on sheet glass by screen process press;
Thermal sintering after d, the printing is handled: kept 30 minutes after being warming up to 323K, and then kept 120 minutes after being warming up to 373K, and then kept 75 minutes after being warming up to 610K, it is stand-by to naturally cool to room temperature.
E, hydrogen plasma handle: produce Low Temperature Hydrogen Plasma by plasma generator, by pressurized air with 0.70W/cm
2Hydrogen plasma is sprayed to the nano-diamond film surface that previous step obtains suddenly, and the time kept 1.8 minutes, and Nano diamond emission point is evenly distributed on the film surface.
Embodiment 2
Thermal sintering after d, the printing is handled: kept 35 minutes after being warming up to 313K, and then kept 130 minutes after being warming up to 383K, and then kept 80 minutes after being warming up to 603K, it is stand-by to naturally cool to room temperature.
E, hydrogen plasma handle: produce Low Temperature Hydrogen Plasma by plasma generator, by pressurized air with 0.70W/cm
2Hydrogen plasma is sprayed to the nano-diamond film surface that previous step obtains suddenly, and the time kept 1.5 minutes, and Nano diamond emission point is evenly distributed on the film surface.
Rest part is identical in embodiment 1.
Embodiment 3
Thermal sintering after d, the printing is handled: kept 25 minutes after being warming up to 323K, and then kept 100 minutes after being warming up to 393K, and then kept 60 minutes after being warming up to 613K, it is stand-by to naturally cool to room temperature.
E, hydrogen plasma handle: produce Low Temperature Hydrogen Plasma by plasma generator, by pressurized air with 0.70W/cm
2Hydrogen plasma is sprayed to the nano-diamond film surface that previous step obtains suddenly, and the time kept 1.5 minutes, and Nano diamond emission point is evenly distributed on the film surface.
Rest part is identical in embodiment 1.
Claims (3)
1, silk screen printing prepares processing method for thermal sintering in the composite nano-diamond film on a kind of Conducting Glass, it is characterized in that, comprises the following steps:
Kept 25-35 minute after being warming up to 313-323K, and then kept 100-130 minute after being warming up to 373-393K, and then kept 60-80 minute after being warming up to 603-613K, naturally cool to room temperature and get final product.
2, silk screen printing prepares processing method for thermal sintering in the composite nano-diamond film on the Conducting Glass as claimed in claim 1, it is characterized in that:
In intelligent sintering oven, carry out.
3, silk screen printing prepares processing method for thermal sintering in the composite nano-diamond film on the Conducting Glass as claimed in claim 1 or 2, it is characterized in that:
Composite nano-diamond film produces Low Temperature Hydrogen Plasma by plasma generator after thermal sintering, by pressurized air with 0.70W/cm
2Hydrogen plasma is sprayed to the nano-diamond film surface that previous step obtains suddenly, and the time kept 1.3-1.5 minute, and Nano diamond emission point is evenly distributed on the film surface.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102338017A CN101428975B (en) | 2008-12-10 | 2008-12-10 | Processing method for thermal sintering in producing composite nano-diamond film on electrically conducting glass substrate |
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| CN2008102338017A CN101428975B (en) | 2008-12-10 | 2008-12-10 | Processing method for thermal sintering in producing composite nano-diamond film on electrically conducting glass substrate |
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| CN101428975A true CN101428975A (en) | 2009-05-13 |
| CN101428975B CN101428975B (en) | 2011-10-05 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101585534B (en) * | 2009-06-18 | 2011-06-01 | 西安交通大学 | Sol-gel method-based method for preparing composite nano diamond thin films |
| CN102832259A (en) * | 2012-08-30 | 2012-12-19 | 北方民族大学 | Window surface self-cleaning device of solar cell panel system |
-
2008
- 2008-12-10 CN CN2008102338017A patent/CN101428975B/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101585534B (en) * | 2009-06-18 | 2011-06-01 | 西安交通大学 | Sol-gel method-based method for preparing composite nano diamond thin films |
| CN102832259A (en) * | 2012-08-30 | 2012-12-19 | 北方民族大学 | Window surface self-cleaning device of solar cell panel system |
| CN102832259B (en) * | 2012-08-30 | 2016-03-30 | 北方民族大学 | A kind of window surface cleaning apparatus for self of solar panel system |
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| Publication number | Publication date |
|---|---|
| CN101428975B (en) | 2011-10-05 |
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Granted publication date: 20111005 Termination date: 20121210 |