CN1700388A - Process for preparing carbon nanotube cathode material - Google Patents

Process for preparing carbon nanotube cathode material Download PDF

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Publication number
CN1700388A
CN1700388A CN 200510017467 CN200510017467A CN1700388A CN 1700388 A CN1700388 A CN 1700388A CN 200510017467 CN200510017467 CN 200510017467 CN 200510017467 A CN200510017467 A CN 200510017467A CN 1700388 A CN1700388 A CN 1700388A
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Prior art keywords
carbon nanotube
slurry
nanotube cathod
cathod
tube
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CN 200510017467
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CN100580844C (en
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李玉魁
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Zhongyuan University of Technology
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Zhongyuan University of Technology
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Publication of CN100580844C publication Critical patent/CN100580844C/en
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Abstract

This invention relates to ultraviolet irradiation and wire printing combination to process the process of carbon nanometer tube and to make the nanometer plasm to process the nanometer negative pattern.

Description

A kind of manufacture craft of carbon nanotube cathode material
Technical field
The invention belongs to the mutual crossing domain of vacuum science technology, nanoscale science and technology and microelectronics science and technology, relate to a kind of with the carbon nano-tube material directional implantation to substrate surface as the preparation technology of Field Emission Cathode Materials, be specifically related to a kind ofly adopt UV-irradiation and silk screen print method to combine to make the manufacture craft of large tracts of land carbon nanotube cathod.
Background technology
At present, for the field emission flat-panel display that utilizes carbon nano-tube to make as cathode material, its negative electrode manufacture craft is varied, has nothing in common with each other.
Utilize the field emission characteristics of the carbon nanotube cathod of growth technique preparation to be better than the field emission characteristics of the carbon nanotube cathod of other implantation method preparation, bigger autoelectronic current can be provided, the directionality of carbon nano-tube and uniformity are all more superior, but be subjected to the restriction of other structure fabrication process characteristic of device, restricting the application of the carbon nanotube cathod of growing method preparation; When carrying out the large tracts of land carbon nanotube cathode material when making, the increase that its cost of manufacture can be at double; The temperature of carrying out carbon nano tube growth is very high, makes selecting to be subjected to very big constraint aspect the making backing material.In addition, be subjected to the influence of concrete technology and equipment, when carrying out the making of large tracts of land carbon nanotube cathod, its uniformity is difficult to be guaranteed.Make aspect the cathode material transplanting carbon nano-tube, sedimentation has simple to operate, and to advantages such as making apparatus are less demanding, but the adhesion of the carbon nanotube cathod of made is very poor, does not have to carry out the feasibility that large area cathode is made; Silk screen print method is the method for another carbon nanotube cathod preparation, its process matched therewith is very complete, can carry out the making of large area cathode, but be subjected to certain restriction aspect the making high resolution display spare, be difficult to realize high-precision display graphics, owing to have only the fraction carbon nano-tube from pulping material, to expose its tip, be difficult to obtain big field emission.
Also there are not at present a kind of carbon nanotube cathod preparation method and manufacture craft practicable, simple to operate, that can meet the each side basic demand.Certainly, in the preparation process of carbon nanotube cathode material, also need to simplify the manufacture craft of device, improve the power that is made into of device, reduce the element manufacturing cost, make the manufacture craft of integral device trend towards oversimplifying, reduce, go back the effective solution of neither one at present making the material requirements of device material.
Summary of the invention
The objective of the invention is to overcome the defective that prior art exists and provide that a kind of manufacture craft is simple, cost of manufacture is cheap, manufacturing process is reliable and stable, be suitable for carrying out the manufacture craft of the carbon nanotube cathode material of large tracts of land carbon nanotube cathod preparation.
The object of the present invention is achieved like this: comprise following making step:
1, the scribing of cathode substrate glass (1): whole plate glass is carried out scribing;
2, the making of negative electrode bus (2): go up evaporation one deck tin indium oxide thin layer at cathode substrate glass (1); Tin indium oxide thin layer to evaporation carries out photoetching, forms negative electrode bus (2);
3, the preparation of carbon nanotube powders powder material: carbon nanotube powder is purified, dispose the central impurity of powder, and carry out the discrete work of agglomerate carbon nanotube particulate;
4, the making of carbon nano-tube slurry: the carbon nanotube powder after at first will dispersing, a small amount of graphite slurry mix, and then mixed slurry and photoresists are stirred in together, and stir evenly, and form the carbon nano-tube slurry of printing usefulness;
5, the printing of carbon nanotube cathod pattern:, the carbon nano-tube slurry is printed onto above the negative electrode bus (2) in conjunction with silk-screen printing technique; Carbon nano-tube slurry after the printing is carried out the initial stage low-temperature bake solidify (temperature: 80 ℃, duration: 30 minutes);
6, the exposure of carbon nanotube cathod slurry: the carbon nanotube cathod slurry on the target substrate glasses (1) exposes; The light source that uses is ultraviolet irradiation;
7, the development of carbon nanotube cathod slurry: the carbon nanotube cathod slurry through UV-irradiation is developed.Under the situation of using negative photoresist, the place of being crossed by UV-irradiation will be retained, and the place of not crossed by UV-irradiation, its photoresists can lose efficacy, be developed liquid and get rid of, be stirred in its photoresists central carbon nano-tube and graphite slurry and also can remove thereupon; If use positive photoresist, then situation is opposite;
8, the high-temperature baking of carbon nanotube cathod slurry: the carbon nanotube cathod slurry that developed is carried out high-temperature baking; Baking temperature is 450 ℃, and the retention time is 30 minutes;
9, the reprocessing of carbon nanotube cathod (3): high-temperature baking is crossed carbon nanotube cathod carry out conventional friction reprocessing, in the hope of further improving the pattern of carbon nanotube cathod (3).
In manufacture craft of the present invention, described backing material be large-scale, have quite good thermal endurance and operability, a High Performance Insulation material with low cost; Described backing material is a glass, as soda-lime glass, and Pyrex; Described carbon nanotube cathod bus is a tin indium oxide thin layer; Described carbon nanotube powder will be purified; Described carbon nano-tube paste composition has carbon nanotube powder, a small amount of graphite slurry and photoresists composition; The printing of described carbon nanotube cathod pattern is finished in conjunction with silk-screen printing technique; Described carbon nano-tube slurry exposure technology with ultraviolet light as light source; Described photoresists can be positive photoresist, also can be negative photoresist; The carbon nanotube cathod slurry of described development will carry out high-temperature baking; Described carbon nanotube cathod will carry out aftertreatment technology.
The present invention has following good effect:
Feature among the present invention just is to have prepared the carbon nano-tube slurry in conjunction with carbon nanotube powder, a small amount of graphite slurry and photoresists, and the large-area manufacturing feasibility of silk-screen printing technique and the developing process that exposes made precision is higher, lines are thinner, the favourable part of lines better quality combines, and makes better carbon nanotube cathod.
1 in manufacture craft of the present invention, has carried out the making of carbon nanotube cathode material in conjunction with the basis of silk-screen printing technique, has to carry out the feasibility that the large tracts of land carbon nanotube cathod is made; 2 in manufacture craft of the present invention, does not adopt special manufacturing materials and special manufacture craft, can greatly reduce the production cost of device; 3 in manufacture craft of the present invention, adopted the bus of tin indium oxide film as carbon nanotube cathod, this exists the favourable part of following several aspects: on the basis in conjunction with photoetching process, can carry out the more making of hachure, help further improving the display resolution of flat device; Tin indium oxide film is transparent, helps normally carrying out in the post-exposure technology; Help further improving the adhesion between carbon nanotube cathod and the backing material; 4 in manufacture craft of the present invention, has added a spot of graphite slurry in the carbon nano-tube slurry, and this helps forming good electricity and contacting in the conduction that further strengthens carbon nano-tube and the backing material ability that communicates; 5 in manufacture craft of the present invention, and carbon nanotube powder (together with graphite slurry) and photoresists are mixed.Because photoresists have certain viscosity, so the carbon nano-tube slurry after being in harmonious proportion can be suitable for the needs of silk-screen printing technique; Because the making of thinner carbon nanotube cathod lines by ultraviolet photoetching one developing process, can be realized in the characteristic place of photoresists.That is to say,, can carry out the making of large tracts of land carbon nanotube cathod, can carry out the carbon nanotube cathod lines of certain precision and make by silk-screen printing technique; By the subsequent technique that photoresists exposure one is developed, can on the basis of the carbon nanotube cathod lines of having made certain precision, produce the carbon nanotube cathod lines that precision is higher, lines are thinner, the lines quality is better.Like this, the favourable part of the higher lines of making precision of the developing process that just the large-area manufacturing feasibility of silk screen print method and photoresists exposed combines, and carries out the making of carbon nanotube cathod line image; In the 6 described in the present invention manufacture crafts, the carbon nanotube cathod that developed is carried out high-temperature baking technology, its main purpose is the photoresists of removing in the residue carbon nanotube cathod.After the high temperature through more than 400 degree, all burnt through the remaining photoresists in back that develop, remaining carbon nanotube (together with graphite slurry) is fixed on the tin indium oxide bus; In the 7 described in the present invention manufacture crafts, adopted conventional friction aftertreatment technology, in the hope of further improving the pattern of carbon nanotube cathod.
Description of drawings
Fig. 1 has provided the vertical structure schematic diagram of cathode construction.
Fig. 2 has provided the schematic diagram of carbon nanotube cathod bus.
Fig. 3 has provided the schematic diagram of zygomite reticulated printing technology printed carbon nanotube on the negative electrode bus.
Fig. 4 has provided the schematic diagram of the carbon nanotube cathod after the exposure.
The implication of symbol is among wherein above-mentioned each figure: 1 cathode substrate glass; 2 negative electrode buss; 3 carbon nanotube cathods;
Embodiment
Shown in Fig. 1,2,3,4, the present invention is further specified the present invention with showing for a more clear understanding of the present invention, but the present invention is not limited to these embodiment below in conjunction with drawings and Examples.
Provide a kind of manufacture craft of carbon nanotube cathode material among the present invention, comprised following making step:
1, the scribing of cathode substrate glass (1): whole plate glass is carried out scribing;
2, the making of negative electrode bus (2): go up evaporation one deck tin indium oxide thin layer at cathode substrate glass (1); Tin indium oxide thin layer to evaporation carries out photoetching, forms negative electrode bus (2);
3, the preparation of carbon nanotube powders powder material: carbon nanotube powder is purified, dispose the central impurity of powder, and carry out the discrete work of agglomerate carbon nanotube particulate;
4, the making of carbon nano-tube slurry: the carbon nanotube powder after at first will dispersing, a small amount of graphite slurry mix, and then mixed slurry and photoresists are stirred in together, and stir evenly, and form the carbon nano-tube slurry of printing usefulness;
5, the printing of carbon nanotube cathod pattern:, the carbon nano-tube slurry is printed onto above the negative electrode bus (2) in conjunction with silk-screen printing technique; Carbon nano-tube slurry after the printing is carried out the initial stage low-temperature bake solidify (temperature: 80 ℃, duration: 30 minutes);
6, the exposure of carbon nanotube cathod slurry: the carbon nanotube cathod slurry on the target substrate glasses (1) exposes; The light source that uses is ultraviolet irradiation;
7, the development of carbon nanotube cathod slurry: the carbon nanotube cathod slurry through UV-irradiation is developed.Under the situation of using negative photoresist, the place of being crossed by UV-irradiation will be retained, and the place of not crossed by UV-irradiation, its photoresists can lose efficacy, be developed liquid and get rid of, be stirred in its photoresists central carbon nano-tube and graphite slurry and also can remove thereupon; If use positive photoresist, then situation is opposite;
8, the high-temperature baking of carbon nanotube cathod slurry: the carbon nanotube cathod slurry that developed is carried out high-temperature baking; Baking temperature is 450 ℃, and the retention time is 30 minutes;
9, the reprocessing of carbon nanotube cathod (3): high-temperature baking is crossed carbon nanotube cathod carry out conventional friction reprocessing, in the hope of further improving the pattern of carbon nanotube cathod (3).

Claims (5)

1, a kind of manufacture craft of carbon nanotube cathode material is characterized in that: comprise following processing step:
1), the scribing of cathode substrate glass (1): whole plate glass is carried out scribing;
2), the making of negative electrode bus (2): go up evaporation one deck tin indium oxide thin layer at cathode substrate glass (1); Tin indium oxide thin layer to evaporation carries out photoetching, forms negative electrode bus (2);
3), the preparation of carbon nanotube powders powder material: carbon nanotube powder is purified, dispose the central impurity of powder, and carry out the discrete work of agglomerate carbon nanotube particulate;
4), the making of carbon nano-tube slurry: the carbon nanotube powder after at first will dispersing, a small amount of graphite slurry mix, and then mixed slurry and photoresists are stirred in together, and stir evenly, and form the carbon nano-tube slurry of printing usefulness;
5), the printing of carbon nanotube cathod pattern:, the carbon nano-tube slurry is printed onto above the negative electrode bus (2) in conjunction with silk-screen printing technique; Carbon nano-tube slurry after the printing is carried out the initial stage low-temperature bake solidify temperature: 80 ℃, the duration: 30 minutes;
6), the exposure of carbon nanotube cathod slurry: the carbon nanotube cathod slurry on the target substrate glasses (1) exposes; The light source that uses is ultraviolet irradiation;
7), the development of carbon nanotube cathod slurry: the carbon nanotube cathod slurry through UV-irradiation is developed.Under the situation of using negative photoresist, the place of being crossed by UV-irradiation will be retained, and the place of not crossed by UV-irradiation, its photoresists can lose efficacy, be developed liquid and get rid of, be stirred in its photoresists central carbon nano-tube and graphite slurry and also can remove thereupon; If use positive photoresist, then situation is opposite;
8), the high-temperature baking of carbon nanotube cathod slurry: the carbon nanotube cathod slurry that developed is carried out high-temperature baking; Baking temperature is 450 ℃, and the retention time is 30 minutes;
9), the reprocessing of carbon nanotube cathod (3): high-temperature baking is crossed carbon nanotube cathod carry out conventional friction reprocessing, in the hope of further improving the pattern of carbon nanotube cathod (3).
2, the manufacture craft of a kind of carbon nanotube cathode material according to claim 1 is characterized in that: described carbon nanotube cathod bus is a tin indium oxide thin layer.
3, the manufacture craft of a kind of carbon nanotube cathode material according to claim 1, it is characterized in that: described carbon nanotube powder will be purified, and described carbon nano-tube paste composition has carbon nanotube powder, a small amount of graphite slurry and photoresists composition.
4, the manufacture craft of a kind of carbon nanotube cathode material according to claim 1 is characterized in that: the printing of described carbon nanotube cathod pattern is finished in conjunction with silk-screen printing technique; Described carbon nano-tube slurry exposure technology with ultraviolet light as light source; Described photoresists can be positive photoresist, also can be negative photoresist.
5, the manufacture craft of a kind of carbon nanotube cathode material according to claim 1, it is characterized in that: the carbon nanotube cathod slurry of described printing will carry out the initial stage low-temperature bake and solidify, the carbon nanotube cathod slurry of described development will carry out high-temperature baking, and described carbon nanotube cathod will carry out aftertreatment technology.
CN200510017467A 2005-03-30 2005-03-30 Process for preparing carbon nanotube cathode material Expired - Fee Related CN100580844C (en)

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Application Number Priority Date Filing Date Title
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CN100580844C CN100580844C (en) 2010-01-13

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101377991B (en) * 2008-10-09 2010-06-16 东华大学 Method for improving cathode field-induced electron emission performance of carbon nanometer tube prepared by printing method
CN101104513B (en) * 2006-07-12 2010-09-29 清华大学 Growth method for single-wall carbon nano-tube
CN103310869A (en) * 2012-03-08 2013-09-18 清华大学 Carbon nanotube slurry and preparation method thereof, and method for preparing cathode emitter with the carbon nanotube slurry

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101104513B (en) * 2006-07-12 2010-09-29 清华大学 Growth method for single-wall carbon nano-tube
CN101377991B (en) * 2008-10-09 2010-06-16 东华大学 Method for improving cathode field-induced electron emission performance of carbon nanometer tube prepared by printing method
CN103310869A (en) * 2012-03-08 2013-09-18 清华大学 Carbon nanotube slurry and preparation method thereof, and method for preparing cathode emitter with the carbon nanotube slurry
CN103310869B (en) * 2012-03-08 2016-06-08 清华大学 Carbon nano tube paste, its preparation method and adopt this carbon nano tube paste to prepare the method for cathode emitter
US10026584B2 (en) 2012-03-08 2018-07-17 Tsinghua University Method for making carbon nanotube slurry

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