CN111261473B - Method for manufacturing single one-dimensional nano-structure field emission cold cathode - Google Patents
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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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- H—ELECTRICITY
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- 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
Abstract
The invention discloses a method for manufacturing a single one-dimensional nano-structure field emission cold cathode, which utilizes the local self-heating effect of a nano-structure body to weld a single one-dimensional nano-structure growing on a conductive substrate on a micro-nano conductive matrix so as to form ohmic contact joint; and cutting the single one-dimensional nanostructure by using a metal probe in an electric melting mode, so that the single one-dimensional nanostructure is separated from the conductive substrate, and a single one-dimensional nanostructure cold cathode based on the micro-nano conductive matrix is formed. The manufacturing method is simple and universal, and can manufacture the single one-dimensional nano-structure cold cathode on the micro-nano conductive substrates of different materials and different shapes based on different types of one-dimensional nano materials. The single cold cathode with one-dimensional nano structure is applied to high-brightness and coherent electron sources, and has important application in electron beam lithography, electron microscopes, scientific research devices and the like.
Description
Technical Field
The invention relates to the technical field of nano material processing technology and vacuum microelectronics, in particular to a method for manufacturing a single field emission cold cathode with a one-dimensional nano structure.
Background
The one-dimensional nanostructure has attracted attention in the fields of novel nanoelectronic devices, optoelectronic devices, energy storage, biological and chemical sensing, field electron emission and the like due to excellent electrical, optical, thermal and magnetic properties of the one-dimensional nanostructure. The one-dimensional nano structure has the characteristic of high length-diameter ratio, so that the one-dimensional nano structure has the advantage of being unique in the application of field electron emission devices.
Field electron emission (field emission for short) refers to a physical process in which electrons inside a material can tunnel through a surface barrier into a vacuum by applying a strong electric field to the surface of a solid material to narrow the width and lower the height of the surface barrier of the material. Compared with the traditional hot cathode electron source, the cold cathode electron source based on the field emission principle has the advantages of quick response, low power consumption, high current density and the like.
The high length-diameter ratio of the high value of the one-dimensional nano structure brings that the emission end face has strong electric field enhancement, can realize low electric field and high-efficiency electron emission, and is applied to a field emission cold cathode. The single cold cathode with the one-dimensional nano structure can realize a high-brightness and coherent electron source, and has important application in electron beam lithography, electron microscopes, scientific research and the like. How to controllably prepare the single one-dimensional nano structure on the micro-nano electrode is a key technology of the cold cathode of the single one-dimensional nano structure.
At present, the method for manufacturing the single cold cathode with the one-dimensional nano structure mainly has two ways: firstly, a single one-dimensional nano structure is grown by depositing a catalyst on a metal or semiconductor tip structure in a self-assembly positioning growth mode, and secondly, the single one-dimensional nano structure is prepared by directly processing a body in an etching mode.
In the method, the former has the problems that the substrate material needs to meet the growth condition of the nano structure and the controllability of the nano structure preparation is poor, and the latter has the problems that the material selection range of the processing technology is small and the manufacturing process is complex.
Disclosure of Invention
The invention provides a method for manufacturing a single one-dimensional nanostructure field emission cold cathode, aiming at solving the problems of poor controllability, harsh preparation conditions, small material selection range and complex manufacturing process in the prior art for preparing the single one-dimensional nanostructure field emission cold cathode.
In order to achieve the purpose of the invention, the technical scheme is as follows: a single one-dimensional nanostructure field emission cold cathode manufacturing method utilizes a local self-heating effect of a nanostructure to weld a single one-dimensional nanostructure growing on a conductive substrate on a micro-nano conductive matrix to form ohmic contact joint; and cutting the single one-dimensional nanostructure by using a metal probe in an electric melting mode, so that the single one-dimensional nanostructure is separated from the conductive substrate, and a single one-dimensional nanostructure cold cathode based on the micro-nano conductive matrix is formed.
The local self-heating adopts a current joule heating mode, and current is conducted in the micro-nano conductive matrix with non-uniform resistance distribution to generate the non-uniform distribution joule heating so as to obtain a local heating effect, so that the contact position between the micro-nano conductive matrix and a single one-dimensional nano structure is the largest resistance area and the generated joule heating is the largest, and therefore welding is formed.
Preferably, the specific steps of the manufacturing method are as follows:
s1: manufacturing a micro-nano conductive substrate by adopting a material with conductivity;
s2: preparing a conductive one-dimensional nano structure on a conductive substrate as a field emission material;
s3: the prepared micro-nano conductive matrix is in van der Waals contact with one end of a single one-dimensional nano structure;
s4: irradiating the contact position of the micro-nano conductive matrix and the single one-dimensional nanostructure by using an electron beam, applying voltage between the micro-nano conductive matrix and the single one-dimensional nanostructure, generating current, generating local high joule heat at the contact position of the micro-nano conductive matrix and the single one-dimensional nanostructure, and heating a contact area in situ to fuse and joint the single one-dimensional nanostructure and the micro-nano conductive matrix to form ohmic contact joint;
s5: and cutting the single one-dimensional nanostructure by using a metal probe in an electric melting mode, so that the single one-dimensional nanostructure is separated from the conductive substrate, and a single one-dimensional nanostructure cold cathode based on the micro-nano conductive matrix is formed.
Further, the micro-nano conductive matrix is prepared by adopting a conductive material with the melting point of over 800 ℃,
still further, the conductive material comprises gold, silver, iron, chromium, tungsten and molybdenum.
Furthermore, the joint between the single one-dimensional nano structure and the micro-nano conductive substrate is combined in a chemical bond mode to form connection with ohmic contact characteristics.
Further, after the step S4 and before the step S5, in order to improve the mechanical contact strength between the single one-dimensional nanostructure and the micro-nano conductive substrate, the bonding position is irradiated with an electron beam, and a deposit is deposited in the contact area by electron beam induction.
Still further, the deposit comprises carbon, carbide, platinum, gold, tungsten; the thickness of the deposit is larger than the diameter of the single one-dimensional nano structure.
The invention has the following beneficial effects:
according to the manufacturing method, a single one-dimensional nanostructure is welded on the micro-nano conductive substrate by utilizing the local self-heating effect of the nanostructure, so that ohmic contact joint is formed, and the included angle between the single one-dimensional nanostructure and the micro-nano conductive substrate can be controlled; the electron beam is used for inducing the sediment to be deposited in the contact area, so that the mechanical contact strength between the single one-dimensional nano structure and the micro-nano conductive substrate can be improved; and a metal probe is utilized to intercept the single one-dimensional nano structure in an electric melting mode, so that the length of the single one-dimensional nano structure is controlled. The manufacturing method is simple and has universality, and the single one-dimensional nano-structure cold cathode can be manufactured on the micro-nano conductive substrates of different materials and different shapes based on different types of one-dimensional nano materials. The single cold cathode with one-dimensional nano structure is applied to high-brightness and coherent electron sources, and has important application in electron beam lithography, electron microscopes, scientific research devices and the like.
Drawings
Fig. 1 is a schematic operation flow diagram of the manufacturing method described in embodiment 1.
The structure comprises a single one-dimensional nanostructure, a 2-conductive substrate, a 3-micro-nano conductive matrix, a 4-electron beam, a 5-voltage source, a 6-Pian meter, a 7-ohmic contact joint area and 8-sediments covering the joint.
FIG. 2 is a single LaB of example 16And characterizing the appearance and electrical characteristics of the nanowire cold cathode.
Wherein, FIG. 2(a) is a single LaB6And (b) an SEM image of the nanowire cold cathode, wherein an I-V curve and an inset graph of the conductivity characterization graph are structural diagrams of corresponding conductivity tests.
FIG. 3 is a single LaB of example 16And (4) characterizing the field emission characteristics of the nanowire cold cathode.
Fig. 3(a) is a field emission I-V characteristic curve, fig. 3(b) is a F-N curve corresponding to fig. 3(a), fig. 3(c) is a stability test result for a period of 1000 seconds, and fig. 3(d) is a corresponding field emission image.
Detailed Description
The invention is described in detail below with reference to the drawings and the detailed description.
Example 1
As shown in fig. 1, a method for manufacturing a single one-dimensional nanostructure field emission cold cathode, in which a local self-heating effect of a nanostructure is utilized to fuse a single one-dimensional nanostructure grown on a conductive substrate on a micro-nano conductive substrate to form ohmic contact joint; and cutting the single one-dimensional nanostructure by using a metal probe in an electric melting mode, so that the single one-dimensional nanostructure is separated from the conductive substrate, and a single one-dimensional nanostructure cold cathode based on the micro-nano conductive matrix is formed.
The local self-heating adopts a current joule heating mode, and current is conducted in the micro-nano conductive matrix with non-uniform resistance distribution to generate non-uniform distribution joule heat to obtain a local heating effect, so that the contact position between the micro-nano conductive matrix and the single one-dimensional nano structure is the largest resistance area and the generated joule heat is the largest, and welding is formed.
In a specific embodiment, the manufacturing method comprises the following specific steps:
step S1: a micro-nano conductive matrix 3 is made of a conductive material;
specifically, a metal sharp needle is selected as a micro-nano structure substrate 3, a tungsten filament is used as a preparation material of the metal sharp needle, a tungsten needle point with the tip diameter within a submicron range is prepared by adopting an electrochemical corrosion method and using 2mol/L sodium hydroxide solution, and then the needle point is washed by deionized water. The micro-nano structure matrix can also be arranged into structures with other shapes, such as columnar structures and the like.
And (3) operating the two prepared tungsten needles by using a nano step control device assembled in a Scanning Electron Microscope (SEM) cavity to enable the tips of the tungsten needles to be in contact with each other, and applying voltage by a voltage source to generate large current to flow through the contact position, so that the tips of the tungsten needles sharpen and remove an oxide layer on the surface. In the embodiment, 3 tungsten needles are prepared, wherein one tungsten needle is used as the micro-nano conductive substrate 3, and the other two tungsten needles are used as metal probes.
The micro-nano conductive substrate 3 is prepared from a conductive material with a melting point of over 800 ℃, and the conductive material includes, but is not limited to, gold, silver, iron, chromium, tungsten and molybdenum.
Step S2: preparing a one-dimensional nanostructure with good conductivity on a conductive substrate 2 as a field emission material; in this embodiment, the single one-dimensional nanostructure 1 is a single LaB6A nanowire.
S3: a nano stepping control device is utilized to control a micro-nano conductive matrix 3 to contact with one end of a single one-dimensional nano structure 1 growing on a conductive substrate 2 to form Van der Waals contact, and the axial directions of the single one-dimensional nano structure 1 and the micro-nano conductive matrix 3 are kept parallel, as shown by a serial number (r) in figure 1; the required angle between the micro-nano conductive matrix 3 and the single one-dimensional nano structure 1 can be controlled;
step S4: when the vacuum degree in the SEM cavity reaches 1 multiplied by 10-3When Pa, irradiating the contact position of the micro-nano conductive matrix 3 and the single one-dimensional nano structure 1 by an electron beam 4 with the acceleration voltage of 10-20kV, applying a proper voltage between the micro-nano conductive matrix 3 and the conductive substrate 2 by a voltage source 5, generating current between the micro-nano conductive matrix 3 and the single one-dimensional nano structure 1 by the applied voltage, and enabling the current flowing through the single one-dimensional nano structure 1 and a contact point to be more than 5 muA, so that local high joule heat is generated at the contact position of the micro-nano conductive matrix and the single one-dimensional nano structure, and fusing and jointing the single one-dimensional nano structure 1 and the micro-nano conductive matrix 3 by heating a thermal contact area in situ to form ohmic contact joint; as shown by the numbers c and c in fig. 1.
S5: and (3) operating the other two tungsten needles as metal probes by using a nano stepping control device, fusing the tungsten needles at a proper position of the single one-dimensional nano structure 1 in a current fusing manner to intercept the single one-dimensional nano structure 1, and separating the single one-dimensional nano structure 1 from the conductive substrate 2, wherein the tungsten needles are shown as a serial number (v) in fig. 1. And then taking out the micro-nano conductive matrix from the SEM cavity to obtain the single one-dimensional nano structure cold cathode based on the micro-nano conductive matrix, as shown by the sequence number (sixty) in the figure 1.
In a specific embodiment, the joint between the single one-dimensional nanostructure and the micro-nano conductive substrate is formed by means of chemical bond combination, so that ohmic contact connection is formed.
In a specific embodiment, after the step S4 and before the step S5, in order to improve the mechanical contact strength between the single one-dimensional nanostructure 1 and the micro-nano conductive substrate 3, the irradiation of the bonding position with the electron beam is continued, and the electron beam 4 is used to induce the deposition of the deposit 8 on the bonding point so as to improve the mechanical contact characteristics of the bonding point. This process continues for more than 2 hours until finally the deposit 8 completely covers the surface of the single one-dimensional nanostructure of the junction, as indicated by the number (r) in figure 1.
In a specific embodiment, the deposit 8 is an amorphous carbon layer including, but not limited to, carbon, carbide, platinum, gold, tungsten; the thickness of the deposit 8 is larger than the diameter of a single one-dimensional nano structure.
The single LaB based on the tungsten needle base body manufactured by the steps is6The nanowire cold cathode is used for carrying out appearance, electrical property and field emission characteristic characterization to illustrate the feasibility of the technical scheme.
This example uses SEM to align single LaB6The morphology of the nanowire cold cathode was characterized as shown in fig. 2 (a). In one aspect, a single LaB6The nanowire is welded on the tip of the tungsten needle in a linear shape and is kept in a parallel state with the axial direction of the tungsten needle; on the other hand, a single LaB at the bonding site6The nanowires are completely covered by the amorphous carbon layer so that the mechanical contact properties of the joint are ensured. Vacuum degree in the cavity of SEM is 5 × 10-4At Pa, the electrical contact characteristics of the joint structure were characterized using a peakley meter, model Keithley 6487, the test structure of which is shown in the inset of fig. 2 (b). FIG. 2(b) shows a single LaB based on a tungsten needle matrix6The characterization result of the electrical characteristics of the nanowire cold cathode can be seen from the figure, and a single LaB6A good ohmic contact is established between the nanowire and the tungsten tip.
A single LaB6The nanowire cold cathode electron source is placed in an ultrahigh vacuum field emission test system, and when the vacuum degree of the system reaches5×10-6When the pressure is Pa, the tungsten needle substrate is heated by a direct current voltage source, so that the temperature of the tungsten needle substrate is kept at about 400 ℃ to remove a single LaB6And gas molecules are adsorbed on the surface of the nanowire cold cathode. After the heating process is finished, the ITO-coated fluorescent screen is used as an anode to carry out single LaB6The field emission characteristics of the nanowire cold cathode are characterized, and the vacuum degree of the system is 2.6 multiplied by 10-6Pa. Fig. 3(a) and 3(b) show the I-V characteristic curve of field emission and the corresponding F-N characteristic curve, and it can be seen that the electron emission behavior satisfies the field electron emission principle. FIG. 3(c) shows a single LaB6The stability test result of the emitting current of the nanowire cold cathode can be found through calculation that a single LaB is under the constant voltage of 1900V6The average current of the nanowire cold cathode reaches 680nA, and the current fluctuation is about 2.17%. FIG. 3(d) shows a single LaB6As can be seen from the figure, the diameter of the light spot of the field emission image of the nanowire cold cathode is less than 1mm, and the brightness of the electron beam spot is uniformly distributed.
In summary, the present embodiment provides a method for manufacturing a single one-dimensional nanostructure field emission cold cathode on a micro-nano conductive substrate based on a local self-heating effect and an electron beam induced deposition effect, in which a single one-dimensional nanostructure is welded on the micro-nano conductive substrate by using the local self-heating effect of the nanostructure to form an ohmic contact joint, and a deposit is induced by using an electron beam to deposit on a contact region, so as to enhance the mechanical contact strength of the joint.
The main advantages of the manufacturing method described in this embodiment include:
the preparation method is simple and universal, and can realize the preparation of single one-dimensional nano structures of different types of materials on different conductive micro-nano substrates;
secondly, the manufacturing method can control the length of the single one-dimensional nano structure and the included angle between the single one-dimensional nano structure and the micro-nano conductive substrate at will;
and thirdly, the manufacturing method can control the area of the welded area, and other key areas of the electron source cannot be polluted in the welding process.
The advantages can ensure the repeatability and stability of the prepared single one-dimensional nano-structure cold cathode, and can be applied to practical equipment and devices as an electron source.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (7)
1. A method for manufacturing a single field emission cold cathode with a one-dimensional nano structure is characterized by comprising the following steps: the manufacturing method utilizes the local self-heating effect of the nanostructure body to weld a single one-dimensional nanostructure growing on a conductive substrate on a micro-nano conductive substrate so as to form ohmic contact joint; cutting the single one-dimensional nanostructure by using a metal probe in an electric melting mode, so that the single one-dimensional nanostructure is separated from the conductive substrate, and a single one-dimensional nanostructure cold cathode based on the micro-nano conductive matrix is formed;
irradiating the contact position of the micro-nano conductive matrix and the single one-dimensional nanostructure by using an electron beam, applying voltage between the micro-nano conductive matrix and the single one-dimensional nanostructure, generating current, generating local high Joule heat at the contact position of the micro-nano conductive matrix and the single one-dimensional nanostructure, and heating the contact area in situ to fuse and joint the single one-dimensional nanostructure and the micro-nano conductive matrix to form ohmic contact joint.
2. The method for manufacturing a single one-dimensional nanostructure field emission cold cathode according to claim 1, wherein the method comprises the following steps: the manufacturing method comprises the following specific steps:
s1: manufacturing a micro-nano conductive substrate by adopting a material with conductivity;
s2: preparing a conductive one-dimensional nano structure on a conductive substrate as a field emission material;
s3: forming Van der Waals contact between the manufactured micro-nano conductive matrix and one end of the single one-dimensional nano structure;
s4: irradiating the contact position of the micro-nano conductive matrix and the single one-dimensional nanostructure by using an electron beam, applying voltage between the micro-nano conductive matrix and the single one-dimensional nanostructure, generating current, generating local high joule heat at the contact position of the micro-nano conductive matrix and the single one-dimensional nanostructure, and heating a contact area in situ to fuse and joint the single one-dimensional nanostructure and the micro-nano conductive matrix to form ohmic contact joint;
s5: and cutting the single one-dimensional nanostructure by using a metal probe in an electric melting mode, so that the single one-dimensional nanostructure is separated from the conductive substrate, and a single one-dimensional nanostructure cold cathode based on the micro-nano conductive matrix is formed.
3. The method for manufacturing a single one-dimensional nanostructure field emission cold cathode according to any one of claims 1 or 2, wherein: the micro-nano conductive matrix is prepared from a conductive material with a melting point of over 800 ℃.
4. The method for manufacturing a single one-dimensional nanostructure field emission cold cathode according to claim 3, wherein: the conductive material comprises one of gold, silver, iron, chromium, tungsten and molybdenum.
5. The method for manufacturing a single one-dimensional nanostructure field emission cold cathode according to any one of claims 1 or 2, wherein: the joint between the single one-dimensional nano structure and the micro-nano conductive substrate is combined in a chemical bond mode to form connection with ohmic contact characteristics.
6. The method for manufacturing a single one-dimensional nanostructure field emission cold cathode according to claim 2, wherein: after the step S4 and before the step S5, in order to improve the mechanical contact strength between the single one-dimensional nanostructure and the micro-nano conductive substrate, the bonding position is irradiated by an electron beam, and deposits are induced on the contact area by the electron beam.
7. The method for manufacturing a single one-dimensional nanostructure field emission cold cathode according to claim 6, wherein: the deposit comprises one of carbon, carbide, platinum, gold and tungsten; the thickness of the deposit is larger than the diameter of the single one-dimensional nano structure.
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| JP4259023B2 (en) * | 2002-02-05 | 2009-04-30 | 富士ゼロックス株式会社 | Carbon nanotube device manufacturing method and carbon nanotube device |
| US20090045720A1 (en) * | 2005-11-10 | 2009-02-19 | Eun Kyung Lee | Method for producing nanowires using porous glass template, and multi-probe, field emission tip and devices employing the nanowires |
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| US9852870B2 (en) * | 2011-05-23 | 2017-12-26 | Corporation For National Research Initiatives | Method for the fabrication of electron field emission devices including carbon nanotube field electron emisson devices |
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