CN115841933B - Cold cathode pointed cone and preparation method thereof, cold cathode pointed cone array and preparation method thereof - Google Patents
Cold cathode pointed cone and preparation method thereof, cold cathode pointed cone array and preparation method thereof Download PDFInfo
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- CN115841933B CN115841933B CN202310160127.9A CN202310160127A CN115841933B CN 115841933 B CN115841933 B CN 115841933B CN 202310160127 A CN202310160127 A CN 202310160127A CN 115841933 B CN115841933 B CN 115841933B
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Abstract
The invention relates to the technical field of cold cathode pointed cones, in particular to a cold cathode pointed cone, a preparation method thereof, a cold cathode pointed cone array and a preparation method thereof. The preparation method of the cold cathode pointed cone comprises the following steps: bombarding the surface of a workpiece by utilizing beam current emitted by an electron microscope, and processing an annular groove on the surface of the workpiece along the depth direction, wherein a column body is formed inside the annular groove; and in the direction from the top to the bottom of the cylinder, processing the cylinder layer by utilizing the beam emitted by the electron microscope, and obtaining the cold cathode pointed cone by increasing and then decreasing the energy intensity of the beam emitted by the electron microscope. The invention adopts the double-beam electron microscope to prepare the cold cathode pointed cone, can realize the integration of in-situ processing and detection, and has high yield.
Description
Technical Field
The invention relates to the technical field of cold cathode pointed cones, in particular to a cold cathode pointed cone, a preparation method thereof, a cold cathode pointed cone array and a preparation method thereof.
Background
The cold cathode spike experiment needs to realize the simulation of sample interface detonation equivalent, the deformation of the conical curved surface section in the top free curved surface extrusion process is close to the real state of impact load, and the maximum pressure and the most stable stress state are required to be obtained in a unit area, so that the macroscopic scale of a conical cylindrical surface experiment modulation sample is smaller and smaller, and the initial 120 mu m is reduced to the current inner cylindrical surface diameter of less than or equal to 20 mu m so as to accommodate more equivalent impact load in an outer cylindrical surface; the configuration of a common nano-needle pressing experimental sample is changed from a plane to an outward curved surface modulation structure, and the modulation structure is more complex; the modulation structure is divided into a long wave structure and a short wave structure, and the long wave modulation structure and the short wave modulation structure are respectively used for researching deformation phenomena caused by pressure and spike deformation conditions under the action of extreme environment and external column surface impact load; the typical wavelength of the long wave structure is 1mm, the amplitude is 0.1mm, the typical wavelength of the short wave structure is 50 mu m, the amplitude is 3 mu m, the roughness of the processing surface is less than or equal to 10nm, the profile is less than or equal to 1 mu m, and the defects are controlled. The current common ultra-precise turning technology is difficult to meet the processing requirement of a new complex curved surface outer surface modulation structure.
In the aspect of stress control regulation and control, the problem of deformation and even fracture of a complex structure in a small space caused by cutting stress is difficult to solve by the traditional processing means, and in the aspect of ultra-precise slotting, the roughness and the smoothness of the surface of a complex curved surface in the small space are difficult to ensure.
In view of this, the present invention has been made.
Disclosure of Invention
An object of the present invention is to provide a method for preparing a cold cathode cone, so as to solve the above technical problems.
The invention also aims to provide the cold cathode pointed cone prepared by the preparation method of the cold cathode pointed cone.
The invention also aims to provide a preparation method of the cold cathode pointed cone array.
The invention also aims to provide the cold cathode pointed cone array prepared by the preparation method of the cold cathode pointed cone array.
In order to achieve the above object of the present invention, the following technical solutions are specifically adopted:
the preparation method of the cold cathode pointed cone comprises the following steps:
bombarding the surface of a workpiece by utilizing beam current emitted by an electron microscope, and processing an annular groove on the surface of the workpiece along the depth direction, wherein a column body is formed inside the annular groove; and in the direction from the top to the bottom of the cylinder, processing the cylinder layer by utilizing the beam emitted by the electron microscope, and obtaining the cold cathode pointed cone by increasing and then decreasing the energy intensity of the beam emitted by the electron microscope.
In one embodiment, before the bombarding the surface of the workpiece with the beam emitted by the electron microscope, the method further includes: carrying out hot rolling treatment on the workpiece; the hot rolling treatment specifically comprises the following steps: and carrying out heat treatment on the original workpiece, and then carrying out rolling treatment.
In one embodiment, the temperature of the heat treatment is 200-400 ℃, and the time of the heat treatment is 1-4 hours.
In one embodiment, the pressure of the rolling treatment is 18-22 MPa, and the time of the rolling treatment is 25-35 min.
In one embodiment, the hot roll treatment is performed in an inert atmosphere.
In one embodiment, the hot rolled workpiece obtained after the hot rolling treatment is naturally cooled, and then the electron microscope is adopted to process the naturally cooled workpiece.
In one embodiment, the workpiece is a polycrystalline material.
In one embodiment, the diameter of the outer circle of the annular groove is 5-12 μm, and the diameter of the inner circle of the annular groove is 1-3 μm.
In one embodiment, the workpiece is located on a stage of the electron microscope; when the annular groove is machined on the surface of the workpiece, a beam emission point of the electron microscope is positioned above the workpiece; and the beam emitted by the electron microscope is perpendicular to the surface of the workpiece, and the beam emission point and the workpiece generate relative motion by moving the objective table so as to form the annular groove.
In one embodiment, when the cylinder is processed, the beam emission point of the electron microscope is positioned right above the top end of the cylinder; the beam emission point and the workpiece are relatively static, and the cylinder is processed by changing the emission direction of the beam emission point.
In one embodiment, during the layer-by-layer processing, the beam bombardment point of the electron microscope is in a serpentine position on the surface of the workpiece.
In one embodiment, in the layer-by-layer processing, the processing depth of each layer is 8-12 atomic layers.
In one embodiment, during the layer-by-layer processing, each layer is stopped for 0.3-1.8 mu s after processing, and the chips generated after processing are removed by vacuumizing.
In one embodiment, the beam energy is maximized during the top to bottom machining of the cylinder when the machining depth is two-thirds to three-quarters of the total depth.
In one embodiment, the beam energy of the initial end and the final end is (4-4.5) x 10 in the process of processing the column from the top to the bottom -7 pC/μm 2 The method comprises the steps of carrying out a first treatment on the surface of the The range of the maximum beam energy is (8.5-8.8) x 10 -7 pC/μm 2 。
The cold cathode pointed cone is prepared by the preparation method of the cold cathode pointed cone.
In one embodiment, the height of the cold cathode pointed cone is 8-15 μm, the taper angle is 5-20 degrees, and the tip diameter of the cold cathode pointed cone is 20-100 nm.
The preparation method of the cold cathode pointed cone array comprises the following steps:
(a) Preparing a cold cathode pointed cone according to the preparation method of the cold cathode pointed cone;
(b) Repeating the operation of step (a), and processing pointed cones at other positions of the workpiece to form a cold cathode pointed cone array.
The cold cathode pointed cone array is prepared by the preparation method of the cold cathode pointed cone array.
Compared with the prior art, the invention has the beneficial effects that:
(1) The cold cathode pointed cone is prepared by adopting the electron microscope, so that the integration of in-situ processing and detection can be realized; the processing of the complex micro-nano structure of the material with weak rigidity, high strength and high hardness can be realized; the yield of the cold cathode pointed cone obtained by the method is up to 100%.
(2) The invention adopts an electron microscope to process the pointed cone at different positions of the workpiece so as to form a cold cathode pointed cone array; the method is easy to operate, and the obtained pointed cone array has higher tip machining precision.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of the position of a cold cathode pointed cone array prepared by hot rolling a workpiece according to the invention;
FIG. 2 is a schematic diagram showing a beam bombardment point of a dual-beam electron microscope in a serpentine shape on a cylinder according to the present invention;
FIG. 3 is a partial top view of a cold cathode cone array in accordance with example 1 of the present invention;
FIG. 4 is a partial side view of a cold cathode cone array of example 1 of the present invention;
FIG. 5 is a top view of a single cold cathode tip in example 1 of the present invention;
FIG. 6 is a side view of a single cold cathode tip in example 1 of the present invention;
FIG. 7 is a side view of a single cold cathode tip in example 2 of the present invention;
FIG. 8 is a side view of a single cold cathode tip in example 3 of the present invention;
FIG. 9 is a graph showing the energy intensity of beam current as a function of depth of processing in example 1 of the present invention;
fig. 10 is a graph showing the change of beam energy intensity with processing depth in comparative example 1 of the present invention.
Reference numerals:
1-objective table, 2-hot roll work piece, 3-annular groove, 4-cylinder, 5-cold cathode pointed cone, 6-beam emission point.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer.
In the description of the present invention, it should be noted that, directions or positional relationships indicated by terms such as "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., are directions or positional relationships based on those shown in the drawings, or are directions or positional relationships conventionally put in use of the inventive product, are merely for convenience of describing the present invention and simplifying the description, and are not indicative or implying that the apparatus or element to be referred to must have a specific direction, be constructed and operated in a specific direction, and thus should not be construed as limiting the present invention.
According to one aspect of the invention, the invention relates to a method for preparing a cold cathode tip cone, comprising the following steps:
bombarding the surface of a workpiece by utilizing beam current emitted by an electron microscope, and processing an annular groove on the surface of the workpiece along the depth direction, wherein a column body is formed inside the annular groove; and in the direction from the top to the bottom of the cylinder, processing the cylinder layer by utilizing the beam emitted by the electron microscope, and obtaining the cold cathode pointed cone by increasing and then decreasing the energy intensity of the beam emitted by the electron microscope.
The traditional machining is to firstly process and then detect the product through detection equipment. The invention adopts SEM-FIB double beam electron microscope to process, and can realize the integration of in-situ processing and detection. Real-time observation and processing of the in-situ cold cathode sharp cone are realized by using an SEM-FIB double-beam electron microscope, and micro-structure processing smaller than 100nm can be realized by improving processing beam current and processing structure, so that the yield is high; in particular, the meaning of high-value materials is great, since for high-value materials the economic losses caused by the occurrence of even a waste product are also significant.
The dual beam current of the dual beam electron microscope, namely electron beam and ion beam, has three main effects: deposition, processing and imaging. The ion Beam (I-Beam) has two functions, namely imaging and cutting, wherein the imaging is mainly used for assisting in positioning a cutting position, the specific principle is similar to that of E-Beam imaging, the ion Beam strikes the surface of a sample, signals such as secondary electrons and the like are excited, the imaging is collected, and the most main function of the I-Beam is cutting and etching. The basic principle of the cutting and etching of FIB (Focused Ion Beam) is that high-voltage high-current accelerates the ion bombardment to the surface of the sample, and the sample is physically destroyed to realize the cutting and etching function. When the ion beam is used for cutting, the electron beam is also required to be used for scanning and real-time imaging observation, and the two beam flows work simultaneously.
In one embodiment, the cylinder comprises a cylinder.
In one embodiment, the workpiece of the present invention is made of polycrystalline material, such as copper.
In one embodiment, before the bombarding the surface of the workpiece with the beam emitted by the electron microscope, the method further includes: carrying out hot rolling treatment on the workpiece; the hot rolling treatment specifically comprises the following steps: and carrying out heat treatment on the workpiece, and then carrying out rolling treatment.
In one embodiment, the temperature of the heat treatment is 200 to 400 ℃, such as 210 ℃, 250 ℃, 280 ℃, 300 ℃, 320 ℃, 350 ℃, etc., and the time of the heat treatment is 1 to 4 hours, such as 1.5 hours, 2 hours, 2.5 hours, 3 hours, or 3.5 hours, etc.
In one embodiment, the pressure of the rolling treatment is 18-22 MPa, such as 19MPa, 20MPa, 21MPa or 22MPa, etc.; the rolling treatment time is 25-35 min, for example 28min, 30min, 32min and the like.
According to the invention, through specific hot rolling treatment, the crystal grains of the polycrystalline material can be sharpened, so that the problem that the polycrystalline material is easy to generate brittle fracture reaction during micro-nano scale processing is solved.
In one embodiment, the hot roll treatment is performed in an inert atmosphere.
In one embodiment, the hot rolled workpiece obtained after the hot rolling treatment is naturally cooled, and then the workpiece is processed by adopting an electron microscope.
In one embodiment, the outer circle diameter of the annular groove is 5-12 μm, such as 6 μm, 7 μm, 8 μm, 9 μm, 10 μm, 11 μm, etc., and the inner circle diameter of the annular groove is 1-3 μm, such as 1 μm, 1.6 μm, 2 μm, 2.6 μm, etc.
In one embodiment, the workpiece is located on a stage of the electron microscope; when the annular groove is processed on the surface of the workpiece, the beam emission point of the electron microscope is positioned above the workpiece; and the beam emitted by the electron microscope is perpendicular to the surface of the workpiece, and the beam emission point and the workpiece generate relative motion by moving the objective table so as to form the annular groove. In the process of machining the annular groove, the beam is used for machining the workpiece layer by layer. When each layer of processing is carried out, the bombardment point of the beam on the workpiece can perform circumferential walking or serpentine walking relative to the workpiece.
In one embodiment, the workpiece is located on a stage of the SEM-FIB dual beam electron microscope; when the cylinder is processed, a double-beam emission point of the SEM-FIB double-beam electron microscope is positioned right above the top end of the cylinder; the cylinder is processed by changing the emitting direction of the double-beam emitting point. During this process, the dual beam emission point is relatively stationary with respect to the stage, i.e., the beam emission point is relatively stationary with respect to the workpiece.
In one embodiment, during the layer-by-layer processing, the beam bombardment point of the SEM-FIB dual beam electron microscope is in a serpentine shape on the surface of the hot rolled workpiece. Thus, the curtain effect can be effectively avoided, and the processing effect is better, wherein the curtain effect means that: curtain-like machined lines are formed on the machined surface, which lines affect the shape accuracy and surface roughness of the final product.
In one embodiment, during the layer-by-layer processing, the processing depth of each layer is 8-12 atomic layers, for example 8 atomic layers, 10 atomic layers, 11 atomic layers, etc.
In one embodiment, during the layer-by-layer processing, each layer is stopped for 0.3 to 1.8 μs after completion of processing, for example, 0.5 μs, 0.7 μs, 0.9 μs, 1 μs, 1.2 μs, 1.5 μs, etc., and debris generated after processing is removed by vacuum pumping.
In one embodiment, the beam energy is maximized when the machining depth is two-thirds to three-quarters of the total depth during the machining of the cylinder from top to bottom. In one embodiment, the beam energy of the initial end and the final end is (4-4.5) x 10 in the process of processing the cylinder from the top end to the bottom end -7 pC/μm 2 For example 4X 10 -7 pC/μm 2 、4.1×10 -7 pC/μm 2 、4.2pC/μm 2 、4.3×10 -7 pC/μm 2 、4.4×10 -7 pC/μm 2 Or 4.5X10 -7 pC/μm 2 Etc.; the range of the maximum beam energy is (8.5-8.8) x 10 -7 pC/μm 2 For example 8.5X10 -7 pC/μm 2 、8.6×10 -7 pC/μm 2 、8.7×10 -7 pC/μm 2 、8.8×10 -7 pC/μm 2 Etc.
When the dual beam electron microscope is used for processing, the deeper the depth (Z-axis direction) to be processed is in a certain depth range, the larger the required dual beam energy is. When the processing material is copper, the processing depth reaches two thirds of the total depth (the lower part is one third), and the double beam energy reaches the maximum; the energy of the double beams needs to be gradually reduced, if the energy is still large, the bottom of the pointed cone is deformed and collapsed due to the fact that crystal grain dislocation occurs in the material crystal, and the pointed cone processing fails.
According to another aspect of the invention, the invention also relates to the cold cathode pointed cone prepared by the preparation method of the cold cathode pointed cone.
In one embodiment, the height of the cold cathode pointed cone is 8-15 μm, the taper angle is 5-20 degrees, and the tip diameter of the cold cathode pointed cone is 20-100 nm.
According to another aspect of the invention, the invention also relates to a preparation method of the cold cathode pointed cone array, comprising the following steps:
(a) Preparing a cold cathode pointed cone according to the preparation method of the cold cathode pointed cone;
(b) Repeating the operation of step (a), and processing pointed cones at other positions of the workpiece to form a cold cathode pointed cone array.
In one embodiment, after machining a pointed cone, the electron microscope is controlled to move the objective table (the displacement operation of the objective table can be controlled by MATLAB input parameters), the relative positions of the objective table and the double-beam emission points are changed, the steps are repeated, the pointed cone is machined at other positions of the workpiece, and after repeated for a plurality of times, the pointed cone array is machined. The preparation method of the cold cathode pointed cone array is simple and feasible, and the obtained pointed cone array has higher pointed precision.
According to another aspect of the present invention, the cold cathode pointed cone array is prepared by the preparation method of the cold cathode pointed cone array.
In a preferred embodiment, the method for preparing the cold cathode pointed cone array comprises the following steps:
(a) Carrying out heat treatment on the original workpiece, and then carrying out rolling treatment; the rolling treatment is carried out in an inert atmosphere; the temperature of the heat treatment is 200-400 ℃, and the time of the heat treatment is 1-4 hours; the pressure of the rolling treatment is 18-22 MPa, and the time of the rolling treatment is 25-35 min; naturally cooling the hot rolled workpiece obtained after the hot rolling treatment to obtain a hot rolled workpiece;
(b) Processing the hot rolled workpiece by adopting a double-beam electron microscope; the processing specifically comprises the following steps: bombarding the surface of a workpiece by utilizing beam current sent by an electron microscope, processing an annular groove on the surface of a hot rolled workpiece along the depth direction, wherein a cylinder is formed in the annular groove, the diameter of the outer circle of the annular groove is 5-12 mu m, and the annular groove is formed in the annular grooveThe inner diameter of the ring is 1-3 mu m; in the direction from the top end to the bottom end of the cylinder, carrying out layer-by-layer processing on the cylinder by adopting a double-beam electron microscope, wherein the beam bombardment point of the double-beam electron microscope is in a snake-shaped position on the surface of the hot rolled workpiece, the processing depth of each layer is 8-12 atomic layers in the layer-by-layer processing process, and in the layer-by-layer processing process, each layer is stopped for 0.3-1.8 mu s after processing, and fragments generated after processing are removed by vacuumizing; the beam energy reaches the maximum value when the processing depth is two-thirds to three-fourths of the total depth in the process of processing the cylinder from the top to the bottom, and the beam energy at the initial end and the final end in the process of processing the cylinder from the top to the bottom are respectively (4-4.5) multiplied by 10 -7 pC/μm 2 The method comprises the steps of carrying out a first treatment on the surface of the The range of the maximum beam energy is (8.5-8.8) x 10 -7 pC/μm 2 ；
(c) Repeating the operation of step (b), and processing pointed cones at other positions of the hot rolled workpiece to form a cold cathode pointed cone array.
In one embodiment, MATLAB is used to draw a gray scale map and a dual beam electron microscope is used to conduct single array processing on the dual beam electron microscope setting parameters.
In one embodiment, the parameter settings for the dual beam electron microscope are shown in table 1.
Table 1 parameter settings for dual beam electron microscope
The following is a further explanation in connection with specific examples.
The position schematic diagram of the cold cathode pointed cone array prepared by hot rolling a workpiece is shown in fig. 1. A schematic diagram of the beam bombardment point of the double beam electron microscope in the invention in a serpentine shape on the surface of the cylinder is shown in fig. 2.
Example 1
The preparation method of the cold cathode pointed cone array comprises the following steps:
(a) Carrying out heat treatment on the copper sheet, and then carrying out rolling treatment, wherein the rolling treatment is carried out in an inert atmosphere; the temperature of the heat treatment is 300 ℃, and the time of the heat treatment is 2 hours; the pressure of the rolling treatment is 20MPa, and the time of the rolling treatment is 30min; cooling the hot rolled workpiece 2 obtained after the hot rolling treatment to obtain the hot rolled workpiece 2;
(b) Processing the hot rolled workpiece 2 by adopting an electron microscope to obtain a cold cathode pointed cone 5; the processing specifically comprises the following steps:
placing a hot rolling workpiece 2 on an objective table 1 of an electron microscope, wherein a beam emission point 6 of the electron microscope is positioned above the hot rolling workpiece 2; the beam current of the electron microscope is perpendicular to the surface of the hot rolled workpiece 2, the beam current emission point 6 and the hot rolled workpiece 2 generate relative motion by moving the objective table 1, the surface of the hot rolled workpiece 2 is bombarded by the beam current emitted by the electron microscope to form an annular groove 3, a cylinder 4 is formed in the annular groove 3, the cylinder 4 is in a cylinder shape, the diameter of the outer circle of the annular groove 3 is 10 mu m, and the diameter of the inner circle of the annular groove 3 is 2 mu m.
In the direction from the top end to the bottom end of the cylinder 4, processing the cylinder 4 layer by utilizing beam current emitted by an electron microscope, wherein a beam current emission point 6 of the electron microscope is positioned right above the top end of the cylinder 4, the beam current emission point 6 and the hot rolling workpiece 2 are relatively static, and processing the cylinder 4 by changing the emission direction of the beam current emission point 6; the beam bombardment point of the electron microscope is in a serpentine shape on the surface of the hot rolled workpiece 2, the processing depth of each layer is 10 atomic layers in the layer-by-layer processing process, and in the layer-by-layer processing process, each layer is stopped for 1 mu s after processing, and scraps generated after processing are removed by vacuumizing; the dual beam energy reaches the maximum value when the machining depth is two-thirds of the total depth in the process of the column 4 from the top to the bottom, and the beam energy of the initial end and the final end is 4.2×10 respectively in the process of the column 4 from the top to the bottom -7 pC/μm 2 The method comprises the steps of carrying out a first treatment on the surface of the The beam energy reaches the maximum value of 8.6x10 -7 pC/μm 2 The method comprises the steps of carrying out a first treatment on the surface of the The graph of the change of the beam energy intensity with the processing depth in this embodiment is shown in fig. 9, where the point a represents that the processing depth is two-thirds of the total depth;
(c) Repeating the operation of the step (b), and processing cold cathode pointed cones 5 at other positions of the hot rolled workpiece 2 to form a cold cathode pointed cone array.
In this embodiment, a partial top view sem of the cold cathode cone array is shown in fig. 3; the partial side view scanning electron microscope image of the cold cathode pointed cone array is shown in fig. 4, wherein the diameter of the tip of the cold cathode pointed cone at the upper right corner of fig. 3 is 20nm; a top view sem of a single cold cathode tip is shown in fig. 5 and a side view sem of a single cold cathode tip is shown in fig. 6.
Example 2
The preparation method of the cold cathode pointed cone array comprises the following steps:
(a) Carrying out heat treatment on the copper sheet, and then carrying out rolling treatment, wherein the rolling treatment is carried out in an inert atmosphere; the temperature of the heat treatment is 400 ℃, and the time of the heat treatment is 1h; the pressure of the rolling treatment is 18MPa, and the time of the rolling treatment is 35min; cooling the hot rolled workpiece 2 obtained after the hot rolling treatment to obtain the hot rolled workpiece 2;
(b) And processing the hot rolled workpiece 2 by adopting a double-beam electron microscope to obtain a cold cathode pointed cone 5, wherein the processing specifically comprises the following steps:
placing a hot rolling workpiece 2 on an objective table 1 of a double-beam electron microscope, wherein a beam emission point 6 of the electron microscope is positioned above the hot rolling workpiece 2; the beam current of the electron microscope is perpendicular to the surface of the hot rolling workpiece 2, the beam current emission point 6 and the hot rolling workpiece 2 generate relative motion by moving the objective table 1, the surface of the hot rolling workpiece 2 is bombarded by the beam current emitted by the electron microscope to form an annular groove 3, a cylinder 4 is formed in the annular groove 3, the cylinder 4 is in a cylinder shape, the diameter of the outer circle of the annular groove 3 is 12 mu m, and the diameter of the inner circle of the annular groove 3 is 3 mu m;
in the direction from the top end to the bottom end of the cylinder 4, the cylinder 4 is processed layer by using the beam emitted by the electron microscope, the beam emission point 6 of the electron microscope is positioned right above the top end of the cylinder 4, the beam emission point 6 and the hot rolled workpiece 2 are relatively static, and the cylinder is aligned by changing the emission direction of the beam emission point 6Processing the body 4; the beam bombardment point of the electron microscope is in a serpentine shape on the surface of the hot rolled workpiece 2, the processing depth of each layer is 12 atomic layers in the layer-by-layer processing process, and the processing is stopped for 1.5 mu s after each layer is processed in the layer-by-layer processing process, and scraps generated after the processing are removed by vacuumizing; the beam energy reaches the maximum value when the machining depth is two-thirds of the total depth in the process of the column 4 from the top to the bottom, and the beam energy of the initial end and the final end is 4×10 respectively in the process of the column 4 from the top to the bottom -7 pC/μm 2 The method comprises the steps of carrying out a first treatment on the surface of the The beam energy reaches the maximum value of 8.5 multiplied by 10 -7 pC/μm 2 ；
(c) Repeating the operation of the step (b), and processing cold cathode pointed cones 5 at other positions of the hot rolled workpiece 2 to form a cold cathode pointed cone array.
A side view of a single cold cathode spike in this embodiment is shown in FIG. 7.
Example 3
The preparation method of the cold cathode pointed cone array comprises the following steps:
(a) Carrying out heat treatment on the copper sheet, and then carrying out rolling treatment, wherein the rolling treatment is carried out in an inert atmosphere; the temperature of the heat treatment is 200 ℃, and the time of the heat treatment is 4 hours; the pressure of the rolling treatment is 22MPa, and the time of the rolling treatment is 25min; cooling the hot rolled workpiece 2 obtained after the hot rolling treatment to obtain the hot rolled workpiece 2;
(b) And processing the hot rolled workpiece 2 by adopting a double-beam electron microscope to obtain a cold cathode pointed cone 5, wherein the processing specifically comprises the following steps:
placing a hot rolling workpiece 2 on an objective table 1 of a double-beam electron microscope, wherein a beam emission point 6 of the electron microscope is positioned above the hot rolling workpiece 2; the beam current of the electron microscope is perpendicular to the surface of the hot rolling workpiece 2, the beam current emission point 6 and the hot rolling workpiece 2 generate relative motion by moving the objective table 1, the surface of the hot rolling workpiece 2 is bombarded by the beam current emitted by the electron microscope to form an annular groove 3, a cylinder 4 is formed in the annular groove 3, the cylinder 4 is in a cylinder shape, the diameter of the outer circle of the annular groove 3 is 6 mu m, and the diameter of the inner circle of the annular groove 3 is 1 mu m;
in the direction from the top end to the bottom end of the cylinder 4, processing the cylinder 4 layer by utilizing beam current emitted by an electron microscope, wherein a beam current emission point 6 of the electron microscope is positioned right above the top end of the cylinder 4, the beam current emission point 6 and the hot rolling workpiece 2 are relatively static, and processing the cylinder 4 by changing the emission direction of the beam current emission point 6; the beam bombardment point of the electron microscope is in a serpentine shape on the surface of the hot rolled workpiece 2, the processing depth of each layer is 8 atomic layers in the layer-by-layer processing process, the processing of each layer is stopped for 0.5 mu s after the processing of each layer is finished, and scraps generated after the processing are removed by vacuumizing; the beam energy reaches the maximum value when the machining depth is two-thirds of the total depth in the process of the column 4 from the top to the bottom, and the beam energy of the initial end and the final end is 4.5X10 respectively in the process of the column 4 from the top to the bottom -7 pC/μm 2 The method comprises the steps of carrying out a first treatment on the surface of the The beam energy reaches the maximum value of 8.8x10 -7 pC/μm 2 ；
(c) Repeating the operation of the step (b), and processing cold cathode pointed cones 5 at other positions of the hot rolled workpiece 2 to form a cold cathode pointed cone array.
A side view of a single cold cathode spike in this embodiment is shown in FIG. 8.
Comparative example 1
Preparation method of cold cathode pointed cone array, wherein beam energy is constant at 4.2×10 during processing -7 pC/μm 2 The graph of the change of the beam energy intensity along with the processing depth is shown in fig. 10, during the processing process, the rear beam can damage the front processed pointed cone tip, the processing precision of the pointed cone tip cannot be achieved, and the processed product is a round table.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (10)
1. The preparation method of the cold cathode pointed cone is characterized by comprising the following steps:
bombarding the surface of a workpiece by utilizing beam current emitted by an electron microscope, and processing an annular groove on the surface of the workpiece along the depth direction, wherein a column body is formed inside the annular groove; and in the direction from the top to the bottom of the cylinder, processing the cylinder layer by utilizing the beam emitted by the electron microscope, and obtaining the cold cathode pointed cone by increasing and then decreasing the energy intensity of the beam emitted by the electron microscope.
2. The method for preparing a cold cathode tip according to claim 1, further comprising, before the bombarding the surface of the workpiece with the beam emitted by the electron microscope: carrying out hot rolling treatment on the workpiece; the hot rolling treatment specifically comprises the following steps: and carrying out heat treatment on the original workpiece, and then carrying out rolling treatment.
3. The method of manufacturing a cold cathode tip according to claim 2, comprising at least one of the following features (1) to (5):
(1) The temperature of the heat treatment is 200-400 ℃, and the time of the heat treatment is 1-4 hours;
(2) The pressure of the rolling treatment is 18-22 MPa, and the time of the rolling treatment is 25-35 min;
(3) The hot rolling treatment is carried out in an inert atmosphere;
(4) Naturally cooling the workpiece obtained after the hot rolling treatment, and processing the workpiece after the natural cooling by adopting the electron microscope;
(5) The workpiece is a polycrystalline material.
4. The method for manufacturing a cold cathode tip cone according to claim 1, wherein the diameter of the outer circle of the annular groove is 5-12 μm, and the diameter of the inner circle of the annular groove is 1-3 μm.
5. The method of manufacturing a cold cathode tip according to claim 1, comprising at least one of the following features (1) to (2):
(1) The workpiece is positioned on the objective table of the electron microscope; when the annular groove is machined on the surface of the workpiece, a beam emission point of the electron microscope is positioned above the workpiece; the beam emitted by the electron microscope is perpendicular to the surface of the workpiece, and the beam emission point and the workpiece generate relative motion by moving the objective table so as to form the annular groove;
(2) When the cylinder is processed, the beam emission point of the electron microscope is positioned right above the top end of the cylinder; the beam emission point and the workpiece are relatively static, and the cylinder is processed by changing the emission direction of the beam emission point.
6. The method of manufacturing a cold cathode tip according to claim 1, comprising at least one of the following features (1) to (5):
(1) In the layer-by-layer processing process, beam bombardment points of the electron microscope form serpentine positions on the surface of the workpiece;
(2) In the layer-by-layer processing process, the processing depth of each layer is 8-12 atomic layers;
(3) In the layer-by-layer processing process, stopping for 0.3-1.8 mu s after each layer of processing is finished, and removing scraps generated after the processing by vacuumizing;
(4) In the process of machining the column from the top to the bottom, when the machining depth is two-thirds to three-fourths of the total depth, the beam energy reaches the maximum value;
(5) In the process of processing the column from the top to the bottom, the beam energy of the initial end and the final end is (4-4.5) multiplied by 10 -7 pC/μm 2 The method comprises the steps of carrying out a first treatment on the surface of the The beam energy reaches the maximumThe value range is (8.5-8.8) ×10 -7 pC/μm 2 。
7. The cold cathode pointed cone prepared by the method for preparing a cold cathode pointed cone according to any one of claims 1 to 6.
8. The cold cathode pointed cone according to claim 7, wherein the height of the cold cathode pointed cone is 8-15 μm, the taper angle is 5 ° -20 °, and the tip diameter of the cold cathode pointed cone is 20-100 nm.
9. The preparation method of the cold cathode pointed cone array is characterized by comprising the following steps of:
(a) Preparing a cold cathode pointed cone according to the preparation method of the cold cathode pointed cone according to any one of claims 1 to 6;
(b) Repeating the operation of step (a), and processing pointed cones at other positions of the workpiece to form a cold cathode pointed cone array.
10. The cold cathode pointed cone array according to claim 9.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1267378A1 (en) * | 2001-06-12 | 2002-12-18 | Hewlett-Packard Company | Method for fabricating self-aligned field emitter tips |
| CN1845872A (en) * | 2003-09-05 | 2006-10-11 | 索尼株式会社 | Fine structure body-producing method, fine structure body, display device, recording device-producing method, and recording device |
| WO2011010739A1 (en) * | 2009-07-23 | 2011-01-27 | 国立大学法人名古屋大学 | Method for producing microstructure |
| US8536564B1 (en) * | 2011-09-28 | 2013-09-17 | Sandia Corporation | Integrated field emission array for ion desorption |
| CN114944311A (en) * | 2022-06-02 | 2022-08-26 | 安阳工学院 | Preparation method of hexaboride nano pointed cone array |
-
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1267378A1 (en) * | 2001-06-12 | 2002-12-18 | Hewlett-Packard Company | Method for fabricating self-aligned field emitter tips |
| CN1845872A (en) * | 2003-09-05 | 2006-10-11 | 索尼株式会社 | Fine structure body-producing method, fine structure body, display device, recording device-producing method, and recording device |
| WO2011010739A1 (en) * | 2009-07-23 | 2011-01-27 | 国立大学法人名古屋大学 | Method for producing microstructure |
| US8536564B1 (en) * | 2011-09-28 | 2013-09-17 | Sandia Corporation | Integrated field emission array for ion desorption |
| CN114944311A (en) * | 2022-06-02 | 2022-08-26 | 安阳工学院 | Preparation method of hexaboride nano pointed cone array |
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