CN103972007B - A kind of TiO 2nanotube triple-pole type field emitting electronic source and preparation method thereof - Google Patents

A kind of TiO 2nanotube triple-pole type field emitting electronic source and preparation method thereof Download PDF

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CN103972007B
CN103972007B CN201410215325.1A CN201410215325A CN103972007B CN 103972007 B CN103972007 B CN 103972007B CN 201410215325 A CN201410215325 A CN 201410215325A CN 103972007 B CN103972007 B CN 103972007B
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tio
nanotube
triple
zno
pole type
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CN103972007A (en
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周雄图
林木飞
郭太良
张永爱
叶芸
李福山
胡海龙
林金堂
胡利勤
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Fuzhou University
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Abstract

The present invention relates to a kind of TiO 2nanotube triple-pole type field emitting electronic source and preparation method thereof.Described TiO 2nanotube triple-pole type field emitting electronic source is with the TiO of vertical substrate grown in negative electrode or grid ad-hoc location 2nanotube is filed emission cathode material, and its preparation method comprises the following steps: first adopt micro-contact printing even print ZnO inculating crystal layer on the ad-hoc location of planar substrates; Then hydro thermal method growing ZnO nanorod on the position being printed with ZnO inculating crystal layer is adopted; Next be that template is at its peripheral growth one deck TiO with ZnO nanorod 2film; Finally by the TiO on ZnO nanorod top 2film etches, and dissolves ZnO nanorod by wet etching, forms TiO at the electrode of planar substrates 2nanotube.Triple-pole type field emission electronic source device prepared by the method, TiO 2nanotube draw ratio is high and density is controlled, functional.

Description

A kind of TiO 2nanotube triple-pole type field emitting electronic source and preparation method thereof
Technical field
The present invention relates to field emission flat panel display technical field, particularly a kind of TiO 2nanotube triple-pole type field emitting electronic source and preparation method thereof.
Background technology
Field emission displays (FieldEmissionDisplay, FED) is a kind of flat panel display of active illuminant of total solids.FED has the advantages such as volume is little, lightweight, low in energy consumption, and in addition, the response time of FED, operating temperature range was-45 ~+85 DEG C at Microsecond grade, had obviously advantage.One-dimensional metal oxide nano-material is high due to draw ratio, is easy to point discharge occurs, and field emission performance is excellent, is considered to one of filed emission cathode material of the best.Wherein, TiO 2monodimension nanometer material not only has low work function (4.5eV), and has good chemistry and thermal stability, and since being found to have an enhancement effect, the research of its field emission performance receives much concern.At present, TiO 2the main preparation methods of nanotube is anode oxidation method, but the TiO prepared by anode oxidation method 2nanotube is substantially all metal titanium sheet substrate or titanium film, prepare the feds of triple-pole type, can only form patterned titanium film, complex process by multi-step process such as plated film, photoetching, etchings; Secondly, the TiO that anode oxidation method can be prepared 2nanotube length is limited, and TiO 2nanotube alignment is too fine and close, affects its field emission performance, and these shortcomings limit it and comprising the application in many photoelectric devices of feds.
For existing TiO 2nanotube is difficult to the problems such as the feds making triple-pole type, the present invention is based on micro-contact printing and ZnO template, proposes a kind of TiO 2nanotube triple-pole type field emitting electronic source and preparation method thereof.
Summary of the invention
The object of the present invention is to provide a kind of triple-pole type field emission electronic source device prepared, and the TiO of this triple-pole type field emission electronic source device 2nanotube draw ratio is high and density is controlled, TiO of good performance 2nanotube triple-pole type field emitting electronic source and preparation method thereof.
For achieving the above object, technical scheme of the present invention is: a kind of TiO 2nanotube triple-pole type field emitting electronic source, the filed emission cathode material of described triple-pole type field emitting electronic source is vertical substrate located growth in the high length-diameter ratio TiO of negative electrode or grid 2nanotube, described TiO 2nanotube is by micro-contact printing ZnO nano particle location, and is that template growth obtains with ZnO nanorod.
Present invention also offers a kind of TiO 2the preparation method of nanotube triple-pole type field emitting electronic source, comprises the following steps,
S01: provide a preparation to have the planar substrates of negative electrode and gate electrode;
S02: adopt micro-contact printing even print ZnO inculating crystal layer on the negative electrode or grid of planar substrates;
S03: adopt hydro thermal method growing ZnO nanorod on the position being printed with ZnO inculating crystal layer;
S04: take ZnO nanorod as template, adopts liquid deposition at its peripheral growth one deck TiO 2film;
S05: by the TiO on ZnO nanorod top 2film etches, and dissolves ZnO nanorod by wet etching, finally forms TiO at the electrode of planar substrates 2nanotube, as triple-pole type filed emission cathode material.
In embodiments of the present invention, described TiO 2nanotube is arranged on the negative electrode of feds, or on the negative electrode being simultaneously arranged at feds and grid, and TiO 2nanotube grows perpendicular to planar substrates.
In embodiments of the present invention, the ZnO inculating crystal layer described in described step S02 is prepared from by printing ZnO nano particle, or becomes the salting liquid containing Zn element of ZnO to be prepared from by the easy heat resolve of printing.
In embodiments of the present invention, described salting liquid is zinc acetate solution or zinc nitrate solution.
In embodiments of the present invention, ZnO nanorod length described in described step S03 in 100 nanometers to 500 microns, diameter is in 10 nanometers to 10 microns, and described ZnO nanorod length and diameter are by the growth temperature of hydrothermal growth, growth-promoting media concentration and growth time state modulator.
In embodiments of the present invention, described TiO 2the caliber of nanotube and length are determined by the diameter of ZnO nanorod and length.
In embodiments of the present invention, the growth of liquid deposition described in described step S04 TiO 2the growth-promoting media that film adopts is ammonium titanium fluoride ((NH 4) 2tiF 6) and boric acid (H 3bO 3), described ammonium titanium fluoride ((NH 4) 2tiF 6) concentration range be 0.05 ~ 0.5 mol/L, the time of deposition is 1 ~ 60min; Described liquid deposition growth TiO 2film is by controlling growth parameter(s) control TiO 2film thickness, i.e. TiO 2nanotube pipe thickness.
In embodiments of the present invention, the TiO on ZnO nanorod top described in described step S05 2film, adopt the glycerite etching of 1% ~ 3% weight ratio HF and 1% ~ 50% weight ratio water, etch period is 1 ~ 60min.
In embodiments of the present invention, ZnO nanorod described in described step S05 adopts boric acid (H 3bO 3) the aqueous solution dissolve, described boric acid (H 3bO 3) concentration is 0.1 ~ 1 mol/L, dissolution time is 0.1 ~ 5 hour.
Compared to prior art, the present invention has following beneficial effect: on the one hand, adopts micro-contact printing to realize the last TiO formed 2the accurate location of nanotube, realizes TiO 2nanotube triple-pole type field emission electron source array; On the other hand, prepared TiO 2nanotube draw ratio is high, and even density is controlled, and field emission performance is good.
Accompanying drawing explanation
Fig. 1 is the schematic cross-section of the field emission electron emission source array electrode that first embodiment of the invention obtains.
Fig. 2 is the schematic cross-section of the micro-contact printing template that first embodiment of the invention obtains.
Fig. 3 is the schematic cross-section that first embodiment of the invention adopts micro-contact printing positioning printing ZnO inculating crystal layer on field-transmitting cathode.
Fig. 4 is the schematic cross-section of first embodiment of the invention located growth ZnO nanorod on field-transmitting cathode.
Fig. 5 is first embodiment of the invention is template liquid deposition one deck TiO with ZnO nanorod on field-transmitting cathode 2the schematic cross-section of film.
Fig. 6 is the TiO that first embodiment of the invention obtains 2the schematic cross-section of nanotube triple-pole type field emitting electronic source.
In accompanying drawing, main element description of symbols is as follows:
01-planar glass substrate; 02-field-transmitting cathode; 03-Flied emission grid; 04-micro-contact printing silicon rubber template; 05-ZnO nano particle; 06-ZnO nanorod; 07-TiO 2film; 08-TiO 2nanotube.
Embodiment
Below in conjunction with accompanying drawing, technical scheme of the present invention is specifically described.
A kind of TiO of the present invention 2nanotube triple-pole type field emitting electronic source, the filed emission cathode material of described triple-pole type field emitting electronic source is vertical substrate located growth in the high length-diameter ratio TiO of negative electrode or grid 2nanotube, described TiO 2nanotube is by micro-contact printing ZnO nano particle location, and is that template growth obtains with ZnO nanorod.
Present invention also offers a kind of TiO 2the preparation method of nanotube triple-pole type field emitting electronic source, comprises the following steps,
S01: provide a preparation to have the planar substrates of negative electrode and gate electrode;
S02: adopt micro-contact printing even print ZnO inculating crystal layer on the negative electrode or grid of planar substrates;
S03: adopt hydro thermal method growing ZnO nanorod on the position being printed with ZnO inculating crystal layer;
S04: take ZnO nanorod as template, adopts liquid deposition at its peripheral growth one deck TiO 2film;
S05: by the TiO on ZnO nanorod top 2film etches, and dissolves ZnO nanorod by wet etching, finally forms TiO at the electrode of planar substrates 2nanotube, as triple-pole type filed emission cathode material.
Described TiO 2nanotube is arranged on the negative electrode of feds, or on the negative electrode being simultaneously arranged at feds and grid, and TiO 2nanotube grows perpendicular to planar substrates.
ZnO inculating crystal layer described in described step S02 is prepared from by printing ZnO nano particle, or becomes the salting liquid containing Zn element of ZnO to be prepared from by the easy heat resolve of printing.
Described salting liquid is zinc acetate solution or zinc nitrate solution.
ZnO nanorod length described in described step S03 is in 100 nanometers to 500 microns, and diameter is in 10 nanometers to 10 microns, and described ZnO nanorod length and diameter are by the growth temperature of hydrothermal growth, growth-promoting media concentration and growth time state modulator.
Described TiO 2the caliber of nanotube and length are determined by the diameter of ZnO nanorod and length.
The growth of liquid deposition described in described step S04 TiO 2the growth-promoting media that film adopts is ammonium titanium fluoride ((NH 4) 2tiF 6) and boric acid (H 3bO 3), described ammonium titanium fluoride ((NH 4) 2tiF 6) concentration range be 0.05 ~ 0.5 mol/L, the time of deposition is 1 ~ 60min; Described liquid deposition growth TiO 2film is by controlling growth parameter(s) control TiO 2film thickness, i.e. TiO 2nanotube pipe thickness.
The TiO on ZnO nanorod top described in described step S05 2film, adopt the glycerite etching of 1% ~ 3% weight ratio HF and 1% ~ 50% weight ratio water, etch period is 1 ~ 60min.
ZnO nanorod described in described step S05 adopts boric acid (H 3bO 3) the aqueous solution dissolve, described boric acid (H 3bO 3) concentration is 0.1 ~ 1 mol/L, dissolution time is 0.1 ~ 5 hour.
In order to allow those skilled in the relevant art understand the present invention better, describe a kind of TiO in detail below in conjunction with drawings and Examples 2the preparation method of nanotube triple-pole type field emitting electronic source.Preferably, glass substrate selected by specific embodiment of the invention midplane substrate, and electrode selects CrCuCr conductive film, the monomer of dimethyl silicone polymer (PDMS) and the ratio column selection 10:1 of crosslinking agent in silicon rubber template.Preferably, the present embodiment selects ZnO nano particle to be that seed crystal carries out micro-contact printing.Preferably, the present embodiment prepares TiO on field-transmitting cathode 2nanotube.
The invention provides preferred embodiment, but should not be considered to be only limitted to embodiment set forth herein.In the drawings, in order to remove the thickness being exaggerated layer and region, but should not be considered to as schematic diagram the proportionate relationship strictly reflecting physical dimension.
At the schematic diagram that this reference diagram is idealized embodiments of the present invention, illustrated embodiment should not be considered to the given shape being only limitted to the region shown in figure, but comprises obtained shape, such as manufactures the deviation caused.All represent with rectangle in the present embodiment, the expression in figure is schematic, but this should not be considered to limit the scope of the invention.
embodiment one
The preparation method of a kind of TiO2 nanotube of first embodiment of the invention triple-pole type field emitting electronic source, comprises the following steps:
(S11)the making of field emission electron source electrode:
The glass substrate choosing two pieces of required sizes carries out scribing, be placed in by glass substrate is Win-10:DI water=3:97 cleaning fluid by volume, the ultrasonic machine cleaning 15min utilizing frequency to be 32KHz, after spray 2min, being placed in volume ratio is again Win-41:DI water=5:95 cleaning fluid, the ultrasonic machine cleaning 10min utilizing frequency to be 40KHz, after circulation running water spray rinsing 2min, recycling frequency is that the ultrasonic machine of 28KHz cleans 10min in DI pure water, dries up be placed on that to be incubated more than 30min in 50 DEG C of cleaning ovens for subsequent use through nitrogen gun.
Get one piece of clean planar glass substrate 01, one side utilizes magnetically controlled sputter method to prepare one deck CrCuCr conductive film wherein, spin coating proceeding is adopted evenly to apply one deck photoresist RZJ-304 on conductive film, 110 DEG C of bakings, after 20 minutes, form parallel electrode pattern through exposure-development on conductive film; This glass substrate is placed in containing Ce (NH 4) 2(NO 3) 6and HClO 4aqueous solution etching liquid in, the metallic member of exposure is etched, and is stayed by the metal that photoresist is protected, and after photoresist cleaning, final forms parallel band electrode, comprises field-transmitting cathode 02 and Flied emission grid 03, as shown in Figure 1.
(S12)micro-contact printing Template preparation:
The field emission electrode corresponding size prepared according to step (S11) designs the mask plate of micro-contact printing, namely needing the position of printing ZnO nano particle to protrude, not needing the position of printing ZnO nano particle for falling in.
Get another block cleaned glass substrate, employing is spin-coated on wherein one side evenly coating one deck photoresist RZJ-304,110 DEG C of bakings are after 20 minutes, photoresist RZJ-304 pattern is formed on the glass substrate through exposure-development, in this pattern, the local photoresist of corresponding negative electrode is developed agent and dissolves, and all the other photoresists remain, and forms micro-contact printing template an inverse pattern.
In the container having the glass substrate of micro-contact printing template an inverse pattern to seal preparation to be placed in and about 10ml trim,ethylchlorosilane molecule (TMCS) is housed, to place after about 5 minutes taking-up, now substrate surface self assembly one deck TMCS, for antiseized.Press ratio row configuration dimethyl silicone polymer (PDMS) mixture of monomer and crosslinking agent 10:1, be stirred to Homogeneous phase mixing.The substrate level of above-mentioned self assembly one deck TMCS is positioned in a container, pour dimethyl silicone polymer (PDMS) mixture into, leave standstill about 30 minutes all to eliminate to bubbling, this container is put into 80 DEG C of baking ovens more than two hours, take out after PDMS solidifies completely, PDMS is separated with substrate, and cuts into required micro-contact printing silicon rubber template 04, as shown in Figure 2.
(S13)micro-contact float printing of ZnO nano particle inculating crystal layer:
Micro-contact printing silicon rubber template 04 is placed in plasma cleaner, utilizes oxygen plasma to bombard and carries out finishing in 3 minutes.Then the suspension PDMS template 04 after finishing being placed in ZnO nano particle is hatched, after 20 minutes, and PDMS template surface self assembly layer of ZnO nano particle 05.During micro-contact printing, by the alignment system of accurate exposure machine, PDMS template (micro-contact printing silicon rubber template 04) ledge is aligned on field emitting electronic source negative electrode institute position.Contact after 5 minutes, remove PDMS template (micro-contact printing silicon rubber template 04), the ZnO nano particle 05 of contact portion will be transferred to field emitting electronic source negative electrode 02, and this process as shown in Figure 3.
(S14)the growth of ZnO nanorod:
The preparation ZnO nanorod growth aqueous solution, zinc nitrate hexahydrate (Zn (NO) in solution 36H 2o) concentration is 25mM, and hexamethylene tetramine (Hexamethylenetetramine, HMTA) concentration is 12.5mM, ammoniacal liquor (NH 3h 2o) concentration is 0.35M.During growth, lie against unsettled for the substrate being provided with ZnO inculating crystal layer in step (S13) beaker bottom (ZnO nano-structure aufwuchsplate down) that reactant liquor is housed, then put into 90 DEG C of constant temperature ovens and react, the reaction time is 6 hours.Taken out by sample after reaction terminates, clean with deionized water rinsing, nitrogen dries up.Vertical-growth is gone out ZnO nanorod 06 by the field-transmitting cathode 02 of field emitting electronic source, as shown in Figure 4.
(S15)take ZnO nanorod as template, adopt liquid deposition at its peripheral growth one deck TiO 2film:
The substrate of ZnO nanorod 06 is had to be placed in 0.075M ammonium titanium fluoride ((NH growth in step (S14) 4) 2tiF 6) and 0.05M boric acid (H 3bO 3) the aqueous solution in, growth have one of ZnO nano 06 rod to face down, carry out TiO 2liquid deposition.After 20min, TiO will be deposited 2the ZnO nanorod 06 of film 07 is by washed with de-ionized water and dry, as shown in Figure 5.
(S16)znO nanorod dissolves, and forms TiO 2nanotube:
Growth in step (S15) there is ZnO/TiO 2substrate is placed in the glycerite 2min containing 3% weight ratio HF and 12% weight ratio water, to etch away the coated TiO in ZnO nanorod 06 top 2film.Then, 0.5MH is immersed in 3bO 3in solution, 2h dissolves remaining ZnO in nanotube, obtains TiO 2nanotube 08 array (Fig. 6).Finally, by TiO 2nanotube 08 cleans with ultra-pure water and dries.
So far, a kind of TiO 2the preparation method of nanotube triple-pole type field emitting electronic source is formed.
Above example mainly describes a kind of TiO of the present invention 2the preparation method of nanotube triple-pole type field emitting electronic source.Although be only described some of them embodiments of the present invention, those of ordinary skill in the art should understand, and the present invention can implement with other forms many not departing from its purport and scope.Therefore, the example shown and way of example are regarded as illustrative and not restrictive, when do not depart from as appended each claim define the present invention spirit and scope, the present invention may contain various amendments and replacement.The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.

Claims (8)

1. a TiO 2the preparation method of nanotube triple-pole type field emitting electronic source, is characterized in that: the filed emission cathode material of described triple-pole type field emitting electronic source is vertical substrate located growth in the high length-diameter ratio TiO of negative electrode or grid 2nanotube, described TiO 2nanotube is by micro-contact printing ZnO nano particle location, and is that template growth obtains with ZnO nanorod;
Described TiO 2the preparation method of nanotube triple-pole type field emitting electronic source, comprises the following steps,
S01: provide a preparation to have the planar substrates of negative electrode and gate electrode;
S02: adopt micro-contact printing even print ZnO inculating crystal layer on the negative electrode or grid of planar substrates;
S03: adopt hydro thermal method growing ZnO nanorod on the position being printed with ZnO inculating crystal layer;
S04: take ZnO nanorod as template, adopts liquid deposition at its peripheral growth one deck TiO 2film;
S05: by the TiO on ZnO nanorod top 2film etches, and dissolves ZnO nanorod by wet etching, finally forms TiO at the electrode of planar substrates 2nanotube, as triple-pole type filed emission cathode material;
Described TiO 2nanotube is arranged on the negative electrode of feds, or on the negative electrode being simultaneously arranged at feds and grid, and TiO 2nanotube grows perpendicular to planar substrates.
2. a kind of TiO according to claim 1 2the preparation method of nanotube triple-pole type field emitting electronic source, is characterized in that: the ZnO inculating crystal layer described in described step S02 is prepared from by printing ZnO nano particle, or becomes the salting liquid containing Zn element of ZnO to be prepared from by the easy heat resolve of printing.
3. a kind of TiO according to claim 2 2the preparation method of nanotube triple-pole type field emitting electronic source, is characterized in that: described salting liquid is zinc acetate solution or zinc nitrate solution.
4. a kind of TiO according to claim 1 2the preparation method of nanotube triple-pole type field emitting electronic source, it is characterized in that: ZnO nanorod length described in described step S03 in 100 nanometers to 500 microns, diameter is in 10 nanometers to 10 microns, and described ZnO nanorod length and diameter are by the growth temperature of hydrothermal growth, growth-promoting media concentration and growth time state modulator.
5. a kind of TiO according to claim 4 2the preparation method of nanotube triple-pole type field emitting electronic source, is characterized in that: described TiO 2the caliber of nanotube and length are determined by the diameter of ZnO nanorod and length.
6. a kind of TiO according to claim 1 2the preparation method of nanotube triple-pole type field emitting electronic source, is characterized in that: the growth of liquid deposition described in described step S04 TiO 2the growth-promoting media that film adopts is ammonium titanium fluoride ((NH 4) 2tiF 6) and boric acid (H 3bO 3), described ammonium titanium fluoride ((NH 4) 2tiF 6) concentration range be 0.05 ~ 0.5 mol/L, the time of deposition is 1 ~ 60min; Described liquid deposition growth TiO 2film is by controlling growth parameter(s) control TiO 2film thickness, i.e. TiO 2nanotube pipe thickness.
7. a kind of TiO according to claim 1 2the preparation method of nanotube triple-pole type field emitting electronic source, is characterized in that: the TiO on ZnO nanorod top described in described step S05 2film, adopt the glycerite etching of 1% ~ 3% weight ratio HF and 1% ~ 50% weight ratio water, etch period is 1 ~ 60min.
8. a kind of TiO according to claim 1 2the preparation method of nanotube triple-pole type field emitting electronic source, is characterized in that: ZnO nanorod described in described step S05 adopts boric acid (H 3bO 3) the aqueous solution dissolve, described boric acid (H 3bO 3) concentration is 0.1 ~ 1 mol/L, dissolution time is 0.1 ~ 5 hour.
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