CN108400076B - A method of vacuum filtration improves field emission performance of carbon nano tube film - Google Patents
A method of vacuum filtration improves field emission performance of carbon nano tube film Download PDFInfo
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- CN108400076B CN108400076B CN201810088424.6A CN201810088424A CN108400076B CN 108400076 B CN108400076 B CN 108400076B CN 201810088424 A CN201810088424 A CN 201810088424A CN 108400076 B CN108400076 B CN 108400076B
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- Prior art keywords
- carbon nano
- tube film
- film
- carbon
- field emission
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/02—Manufacture of electrodes or electrode systems
- H01J9/022—Manufacture of electrodes or electrode systems of cold cathodes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
Abstract
The invention discloses a kind of methods that vacuum filtration improves field emission performance of carbon nano tube film, this method mixes the aqueous solution of carbon nano-tube material and surfactant, it is allowed to form a film by vacuum filtration, then it is allowed to be attached to the surface of conductive tape, the film is placed in room temperature ~ 100 DEG C again, relative air humidity is to allow surface voluntarily to crack under the environmental condition that 10 ~ 100%, cross-ventilation speed is 0 ~ 2 m/s, it places it in vacuum oven and is dried later, obtain carbon nano tube membrane field emission cathode.Experimental result confirms there is very excellent field emission performance using the carbon nano-tube film that the present invention is prepared.
Description
Technical field
The present invention relates to a kind of film preparing technology, it is especially applied to vacuum electronic transmitting and novel flat-plate and shows etc. answer
With the film preparing technology in field, and in particular to a kind of to use how vacuum filtration technique passes through when preparing carbon nano-tube film
Optimizing Process Parameters show crackle by film automatically, the method to obtain the field-transmitting cathode thin-film material haveing excellent performance.
Background technique
In recent years, lot of research all shows that carbon nanotube is most potential field emission flat panel display (FED) yin
Pole material, and carbon nano-tube film FED also had prototype showpiece to emerge, but carbon nano-tube film FED is difficult to be formed into so far
Ripe product goes on FPD market.A major reason of this hard case is caused to be the field hair of carbon nano-tube film
Penetrating performance also needs to further increase.In consideration of it, improving the performance of carbon nano-tube film feds, including threshold electric field and threshold
It is worth electric field, Flied emission current density stability, field transmitting uniformity, adhesion strength between film and substrate etc. is as field emission
The hot research problem in field.The method for currently commonly preparing carbon nanotube cathod film mainly includes silk screen print method, electricity
Swimming method, spray coating method, dip coating etc., but these preparation methods all have the shortcomings that respective, the table of especially uncontrollable film
Face pattern and obtain the feds haveing excellent performance.
Summary of the invention
The object of the present invention is to provide a kind of methods that can be improved cathode material field emission performance, are taken out by optimization vacuum
Filtering technology obtains the carbon nano-tube film that crackle is contained on surface, and being made into field-transmitting cathode can be enhanced field emission performance, obtain
The field emission display that must be had excellent performance.
Realizing the specific technical solution of the object of the invention is:
A method of vacuum filtration improve field emission performance of carbon nano tube film, this method comprising the following specific steps
Step 1: preparation is used for the dispersing agent of dispersing Nano carbon tubes
After surfactant and deionized water that mass ratio is 1:10~100 are mixed, magnetic agitation 1 at room temperature
It~60 minutes, is allowed to uniformly mixed, is as used for the dispersing agent of dispersing Nano carbon tubes；
Step 2: preparing carbon nano tube dispersion liquid
Taking mass ratio is that the carbon nanotube of 1:0.2~10 is mixed with above-mentioned dispersing agent, and magnetic force stirs at room temperature
It mixes 1~60 minute, is then sonicated 1~3 hour, is finally centrifuged 1~20 minute, obtains under 500~8000 revs/min of revolving speed
To upper layer troubled liquor be required carbon nano tube dispersion liquid；
Step 3: preparing carbon nanotube emission electrode
(1) vacuum filtration prepares carbon nano-tube film
One water system miillpore filter (aperture: 0.1~0.5 μm) of tiling, the carbon prepared is received in Vacuum filtration device
Mitron dispersion liquid slowly pours into bottle,suction, is filtered by vacuum.Filtering speed is 1~10 milliliter per minute, according to practical feelings
Condition filters time control and is rinsed at 1~60 minute, and when filtering with deionized water, until not having foam to go out in filtrate bottle
It is existing；Then filter membrane is removed, carbon nanotube is covered on filter membrane surface relatively uniformly at this time, and as required carbon nanotube is thin
Film.
(2) transfer of carbon nano-tube film and post bake
One section of conductive tape is taken out as substrate, the film layer covered on conductive tape is torn off, it is made to be tightly attached to carbon nanotube
Above film.Filter membrane is torn after cutting, naked be exposed on the external under environmental condition of the carbon nano-tube film on surface is allowed sufficiently voluntarily to split
It opens；Carbon nano-tube film is placed in vacuum oven again and is dried 1~10 hour under the conditions of 50~350 DEG C, is finally taken out
It is to be measured.
Step 4: improving field emission performance of carbon nano tube film
Carbon nano-tube film obtained will be optimized as emitting cathode and be assembled into feds, it is true to be placed in Flied emission test
In empty set system.During testing the field emission performance of carbon nano-tube film, which shows excellent
Different field emission performance, Turn-on voltage is down to 0.3~0.7V/ μm, and threshold field strength is down to 0.6~1.1V/ μm, Flied emission
It can increase.
The carbon nanotube is single-walled carbon nanotube, double-walled carbon nano-tube or multi-walled carbon nanotube.
The surfactant be neopelex, polypropylene tetramer benzene sulfonic acid sodium salt, nekal, yin from
Sub- polyacrylamide, soap, carboxylate, sulfuric acid or phosphate ester salt.
The adhesive tape is two-sided conductive tape or single-sided conductive adhesive tape.
The external environment condition is room temperature~100 DEG C, and relative air humidity is 10~100%, and cross-ventilation speed is 0
~2m/s.
Beneficial effects of the present invention: taking the technological parameter of the vacuum filtration of optimization, makes carbon nano-tube film hair obtained
It penetrates cathode and voluntarily tears crack, more nanotubes emitting tips is allowed to be exposed, in the Flied emission energy of enhancing electrode itself
Electric field shielding effect is reduced while power, to be integrally improved field emission performance, obtains the feds haveing excellent performance.
Detailed description of the invention
Fig. 1 is the carbon nanotube thin film material object schematic diagram that the embodiment of the present invention has been filtered by vacuum；
Fig. 2 is the not cracked carbon nano-tube film pictorial diagram and its SEM overhead view image in surface；
Fig. 3 is the cracked carbon nano-tube film pictorial diagram in surface and the wherein SEM overhead view image at one near crack；
Fig. 4 is the current density of the embodiment of the present invention with field strength change curve.
Specific embodiment
Present invention will be further explained with reference to the attached drawings and specific examples, but protection scope of the present invention is simultaneously
It is not limited to this.
The present invention includes specific steps:
Step 1: preparation is used for the dispersing agent of dispersing Nano carbon tubes
The neopelex of quality 1g is mixed with the deionized water of 100g, magnetic force stirs at room temperature
It mixes 15 minutes, is allowed to uniformly mixed, be as used for the dispersing agent of dispersing Nano carbon tubes；
Step 2: preparing carbon nano tube dispersion liquid
The double-walled carbon nano-tube of quality 100mg is taken to be mixed with the above-mentioned dispersing agent of 50ml, magnetic force stirs at room temperature
It mixes 15 minutes, is then sonicated 1 hour, is finally centrifuged 5 minutes under 1000 revs/min of revolving speed, obtained upper layer muddiness
Liquid is the carbon nano tube dispersion liquid needed for testing；
Step 3: preparing carbon nanotube emission electrode
(1) vacuum filtration prepares carbon nano-tube film
One water system miillpore filter (aperture: 0.45 μm) of tiling, the carbon nanotube that will be prepared in Vacuum filtration device
Dispersion liquid slowly pours into bottle,suction, is filtered by vacuum.Filtering speed is 2.5 milliliters per minute, and filtering the time is 30 minutes,
And rinsed when filtering with deionized water, until there is no foam appearance in filtrate bottle；Then filter membrane is removed, carbon nanotube has been at this time
It has been covered on filter membrane surface, as required carbon nano-tube film relatively uniformly.(as shown in Figure 1).
(2) transfer of carbon nano-tube film and post bake
One section of conductive tape is taken out as substrate, the film layer covered on conductive tape is torn off, it is made to be tightly attached to carbon nanotube
Above film, then by film be cut into 1cm × 1cm square carry out field emission performance test.Filter membrane is torn, allows sample surfaces
Under the exposed environmental condition indoors of carbon nano-tube film (29 DEG C of temperature, humidity 50%) sufficiently voluntarily split (reference pair ratio Fig. 2 with
Fig. 3).Fig. 2 a is the optical photograph for the carbon nano-tube film in crack do not occur, and Fig. 2 b is the scanning electron microscope amplification of 2a
Figure；Fig. 3 a is the optical photograph for the carbon nano-tube film that surface occurs behind crack, and Fig. 3 b is that the scanning electron in 3a at crack is aobvious
Micro mirror enlarged drawing.Carbon nano-tube film sample is placed in vacuum oven again and is dried 5 hours under the conditions of 80 DEG C, is finally taken
Sample is to be measured out.
Step 4: improving field emission performance of carbon nano tube film
The carbon nano-tube film and silk of carbon nano-tube film (containing crackle in surface) made from optimizing, surface flawless
The carbon nano-tube film that wire mark brush method is prepared is assembled into feds as emitting cathode respectively, is placed in Flied emission test
Field emission performance contrast test is carried out in vacuum system.As shown in figure 4, horizontal axis represents applied external electrical field intensity, with E table
Show (unit are as follows: every micron of volt), the longitudinal axis represents the emission current densities of the film sample, indicates (unit are as follows: microampere is every with J
Square centimeter).By comparing different vacuum filtration conditions, preferably the vacuum filtration sample with face crack possesses for discovery
Best field emission performance, field emission performance are 10 μ A/cm in current density2The threshold electric field at place is 0.52V/ μm and in electricity
Current density is 1000 μ A/cm2The threshold field at place is 1.05V/ μm, the Flied emission for the vacuum filtration sample that specific surface is not split
Energy (Turn-on voltage is 0.71V/ μm, and threshold field strength is 1.37V/ μm) is much lower, and prepares than common silk screen print method
The field emission performance (Turn-on voltage is that 0.81V/ μm of threshold field strength is 1.41V/ μm) of obtained carbon nano-tube film is also more excellent
It is different.Through this embodiment, effect of the present invention for improving field emission performance of carbon nano tube film is clearly and effective.
The embodiment described is the preferred embodiment of the present invention, but the present invention is not limited to the above embodiments, not
In the case where substantive content of the invention, any conspicuous improvement that those skilled in the art can make, replacement
Or modification all belongs to the scope of protection of the present invention.
Claims (4)
1. a kind of method that vacuum filtration improves field emission performance of carbon nano tube film, which is characterized in that this method includes following
Specific steps:
Step 1: preparation is used for the dispersing agent of dispersing Nano carbon tubes
After surfactant and deionized water that mass ratio is 1:10 ~ 100 are mixed, 1 ~ 60 point of magnetic agitation at room temperature
Clock is allowed to uniformly mixed, is as used for the dispersing agent of dispersing Nano carbon tubes；
Step 2: preparing carbon nano tube dispersion liquid
Taking mass ratio is that the carbon nanotube of 1:0.2 ~ 10 is mixed with above-mentioned dispersing agent, at room temperature magnetic agitation 1 ~ 60
Minute, it is then sonicated 1 ~ 3 hour, is finally centrifuged 1 ~ 20 minute under 500 ~ 8000 revs/min of revolving speed, obtained upper layer is muddy
Turbid body is required carbon nano tube dispersion liquid；
Step 3: preparing carbon nanotube emission electrode
(1) vacuum filtration prepares carbon nano-tube film
Tile a water system miillpore filter in Vacuum filtration device, and the carbon nanotube mixed aqueous solution prepared is slowly poured into
In bottle,suction, it is filtered by vacuum；Suction filtration speed is 1 ~ 10 ml/min, filters time control at 1 ~ 60 minute, and side is taken out
Filter side is rinsed with deionized water, until not having foam appearance in filtrate bottle；Then filter membrane is removed, carbon nanotube is equably covered at this time
It covers in filter membrane surface, as required carbon nano-tube film；Wherein, the aperture of the water system miillpore filter is 0.1 ~ 0.5 μm；
(2) transfer of carbon nano-tube film and post bake
One section of conductive tape is taken out as substrate, the film layer covered on conductive tape is torn off, it is made to be tightly attached to carbon nano-tube film
Above；Cut after tear off filter membrane, allow the carbon nano-tube film on surface it is naked be exposed on the external under environmental condition sufficiently voluntarily split and
Obtain carbon nano-tube film；The carbon nano-tube film is placed in vacuum oven again and dries 1 ~ 10 under the conditions of 50 ~ 350 DEG C
Hour, to remove the moisture in film and make film and substrate that there is good adhesiveness, finally take out to be measured；
Step 4: test field emission performance of carbon nano tube film
Feds are assembled into using carbon nano-tube film obtained as emitting cathode, are placed in Flied emission test vacuum system
In；During testing the field emission performance of carbon nano-tube film, which shows Flied emission
Can, Turn-on voltage is 0.3 ~ 0.7 V/ μm, and threshold field strength is 0.6 ~ 1.1 V/ μm；Wherein:
External environment condition described in step 3 is room temperature ~ 100 DEG C, and relative air humidity is 10 ~ 100%, and cross-ventilation speed is 0 ~ 2
m/s。
2. the method according to claim 1, wherein the carbon nanotube is single-walled carbon nanotube, double-walled carbon is received
Mitron or multi-walled carbon nanotube.
3. the method according to claim 1, wherein the surfactant is neopelex, four
Polypropylene benzene sulfonic acid sodium salt, nekal, anionic polyacrylamide, soap, carboxylate, sulfuric acid or phosphate
Salt.
4. the method according to claim 1, wherein the adhesive tape is two-sided conductive tape or single-sided conductive glue
Band.
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