阅读说明：本技术 一种稀土六硼化物场发射尖锥阵列的加工方法 (Processing method of rare earth hexaboride field emission pointed cone array ) 是由 张伟 李元成 张晓兵 蔡敏 纪亮 焦佳能 于 2019-11-19 设计创作，主要内容包括：本发明提供的一种稀土六硼化物场发射尖锥阵列的加工方法,是通过激光复合电化学刻蚀加工稀土六硼化物场发射尖锥阵列,利用激光加工技术加工尖锥结构的雏形,再利用电化学刻蚀法进一步提高尖锥结构的曲率半径和表面质量,将激光加工技术和电化学刻蚀法有机复合到稀土六硼化物场发射尖锥阵列加工中,从而充分利用了激光加工技术和电化学刻蚀法的优点。本发明实现了对稀土六硼化物表面尖锥阵列高效加工,并且制得尖锥阵列形貌均匀、曲率半径小。(The invention provides a processing method of a rare earth hexaboride field emission pointed cone array, which is characterized in that the rare earth hexaboride field emission pointed cone array is processed by laser composite electrochemical etching, a prototype of a pointed cone structure is processed by utilizing a laser processing technology, the curvature radius and the surface quality of the pointed cone structure are further improved by utilizing an electrochemical etching method, the laser processing technology and the electrochemical etching method are organically combined into the processing of the rare earth hexaboride field emission pointed cone array, and therefore, the advantages of the laser processing technology and the electrochemical etching method are fully utilized. The invention realizes the high-efficiency processing of the rare earth hexaboride surface pointed cone array, and the manufactured pointed cone array has uniform appearance and small curvature radius.)

1. A processing method of a rare earth hexaboride field emission pointed cone array is characterized by comprising the following steps:

(1) performing mechanical polishing and cleaning pretreatment on the surface to be processed of the rare earth hexaboride;

(2) depositing an electrochemical corrosion resistant mask on the surface to be processed of the rare earth hexaboride pretreated in the step (1);

(3) processing the surface to be processed of the rare earth hexaboride with the electrochemical corrosion resistant mask deposited in the step (2) by utilizing a laser processing technology to form an array structure with three-dimensional morphological characteristic array units;

(4) further etching and processing the surface of the array structure formed in the step (3) by adopting an electrochemical etching method to form a pointed cone array;

(5) and (4) removing the electrochemical corrosion resistant mask on the surface of the rare earth hexaboride subjected to electrochemical etching in the step (4), and cleaning the surface to obtain the rare earth hexaboride field emission pointed cone array.

2. The method for processing the rare earth hexaboride field emission cone array according to claim 1, wherein the rare earth hexaboride in the step (1) comprises: LaB₆、CeB₆、PrB₆、NdB₆、SmB₆、GdB₆And YbB₆Any one of them.

3. The method for processing the rare earth hexaboride field emission pointed cone array as claimed in claim 1, wherein the specific operations of the cleaning pretreatment in the step (1) are as follows: putting the rare earth hexaboride into an acetone solution, performing ultrasonic treatment for 10min, washing with alcohol to remove greasy dirt and impurities on the surface, washing with deionized water, and drying.

4. The method as claimed in claim 1, wherein in step (2), the thickness of the electrochemical corrosion-resistant mask is greater than 100 nm.

5. The method of claim 3, wherein the electrochemical corrosion resistant mask is formed by plasma enhanced chemical vapor deposition.

6. The method for processing the rare earth hexaboride field emission pointed cone array as claimed in claim 1, wherein the laser in the step (3) has a pulse width of 100 nanoseconds or less and a wavelength of 1064 nanometers or less.

7. The method for processing the rare earth hexaboride field emission pointed cone array as claimed in claim 1, wherein the three-dimensional shapes in the three-dimensional topographic feature array units in the step (3) are generally cylindrical, square column, cylinder-like, square column-like and cone-like shapes.

8. The method according to claim 1, wherein the electrolyte used in the electrochemical etching method in step (4) comprises any one of phosphoric acid, ethanol, water, hydrochloric acid, ethanol, water, and sodium chloride, ethanol, and water.

9. The method for processing a rare earth hexaboride field emission pointed cone array as claimed in claim 7, wherein in the electrochemical etching method in step (4), the rare earth hexaboride is connected with a power supply anode to form an anode, graphite is used as a cathode, and etching is carried out for 1.5-4 hours to form the pointed cone array.

Technical Field

The invention belongs to the technical field of rare earth hexaboride material processing, and particularly relates to a method for processing a rare earth hexaboride field emission pointed cone array through laser composite electrochemical etching.

Background

Rare earth hexaboride REB₆(RE ═ La, Ce, Pr, Nd, Sm, Gd, Yb) is excellentThe electron emission cathode material has the performance characteristics of high melting point, high conductivity, good thermal stability and chemical stability, active cathode surface and the like. In order to obtain a large emission current density to ensure that the REB6 is applied to the field of large current emission, a pointed cone array with a large number density and a small curvature radius must be processed on the surface of the REB 6. Due to REB₆The mechanical properties of the hard and brittle materials lead to that the hard and brittle materials are easy to occur when mechanical micromachining is used, or the quantity density and the curvature radius of the pointed cone array can not meet the use requirements, meanwhile, the REB6 has stable physical and chemical properties, the materials are difficult to machine by the micromachining technologies such as ion beam etching, electron beam exposure, chemical etching and the like, and the pointed cone array with large quantity density and small curvature radius is processed by exploring new processes and new methods and has great practical value.

Disclosure of Invention

(1) Technical problem to be solved

In view of the fact that the existing micromachining technologies such as mechanical machining, ion beam etching, electron beam exposure and chemical etching are difficult to meet the machining requirement of the rare earth hexaboride surface pointed cone array, the invention provides a REB for laser composite electrochemical etching machining₆The method of the field emission pointed cone array can realize the high-efficiency processing of the pointed cone array on the surface of the rare earth hexaboride, and has uniform appearance and small curvature radius.

(2) Technical scheme

A processing method of a rare earth hexaboride field emission pointed cone array comprises the following steps:

(1) performing mechanical polishing and cleaning pretreatment on the surface to be processed of the rare earth hexaboride;

(2) depositing an electrochemical corrosion resistant mask on the surface to be processed of the rare earth hexaboride pretreated in the step (1);

(3) processing the surface to be processed of the rare earth hexaboride with the electrochemical corrosion resistant mask deposited in the step (2) by utilizing a laser processing technology to form an array structure with three-dimensional morphological characteristic array units;

(4) further etching and processing the surface of the array structure formed in the step (3) by adopting an electrochemical etching method to form a pointed cone array;

(5) and (4) removing the electrochemical corrosion resistant mask on the surface of the rare earth hexaboride subjected to electrochemical etching in the step (4), and cleaning the surface to obtain the rare earth hexaboride field emission pointed cone array.

Further, the rare earth hexaboride in the step (1) comprises: LaB₆、CeB₆、PrB₆、NdB₆、SmB₆、GdB₆And YbB₆Any one of them.

Further, in the step (1), the specific operation of the cleaning pretreatment is as follows: putting the rare earth hexaboride into an acetone solution, performing ultrasonic treatment for 10min, washing with alcohol to remove greasy dirt and impurities on the surface, washing with deionized water, and drying.

Further, in the step (2), the thickness of the anti-electrochemical corrosion mask is greater than 100 nm.

Further, the electrochemical corrosion resistant mask is manufactured by adopting plasma enhanced chemical vapor deposition.

Further, the pulse width of the laser in the step (3) is less than or equal to 100 nanoseconds, and the wavelength is less than or equal to 1064 nanometers.

Further, the three-dimensional shapes in the three-dimensional topographic feature array unit in the step (3) are generally cylindrical, square column, cylinder-like, square column-like and cone-like shapes.

Further, the electrolyte used in the electrochemical etching method in the step (4) includes any one of electrolyte made of phosphoric acid, ethanol and water, electrolyte made of hydrochloric acid, ethanol and water, and electrolyte made of sodium chloride, ethanol and water.

Further, in the electrochemical etching method in the step (4), the rare earth hexaboride is connected with a positive electrode of a power supply to form an anode, graphite is used as a cathode, and etching is carried out for 1.5-4 hours to form a pointed cone array.

According to the technical scheme, the beneficial effects of the invention are as follows:

according to the invention, the rare earth hexaboride field emission pointed cone array is processed by laser composite electrochemical etching, the prototype of the pointed cone structure is processed by using a laser processing technology, the curvature radius and the surface quality of the pointed cone structure are further improved by using an electrochemical etching method, and the laser processing technology and the electrochemical etching method are organically combined into the processing of the rare earth hexaboride field emission pointed cone array, so that the advantages of the laser processing technology and the electrochemical etching method are fully utilized. Compared with the method for directly processing the pointed cone array by utilizing the laser processing technology, the method can obtain the pointed cone structure with smaller curvature radius and better surface quality; compared with an electrochemical etching method, the method saves a complex photoetching link, simplifies the processing procedure, carries out electrochemical etching on the basis of laser processing prototypes, reduces the etching removal amount and greatly improves the processing efficiency.

Drawings

FIG. 1 is a schematic diagram of the processing method of the rare earth hexaboride field emission pointed cone array of the present invention, wherein 1-rare earth hexaboride, 2-electrochemical corrosion resistant mask, 3-laser beam, 4-pointed cone array, step A is mechanical polishing and cleaning pretreatment, step B is preparation of electrochemical corrosion resistant mask, step C is laser processing, step D is electrochemical etching, and step E is removal of electrochemical corrosion resistant mask.

Detailed Description

The embodiments of the present invention will be described in further detail with reference to the drawings and examples. The following detailed description of the embodiments and the accompanying drawings are provided to illustrate the principles of the invention and are not intended to limit the scope of the invention, i.e., the invention is not limited to the embodiments described, but covers any modifications, alterations, and improvements in the parts, components, and connections without departing from the spirit of the invention.

It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present application will be described in detail below with reference to the embodiments with reference to the attached drawings.