CN112701023B - Preparation method of flexible transparent field emission cold cathode - Google Patents
Preparation method of flexible transparent field emission cold cathode Download PDFInfo
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- CN112701023B CN112701023B CN202011593091.6A CN202011593091A CN112701023B CN 112701023 B CN112701023 B CN 112701023B CN 202011593091 A CN202011593091 A CN 202011593091A CN 112701023 B CN112701023 B CN 112701023B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J1/00—Details of electrodes, of magnetic control means, of screens, or of the mounting or spacing thereof, common to two or more basic types of discharge tubes or lamps
- H01J1/02—Main electrodes
- H01J1/30—Cold cathodes, e.g. field-emissive cathode
- H01J1/304—Field-emissive cathodes
- H01J1/3042—Field-emissive cathodes microengineered, e.g. Spindt-type
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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
- H01J9/025—Manufacture of electrodes or electrode systems of cold cathodes of field emission cathodes
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Abstract
The invention belongs to the field of field emission cold cathodes, and provides a preparation method of a flexible transparent field emission cold cathode. The preparation method mainly comprises 4 parts of (1) depositing a conductive transparent gold film on a flexible transparent substrate; (2) attaching an AAO template on the substrate on which the gold film is deposited; (3) preparing a spindt type metal array by using a vacuum physical deposition technology; (4) and removing the AAO template. The preparation method of the flexible transparent field emission cold cathode is simple, has low cost, can be used for large-area preparation, and has wide application prospect in the fields of flexible flat panel displays and the like.
Description
Technical Field
The invention belongs to the technical field of electronic material preparation, particularly relates to a preparation method of a flexible transparent field emission cold cathode, and particularly relates to a preparation method of a flexible transparent field emission spindt cathode.
Background
The principle of field emission is that the height and width of the surface potential barrier of a material are reduced by an external electric field, and electrons pass through the surface potential barrier due to the tunnel effect to form electron emission. The field emission cold cathode can be divided into: a metal pointed cone array type represented by spindt type cathodes, a new material type represented by carbon nanotubes, transition metal oxides and the like, and the structure mainly comprises: emitter tip cone, insulating layer, conductive layer, and gate. Nowadays, the field emission cold cathode has been widely used in various fields, such as field emission display screen, which combines the advantages of cathode ray tube and liquid crystal display, and has the characteristics of clear image quality, low power consumption, long service life, fast response, etc., and in addition, it is also used in the fields of transistor, vacuum microwave tube, X-ray tube, electron microscope, etc.
With the development of flexible electronic devices, flexible cold cathode materials are also receiving attention. Compared with the traditional field emission cold cathode, the flexible cold cathode material has good emission performance and is beneficial to realizing the requirements of miniaturized design, convenient carrying and low manufacturing cost of electronic devices. Therefore, the preparation of the flexible field emission cold cathode material is of great significance for being applied to the fields of rollable displays and the like in the future.
The cold cathode, as a core component of a flexible field emission device, is one of the hot spots of current field emission research. However, the preparation method of spindt type cold cathode still has a great limitation, the traditional preparation process mostly adopts a photoetching method to prepare the array cathode, so that the integration level of the spindt type cathode array is low, the electron emission capability and the emission current density are difficult to greatly improve, if the integration level is improved, the requirement on the precision of photoetching equipment is higher, so that the cost is greatly improved, and in addition, some novel preparation methods, such as a thermal oxidation method, a chemical vapor deposition technology, an ultraviolet photoetching technology and the like, also have the defects of unstable emission performance and the like.
Therefore, the present invention uses a method of preparing a spindt type cold cathode by vacuum physical deposition technique. On the mica sheet plated with the conductive gold film, an AAO template with proper height and aperture is selected, and a good spindt tip cone is formed by controlling the metal deposition rate and utilizing the shielding effect and is applied to a cold cathode.
Disclosure of Invention
The invention aims to provide a preparation method of a flexible transparent field emission spindt cold cathode, which is simple in method, low in cost and capable of being prepared in a large area, so as to solve the problems that the current field emission cold cathode is difficult to prepare in a large area and the like.
In order to achieve the purpose, the invention adopts the following technical method:
a flexible transparent field emission cold cathode comprising: the metal array comprises a high-temperature-resistant transparent flexible substrate and a spindt type metal array deposited on the substrate. Wherein the high-temperature resistant transparent flexible substrate is a mica sheet.
A preparation method of a flexible transparent field emission cold cathode is characterized by comprising the following steps:
(1) depositing a conductive transparent gold film on a flexible transparent substrate;
(2) attaching an AAO template on the substrate on which the gold film is deposited;
(3) preparing a spindt type metal array by using a vacuum physical deposition technology;
(4) and removing the AAO template to obtain the field emission cathode material.
As a further improvement of the present invention, a pulsed laser deposition technique is used to deposit a conductive film on a substrate.
As a further improved technical scheme of the invention, a dropper is used for sucking a proper amount of ethanol, the ethanol is dripped on the substrate, and the AAO template is attached to the substrate before the ethanol is completely volatilized.
As a further improved technical scheme of the invention, a spindt type metal array is prepared on a substrate by using a magnetron sputtering technology, a pulse laser deposition technology, an electron beam evaporation technology and the like. The deposited spindt-type metal can be selected from metals with smaller work function, such as Ti, Wu and the like, and the shape of the metal is spindt type, which is beneficial to the emission of electrons;
as a further improvement of the invention, when the spindt type metal array is deposited, the substrate temperature is controlled to be 300-500 ℃, the beam current of the electron beam is controlled to be 100-200 mA, and the deposition rate is controlled to be 1-2 nm/s, so that the good spindt type metal array can be obtained.
As a further improvement of the invention, an adhesive tape bonding method is adopted to directly stick off the AAO, so that the influence of the traditional solution corrosion method on spindt type metal is avoided.
The beneficial effects of the invention are: by utilizing the AAO template and using the vacuum physical deposition technology, the flexible transparent field emission spindt cathode can be manufactured in a large area, and the conventional complex preparation method is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a flow chart of a method of making a flexible transparent field emission cathode according to the present invention;
FIG. 2 is a pictorial representation of the application of an AAO film of the present invention to a substrate having an electrically conductive layer;
FIG. 3 is a schematic diagram of the principle of the present invention for forming spindt type metal using an AAO template;
FIG. 4 is a cross-sectional view of a spindt-type metal array obtained by deposition of an AAO film and the AAO film peeled off in accordance with the present invention;
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the present invention is described in detail below with reference to the accompanying drawings and detailed description.
The invention provides a preparation method of a flexible transparent field emission cold cathode, which comprises the steps of depositing a conductive transparent gold film on a flexible transparent substrate as shown in figure 1; attaching an AAO template on the substrate on which the gold film is deposited; preparing a spindt type metal array by using a vacuum physical deposition technology; and removing the AAO template.
In the specific implementation, the used high-temperature-resistant transparent flexible material is a mica sheet, and has better flexibility and light transmission; the metal of the deposited conductive layer is Au, and the data show that the Au has higher conductivity and good light transmittance in a certain thickness range.
Further, in the specific implementation, a proper amount of ethanol is sucked by a dropper, and is dripped on the substrate plated with the conductive layer, and before the ethanol is completely volatilized, the AAO template is attached to the substrate, and the effect is shown in FIG. 2 (the lower left corner is an enlarged view of the AAO template on the substrate, and the upper right corner is an enlarged view of the deposited Au conductive layer).
Further, in the present invention, as shown in fig. 3, the principle of forming the spindt-type metal array based on the AAO template is that, due to the hole-like structure of the AAO template and the shielding effect, when metal is deposited into the AAO template, a pointed cone shape is formed. FIG. 4 is a cross-sectional view of the prepared spindt-type metal array, and from the upper view, the spindt-type metal array is nested in the AAO template, and the diameter of the spindt-type metal is about 250nm and is consistent with the size of the AAO template. The lower figure shows that the AAO template has been partially filled after stripping, with the vacated pointed cone portions, i.e., the metal pointed cones deposited on the substrate.
The electron beam evaporation technology used by the invention comprises the following specific steps: mounting a target material in a cathode target groove of an electron beam evaporation device, placing a substrate which is attached with an AAO template and contains a conductive layer into a sample table for fixing, and shielding the sample table by a baffle; the device is pumped, a mechanical pump is firstly opened, an angle valve is opened, the vacuum coating chamber is pre-pumped, the angle valve is closed after the vacuum degree is less than 10Pa, an electromagnetic valve is opened, a molecular pump is opened, and a gate valve is opened after the vacuum degree is less than 1 Pa; and turning on a temperature control power supply, and heating the substrate to 300-500 ℃. When the internal pressure of the device is less than 5 x 10-4 pa; turning on a power supply of an electron beam evaporation source, adjusting 'preset' and preheating for 2-3 minutes; opening a high-voltage button, adjusting the light spot to the center of the target, and slowly increasing the beam current to 100-200 mA; and after the deposition rate is stabilized at 1-2 nm/s, opening the baffle plate to perform deposition.
The invention uses a magnetron sputtering technology (PLD), which comprises the following steps: placing the target material on a target groove, and fixing the sample on a sample table; performing vacuum pumping on the device until the pressure is reduced to below 10^ -4 KPa; and turning on the laser, setting a mode, adjusting the laser position and carrying out sputtering deposition.
The invention utilizes the AAO template and the shielding effect to deposit the spindt tip cone on the mica sheet with the Au conducting layer, can obtain a field emission cathode with more uniformity and larger area, and improves the prior method which has high cost and is difficult to prepare in large scale. Meanwhile, the field emission cathode manufactured by the method has good light transmission and flexibility, so that the application range of the field emission cathode is greatly expanded, and the method has great practical significance.
The following detailed description is made of a method for manufacturing a flexible transparent field emission cold cathode by using specific examples:
example 1:
the high-temperature resistant transparent flexible substrate adopts a mica sheet with the side length of 1cm and the thickness of 0.1mm, the mica sheet is subjected to ultrasonic cleaning for 15min by using absolute ethyl alcohol, the mica sheet is taken out and dried, and then is fixed on a PLD sample table, a gold target is arranged on a target groove, a mechanical pump is started, Ar gas is introduced, a gate valve and a molecular pump are opened, and the device is subjected to vacuum air suction until the pressure is reduced to be below 10^ 4 KPa; and (3) turning on the laser, setting a mode, adjusting the laser position, and sputtering for 30 min. Taking out the mica sheet deposited with the Au conductive layer, sucking a proper amount of ethanol by a dropper, dropping the ethanol on the central part of the mica sheet, and attaching the AAO template to the substrate by using tweezers before the ethanol is completely volatilized. Waiting for completely drying, fixing the substrate on a sample table, placing the sample table into a vacuum coating chamber of an electron beam evaporation device, placing a Ti target into a cathode target groove, exhausting the device to ensure that the pressure in the device is less than 5 x 10-4 pa and the temperature is 300 ℃, turning on a power supply of the electron beam evaporation source, adjusting the preset to ensure that the current of a gun filament is 0.2-0.3A, and adjusting the preset value to 0.5A after preheating for 3 minutes; adjusting a high-voltage selection switch to 6KV, adjusting a light spot to the center of the target by pressing a high-voltage knob, slowly increasing the beam current to 100-200 mA, and controlling the deposition rate to 1-2 nm/s; the shutter was opened for deposition and the film thickness was recorded by a film thickness meter for 500nm deposition. And taking out after the deposition is finished, and using an adhesive tape to stick off the AAO template to obtain the flexible transparent field emission cold cathode.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A preparation method of a flexible transparent field emission cold cathode is characterized by comprising the following steps:
(1) depositing a conductive transparent gold film on a flexible transparent substrate;
(2) attaching an AAO template on the substrate on which the gold film is deposited;
(3) preparing a spindt type metal array by using a vacuum physical deposition technology;
(4) and removing the AAO template to obtain the field emission cathode material.
2. The method of claim 1, wherein the flexible transparent field emission cold cathode comprises: the metal array comprises a high-temperature-resistant flexible transparent substrate, a conductive transparent gold film and a spindt type metal array deposited on the conductive transparent gold film.
3. The method for preparing the flexible transparent field emission cold cathode according to claim 1 or 2, wherein the substrate material is a high temperature-resistant flexible transparent material.
4. The method for preparing a flexible transparent field emission cold cathode according to claim 1 or 2, wherein in the step (1), the substrate is ultrasonically cleaned with ethanol.
5. The method for preparing a flexible transparent field emission cold cathode according to claim 1 or 2, wherein in the step (2), a proper amount of ethanol is sucked by a dropper, and is dropped on the substrate, and before the ethanol is completely volatilized, the AAO template is attached to the substrate.
6. The method for preparing a flexible transparent field emission cold cathode according to claim 1 or 2, wherein in the step (3), the deposition technique is any one of a magnetron sputtering technique, a pulsed laser deposition technique or an electron beam evaporation technique.
7. The method according to claim 1 or 2, wherein in step (3), the metal with lower work function is selected from the metals deposited and has a spindt type shape.
8. The method for preparing a flexible transparent field emission cold cathode according to claim 1 or 2, wherein in the step (4), the AAO template is removed by using an adhesive tape to obtain the flexible transparent field emission cold cathode.
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| US4990766A (en) * | 1989-05-22 | 1991-02-05 | Murasa International | Solid state electron amplifier |
| US5507676A (en) * | 1994-11-18 | 1996-04-16 | Texas Instruments Incorporated | Cluster arrangement of field emission microtips on ballast layer |
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