CN115161649A - Surface treatment method for metal part of molecular beam epitaxy equipment - Google Patents
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/19—Iron or steel
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F17/00—Multi-step processes for surface treatment of metallic material involving at least one process provided for in class C23 and at least one process covered by subclass C21D or C22F or class C25
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F4/00—Processes for removing metallic material from surfaces, not provided for in group C23F1/00 or C23F3/00
- C23F4/02—Processes for removing metallic material from surfaces, not provided for in group C23F1/00 or C23F3/00 by evaporation
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/08—Iron or steel
- C23G1/088—Iron or steel solutions containing organic acids
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/16—Polishing
- C25F3/22—Polishing of heavy metals
- C25F3/24—Polishing of heavy metals of iron or steel
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Electrochemistry (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The invention discloses a surface treatment method for a metal part of molecular beam epitaxy equipment, which comprises the following steps: firstly, performing an electropolishing process flow, after degreasing, rinsing water, ultrasonic wave, pickling, rinsing water, electropolishing, rinsing water, neutralizing, rinsing water and drying, detecting the surface of a workpiece by using an optical instrument, running a processing algorithm, and further processing by using a high-energy electron beam obtained by accelerating by using an electron cyclotron. The metal component after the surface treatment method can meet the requirement of the molecular beam epitaxy equipment on an ultrahigh vacuum environment.
Description
Technical Field
The invention relates to the field of molecular beam epitaxy, in particular to a surface treatment method for a metal part of molecular beam epitaxy equipment.
Background
Because the working environment required by the Molecular Beam Epitaxy (MBE) technology is ultrahigh vacuum, the system must meet good sealing performance, the roughness and the cleanliness of the structural surface of the ultrahigh vacuum cavity and each part connected with the cavity are key indexes influencing the sealing performance of the ultrahigh vacuum cavity, and the surface treatment process of the ultrahigh vacuum cavity is directly related to the sealing performance of the structural surface of the ultrahigh vacuum cavity.
The control and optimization of the sealing performance of the ultra-high vacuum cavity structure surface aim to meet the strict requirement of the ultra-high vacuum cavity on the ultra-high vacuum degree, wherein the optimization of the surface treatment process is carried out on the ultra-high vacuum cavity structure surface to reduce the residue of impurities on the surface of the ultra-high vacuum cavity, and the method is a main technical means for realizing the sealing performance of the ultra-high vacuum cavity structure surface.
In the prior art, when a metal part is subjected to surface treatment, in order to improve the smoothness, corrosion resistance and oxidation resistance of the metal surface, an electrochemical polishing method of mechanical polishing or acid pickling and electrolytic polishing is usually adopted, but because the mechanical polishing needs a more precise mechanical device for a surface with lower roughness and cannot treat positions which are not beneficial to processing, such as corners and the like, at the same time, the adhesion between a metal surface treatment solution used for the electrochemical polishing and the metal surface is limited, the used metal surface treatment solution often contains sulfuric acid and hydrochloric acid, and the metal surface treatment solution has strong corrosivity and certain toxicity. Because the metal surface can receive inhomogeneous erosion, will produce the uneven scheduling problem of surface treatment effect, will influence the performance and the life of target equipment, even through the quantity of metal surface treatment agent or extension processing time, also can cause a large amount of wasting of resources, increased the waste liquid pollution risk, increased treatment cost. Therefore, it is necessary to develop a more energy-saving, green and efficient surface treatment method capable of significantly improving the surface smoothness, corrosion resistance and oxidation resistance of metal parts and achieving uniform treatment effect on the surfaces of the metal parts to meet the requirement of ultrahigh vacuum required by corresponding equipment.
For this reason, in combination with the prior art, a method of surface-treating a metal part using a novel electrolyte and a high-energy electron beam has been proposed. The components of the novel electrolyte do not contain sulfuric acid and hydrochloric acid, the corrosivity of the novel electrolyte to metal is reduced by adjusting the proportion of other acids and adding an organic solution, the difficulty of waste liquid treatment is further reduced under the condition that the working efficiency of the novel electrolyte is not influenced, and the novel electrolyte is more green and environment-friendly. The method for treating the surface of the metal part by using the high-energy electron beam comprises the following steps: on one hand, the high-energy electron beams bombard the surface of the metal part, so that the bombarded material is quickly evaporated to avoid the melting of the surrounding material, the degassing of the material and the selective evaporation of impurities are realized, the working time and the cooling time are short, and the working area range and the surface treatment degree are efficient and controllable; on the other hand, the electron beam processing avoids the problems of solution waste, pollution and the like caused by other processing methods, and is clean and energy-saving.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, pursues the requirement of a molecular beam epitaxy system (MBE) on higher vacuum degree, and provides a method for treating the surface of a metal part of molecular beam epitaxy equipment, which has the advantages of simple operation, wide application range, energy conservation, greenness, flexibility, controllability, precision and high efficiency. The roughness of the ultra-high vacuum cavity treated by the metal part surface treatment method can reach Ra of less than or equal to 0.5 mu m, the surface ripples of the structural surfaces of the cavity and the part are effectively reduced, the texture orientation and the line thickness are more uniform, the amount of gas released by impurities is less, the surface quality of the ultra-high vacuum cavity and the part is improved, and the sealing property of the structural surface of the ultra-high vacuum cavity component is effectively ensured.
In order to achieve the purpose, the technical scheme of the invention is to design a surface treatment method for a metal part of molecular beam epitaxy equipment, the adopted material is SUS300 series stainless steel (low-carbon steel containing 10-20% of Cr, the low-carbon steel has the advantages of excellent corrosion resistance, low outgassing rate, no magnetism, good weldability, low electric conductivity and thermal conductivity, can work at-270-900 ℃ and the like, and is widely applied in high vacuum and ultrahigh vacuum systems) and comprises the following operation steps:
s1: pre-cleaning, firstly, adopting a water-soluble alkaline cleaning agent (a mixed aqueous solution of sodium carbonate and sodium hydroxide, wherein the mass fraction of the sodium carbonate is 3 percent, and the mass fraction of the sodium hydroxide is 1.5 percent) to degrease and degrease the sealing surface according to the processing condition of a workpiece, and then adopting tap water with certain pressure to perform primary high-pressure washing on the sealing surface;
s2: ultrasonic pickling with ultrasonic frequency of 40-100 kHz and power density of not less than 0.4W/cm 2 The ultrasonic pickling temperature is 40-80 ℃. In the mixed solution used for pickling, phosphoric acid (85%) 3 PO 4 ) The mass ratio of (A) is 0.4 to 0.6, the mass ratio of the organic acid mixed solution (including citric acid, organic phosphonic acid, etc.) at an appropriate working temperature is 0.3 to 0.5, and the mass ratio of water is 0.1 to 0.2. The pickling time (including soaking time) should not be less than 25min. After the pickling is finished, washing the surface pickling solution by using pure water (sewage or tap water cannot be used, the same shall apply below) with a certain pressure;
s3: electrolytic polishing using phosphoric acid (H) 3 PO 4 85%) of 0.7-0.8, the mass ratio of corrosion inhibitors such as chromic anhydride (CrO 3), glycerol, methyl cellulose and the like is less than or equal to 0.1, the mass ratio of water is 0.1-0.2, and the temperature is 60-80 ℃. And during electrolysis, the voltage is 6-10V, the workpiece is taken out after polishing for 4-7 min, and polishing is repeated for several times, and the polishing time is correspondingly shortened every time to enable the part to reach higher finish, and the step can finally enable Ra to reach about 1 mu m. After the electrolysis is finished, washing the surface electrolyte by pure water with certain pressure;
s4: neutralizing with sodium carbonate water solution with a certain mass fraction (25 wt%), washing with pure water with a certain pressure to remove the surface neutralization solution, and drying;
s5: detecting the surface of a metal part by using an optical detection instrument, wherein a hardware frame of the instrument mainly comprises an illuminating device, a CCD (charge coupled device) camera, an image processing computer and a server, the special infrared light source array is adopted for illumination, after relevant information of the rough condition of the surface of the metal part is obtained, the surface of the metal part to be processed is reasonably divided into a plurality of rows and columns, a set series of processing algorithm programs are operated, a plurality of groups of data schemes such as the energy, beam intensity, processing time, processing times of electron beams and the focal diameters of the electron beam source end and the electron beams required by each region in a subsequent high-energy electron beam processing link are calculated, and an optimal scheme is selected from multiple angles such as energy consumption, efficacy and the like;
s6: use the heightThe surface of the metal part can be processed by electron beams, the used high-energy electron beams are generated by an electron cyclotron, the acceleration upper limit is 30MeV, the acceleration voltage range is 30-150 kV, the wavelength is less than 0.1 angstrom, the beam intensity is more than 10mA, and the power density is more than or equal to 10 2 W/cm 2 The diameter of the electron beam focal point is about 0.1-1 mm;
s7: and (5) washing the surface scraps with pure water at a certain pressure, drying, performing surface optical detection again in S5, returning to S6 if the detection result does not meet the expected requirement, performing the operation again, packaging if the detection result meets the requirement, and placing the finished product.
According to the invention, firstly, the surface of a metal part for molecular beam epitaxy equipment is cleaned by adopting an alkaline cleaning agent, so that oily stains on the surface of the metal part are effectively removed, and the working efficiency of subsequent electropolishing and the service life of electrolyte are ensured; the ultrasonic pickling is used for further processing the structural surface of the metal component, welding spattering slag, slag inclusion, a surface oxide film and the like of the structural surface of the metal component are removed, the electrolytic polishing process is used for further polishing the structural surface of the metal component, surface ripples are effectively reduced, meanwhile, the smoothness of the surface of the metal component is guaranteed, and the sealing property of the surface of the metal component is improved; the neutralization treatment process effectively eliminates the corrosion effect of the pickling solution and the electrolyte remained on the surface of the metal part in the prior process flow on the surface of the metal part; tap water and pure water are repeatedly adopted to wash the surface of the metal part at high pressure, so that residual solution on the surface of the metal part is effectively washed, and the cleanliness of the structural surface of the ultrahigh vacuum cavity is ensured; the drying process ensures the drying performance of the finished product on the surface of the metal part.
The invention uses ultrasonic pickling technology to improve the pickling efficiency and the utilization rate of pickling solution. The ultrasonic pickling process is an efficient rust removing and scale removing technology developed in recent years, and the rust removing principle is similar to that of the ultrasonic degreasing described above, except that the solution is changed into an acidic substance. The ultrasonic pickling can greatly improve the pickling efficiency, and even if the workpieces have complicated geometric shapes, the low-concentration pickling solution can achieve very satisfactory effect under the action of ultrasonic waves. In particular, before phosphorization, the steel welding assembly can remove rust and welding scale on the assembly in a short time under the action of ultrasonic waves in a mixed pickling solution taking phosphoric acid as a main component. Therefore, the production field, the investment and the process time can be greatly saved, the resources are saved, and the aim of clean production is fulfilled.
The invention takes organic acid as additive to avoid the over-strong corrosion of the surface of the metal part of the molecular beam epitaxy equipment by the acid cleaning solution and improve the ability of chelating metal ions, and has the functions of accelerating rust removal and prolonging the service life of the rust remover.
Electropolishing as used in the present invention is part of electropolishing, which is based on the same basic principle as chemical polishing, i.e., by selectively dissolving small protrusions from the surface of the material to smooth the surface. The electropolishing process can be broadly divided into two steps: (1) Macroscopically flattening, diffusing dissolved products into electrolyte, reducing the geometric roughness of the surface of the material, and enabling Ra to be larger than 1 mu m. (2) Smooth glimmering, anode polarization and improved surface brightness, ra is less than 1 μm.
Compared with the mechanical polishing method widely used in the market at present, the electropolishing used in the invention is a process of (1) mechanically polishing and grinding the polished surface to obtain a smooth surface, thus a cooling hardened deformation layer is arranged on the stainless steel surface and some polishing abrasive materials are also included, and the electropolishing is a process of leveling the polished surface by electrochemical dissolution. No deformation layer is generated on the surface, foreign matters are not added, and simultaneously, a layer of oxide film is formed on the polished surface due to oxygen precipitation in the electrolytic process, so that the corrosion resistance of the polished surface is further improved. (2) For parts with complex shapes, wires, thin plates or small parts have difficult processability by mechanical polishing, and the electrolytic polishing has very good processability, so that the details which are not easy to be mechanically processed can be processed. (3) The electric polishing can improve the light reflection performance of the surface of the part more than the mechanical polishing. (4) The electropolishing has a leveling effect and can remove surface impurities, so that the electron cold emission of the metal is reduced. Meanwhile, compared with other treatment methods such as chemical polishing, the method can eliminate the influence of cathode reaction and has better effect.
The present invention is intended to ensure the smoothness of the surface of a metal member used for a molecular beam epitaxy apparatus, since the duration of electropolishing greatly affects the polishing quality. The initial period of time, in which the planarization rate is greater and then gradually slows down, even damaging the surface finish that has occurred, should be shortened as the current density and temperature increase. Therefore, the method of polishing is adopted for several times, and the polishing time is not long, so that the surface with higher smoothness is obtained.
In order to prevent the surface of a metal part used for molecular beam epitaxy equipment from being too strong to be corroded by electrolyte, the invention adds a small amount of organic matters (such as glycerol, methyl cellulose and the like) as corrosion inhibitors.
The invention uses high-energy electron beams to process the surface of a metal part, and because electrons moving at high speed have the wave property, when the high-speed electrons irradiate the metal surface, the incident electrons can penetrate into the metal surface to a certain depth and interact with atomic nuclei and electrons of matrix metal. Since the mass of the incident electrons differs greatly from the mass of the nuclei, they collide elastically with the nuclei. Therefore, the energy transfer is mainly completed by the collision of electron beams and electrons on the metal surface layer, and the transferred energy is immediately transferred to atoms on the metal surface layer in the form of heat energy in the process, so that the temperature of the treated metal surface layer is rapidly increased, the components and the structure of the surface layer are changed, and the surface modification effect is achieved. The material can be subjected to surface heat treatment, welding, etching, drilling, smelting or directly sublimed by the heat effect of the electron beam. Electron beam exposure is a process that utilizes the effect of electron beam radiation. As a heating tool, electron beams are characterized by high power and high power density, which can instantaneously transfer energy to a workpiece, whose parameters and positions can be accurately and rapidly adjusted, can be computer-controlled and processed in a contamination-free vacuum. When the power density of the electron beam reaches 10 5 ～10 6 When the electron beam is in watt/square centimeter, the material at the bombardment position of the electron beam is locally melted; if the electron beam is moved relative to the workpiece, the molten metal is solidified. Further, when the focusing method is used, the power density is 10 6 ～10 8 The electron beam of watt/cm bombards periodically the fixed point on the surface of the material, and the proportion of the bombarding time and the rest time of the electron beam is properly controlled, so that the bombarded material can be quickly evaporated to avoid the melting of the surrounding material, and the etching, drilling or cutting of the electron beam can be realized. The electron beam heating can maintain the material in a melting state in vacuum for a long time, realize the degassing of the material and the selective evaporation of impurities, and can be used for preparing high-purity materials. In summary, various processes can be performed according to the electron beam power density and the action time of the electron beam and the material.
In order to save space resources required by processing, enlarge the regulation range of the electron beam and facilitate the regulation, the invention preferably adopts the technical scheme that the electron cyclotron is replaced by an electron gun. At the same time, the electron gun is less expensive to maintain than the electron cyclotron.
In order to improve the processing efficiency of the electron beam, enlarge the regulation range of the electron beam and facilitate the regulation, the preferred technical scheme is to arrange a plurality of electron beam emitting ports into a plane to realize the processing of a plurality of areas at the same time.
In order to ensure the cleanliness of the surface of the metal part in each step of operation process and prepare cleaning for the next step of process, the invention preferably adopts the technical scheme that the pressure of the water body used for high-pressure cleaning is 140-170 Bar.
In order to ensure the drying performance of the surface of the metal part for the molecular beam epitaxy equipment, a further preferable technical scheme is that the drying mode is hot air drying, and the drying temperature is 100-140 ℃.
The invention has the advantages and beneficial effects that:
1. overcomes the defects of the prior art, and ensures that a molecular beam epitaxy system (MBE) is convenient to meet the requirement of higher vacuum degree.
2. The processing method is not only not suitable for the conditions with high vacuum degree requirements like a molecular beam epitaxy system (MBE), but also suitable for other metal parts needing to reach the high vacuum degree system.
3. Compared with other widely used methods, the processes of ultrasonic pickling, high-energy electron beam processing and the like adopted by the invention have the advantages of less resource consumption, shorter time consumption, more energy conservation, environmental protection and high efficiency.
4. The technological links of optical instrument measurement and high-energy electron beam processing adopted in the invention realize automatic control equipment through local regional processing, algorithm selection operation scheme and the like, and the produced product has high quality, extremely high precision control, small size influence and uniform polishing, so that the surface and dead angle parts of the whole workpiece can achieve consistent mirror surface effect, and the chemical property of the surface of the product can be enhanced.
Drawings
FIG. 1 is a flow chart of the method of the present invention
FIG. 2 is a schematic view of an electron cyclotron orbit
FIG. 3 is a schematic view of electron beam contacting a metal surface
Detailed Description
The following description of the embodiments of the present invention will be made with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Example 1
The surface treatment method for the metal part of the molecular beam epitaxy equipment is adopted to treat the surface of the metal part made of SUS304 stainless steel, wherein
S1: pre-cleaning, firstly, adopting a water-soluble alkaline cleaning agent (a mixed aqueous solution of sodium carbonate and sodium hydroxide, wherein the mass fraction of the sodium carbonate is 3 percent, and the mass fraction of the sodium hydroxide is 1.5 percent) to degrease and degrease the sealing surface according to the processing condition of a workpiece, and then adopting tap water with the power of 140Bar to carry out primary high-pressure washing on the sealing surface;
s2: ultrasonic pickling with ultrasonic frequency of 60kHz and power density of 0.5W/cm 2, The ultrasonic pickling temperature is 60 ℃. Phosphoric acid (85% H) in the mixed solution used for pickling 3 PO 4 ) The mass ratio of (a) is 0.5, the mass ratio of the organic acid mixed solution (containing citric acid, organic phosphonic acid, etc.) at an appropriate operating temperature is 0.35, and the mass ratio of water is 0.15. Pickling time (including soaking time) is 3And 0min. After the acid washing is finished, washing the surface acid washing solution by using 140Bar pure water (sewage or tap water cannot be used, the same is applied below);
s3: electrolytic polishing using phosphoric acid (H) 3 PO 4 85%) of 0.7, of corrosion inhibitors such as chromic anhydride (CrO 3), glycerol, methyl cellulose and the like of 0.1, of 0.2, and of water at 70 ℃. And during electrolysis, the voltage is 7V, the workpiece is taken out after 7min of polishing, the polishing is repeated for several times, the polishing time is correspondingly shortened every time, and the polishing time is adjusted to be 6.5min, 6min and 5.5min according to the situation. After the electrolysis is finished, the surface electrolyte is washed by pure water of 140 Bar;
s4: performing neutralization treatment by using a sodium carbonate aqueous solution with the mass fraction of 25%, then washing the surface neutralization solution by using 140Bar pure water, and drying at 120 ℃;
s5: and (3) detecting the surface of the metal part by using an optical detection instrument, and selecting an optimal high-energy electron beam processing scheme provided by an algorithm according to the existing conditions. For example: the beam intensity is 60mA, the diameter of an electron beam focus is about 0.5mm, and the power density is 110W/cm 2 ；
S6: processing the surface of the metal part by using a high-energy electron beam, wherein the high-energy electron beam is generated by an electron cyclotron, and relevant parameters of the high-energy electron beam are determined by S5;
s7: and (3) washing the surface scraps by using 140Bar pure water, drying at 120 ℃, performing surface optical detection again in S5, returning to S6 if the detection result does not meet the expected requirement, performing the operation again, and packaging and placing the finished product if the detection result meets the requirement.
Example 2
Example 2 differs from example 1 in that the surface of the metal part to be machined is rinsed with tap water or pure water at a pressure of 150 Bar. The electropolishing can be partially modified by using phosphoric acid (H) 3 PO 4 85%) of 0.75, of corrosion inhibitors such as chromic anhydride (CrO 3), glycerol, methyl cellulose and the like of 0.05, of 0.2, and of water at 80 ℃. During electrolysis, the workpiece is taken out after polishing for 6.5min, and is polished repeatedly for several times, and the polishing time of each time is correspondingly shortenedThe polishing time was adjusted to 6min, 5.5min, 5min as appropriate. The electron beam source is changed into the electron gun, the acceleration voltage range of the electron gun is wider, and the regulation and the control are more convenient. On the basis of the embodiment 1, the time of electrolytic polishing is further shortened, the space is saved, the cost is reduced, and the operation difficulty and the resource cost of electron beam processing are reduced.
Example 3
Example 3 differs from example 1 in that the surface of the metal part to be machined is rinsed with tap water or pure water at a pressure of 160 Bar. And during electrolysis, the voltage is 9V, the workpiece is taken out after polishing for 6min, polishing is repeated for several times, the polishing time is correspondingly shortened every time, and the polishing time is adjusted to 5.5min, 5min and 4.5min according to the situation. The electron beam source is used instead of an array of electron guns. On the basis of the embodiment 1, the electrolytic polishing time is further shortened, the space is saved, and the cost is reduced by improving the working temperature and the voltage and changing the solution ratio; the face-to-face processing is realized by changing the electron beam 'face source' formed by a plurality of electron guns, and the efficiency is improved.
Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make many possible variations and modifications to the disclosed solution, or modify equivalent embodiments using the teachings disclosed above, without departing from the scope of the solution. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention should fall within the protection scope of the technical scheme of the present invention, unless the technical spirit of the present invention departs from the content of the technical scheme of the present invention.
Claims (7)
1. A surface treatment method for a metal part of molecular beam epitaxy equipment is characterized by comprising the following operation steps:
s1: pre-cleaning: degreasing according to the processing condition of the workpiece, and flushing water to clean the surface;
s2: ultrasonic pickling, washing the surface pickling solution with clear water (sewage or natural water is unavailable);
s3: electrolytic polishing (repeated for multiple times), and rinsing;
s4: neutralizing, rinsing and drying;
s5: performing surface optical detection, and operating a processing algorithm program;
s6: processing by high-energy electron beams;
s7: rinsing, drying, carrying out surface optical detection, repeating S6 if the detection result does not meet the expected requirement, and finishing packaging if the detection result meets the requirement.
2. The surface treatment method of a metal part of molecular beam epitaxy equipment as claimed in claim 1, wherein in the electrolytic polishing process, the electrolyte is heated to 60-80 ℃, the workpiece to be electropolished is fixed on the anode by a proper hanger and the workpiece is kept opposite to the cathode, then the voltage is adjusted to 6-10V, the workpiece is taken out after polishing for 4-7 min, and polishing is repeated for several times, and the time of each polishing is correspondingly shortened to enable the part to reach a higher finish, and finally Ra reaches about 1 μm.
3. The method for surface treatment of a metal member of molecular beam epitaxy apparatus as claimed in claim 2, wherein phosphoric acid (H) is used as the electrolyte in the electrolytic polishing process 3 PO 4 85%) of 0.7-0.8, the mass ratio of corrosion inhibitors such as chromic anhydride (CrO 3), glycerol, methyl cellulose and the like is less than or equal to 0.1, and the mass ratio of water is 0.1-0.2.
4. The method of claim 1, wherein the surface condition of the workpiece is obtained by a precision optical instrument after the completion of the electropolishing and cleaning of the workpiece, thereby facilitating further processing. The hardware frame of the instrument mainly comprises an illuminating device, a CCD camera, an image processing computer and a server, wherein the illuminating device adopts a special infrared light source array.
5. The surface treatment method of a metal member for molecular beam epitaxy apparatus as claimed in claim 1, wherein the surface treatment is performed by an electron beam processing technique to obtain a surface with a higher finish.
6. The surface treatment method for a metal member of a molecular beam epitaxy apparatus as claimed in claim 5, wherein the surface treatment is carried out by an electron beam processing technique, and wherein the high-energy electron beam is generated by an electron cyclotron accelerator, and has an acceleration upper limit of 30MeV, a wavelength of less than 0.1A, a beam intensity of more than 10mA, and a power density of not less than 100W/cm2.
7. The method of surface treatment of a metal part of molecular beam epitaxy equipment according to claim 5, wherein the surface treatment is performed by an electron beam machining technique, and the method is characterized in that according to the optical detection result of the surface of the metal part of molecular beam epitaxy equipment according to claim 1, the surface of the metal part to be machined is reasonably divided into a plurality of rows and columns of areas, a machining algorithm program is correspondingly operated, a plurality of data schemes such as energy, beam intensity, machining time, machining times of electron beams and distance between a source end of the electron beams and a machining surface required by machining of each area are calculated, and an optimum one is selected from multiple angles such as energy consumption and efficacy to perform area-by-area machining on the surface of the metal part to be machined.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1107514A (en) * | 1953-06-05 | 1956-01-03 | Metal surface treatment process and its applications | |
| CN106346127A (en) * | 2016-10-25 | 2017-01-25 | 桂林电子科技大学 | Method for micro-melting and polishing carbon steel by scanning electron beams |
| CN109881243A (en) * | 2019-03-20 | 2019-06-14 | 江阴市光科光电精密设备有限公司 | A kind of grinding technics of ultrahigh vacuum cavity |
| CN110846711A (en) * | 2019-12-03 | 2020-02-28 | 浙江天阳钢管有限公司 | Precise stainless steel pipe electrolytic polishing process and electrolyte thereof |
| US11136688B1 (en) * | 2018-08-08 | 2021-10-05 | University Of Louisville Research Foundation, Inc. | Use of electropolishing for uniform surface treatment of metal components with complex external geometries |
| CN114211209A (en) * | 2021-12-27 | 2022-03-22 | 众至达精密机械科技(昆山)有限公司 | Surface processing technology for high-finish electronic metal structural part |
-
2022
- 2022-05-07 CN CN202210495823.0A patent/CN115161649A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1107514A (en) * | 1953-06-05 | 1956-01-03 | Metal surface treatment process and its applications | |
| CN106346127A (en) * | 2016-10-25 | 2017-01-25 | 桂林电子科技大学 | Method for micro-melting and polishing carbon steel by scanning electron beams |
| US11136688B1 (en) * | 2018-08-08 | 2021-10-05 | University Of Louisville Research Foundation, Inc. | Use of electropolishing for uniform surface treatment of metal components with complex external geometries |
| CN109881243A (en) * | 2019-03-20 | 2019-06-14 | 江阴市光科光电精密设备有限公司 | A kind of grinding technics of ultrahigh vacuum cavity |
| CN110846711A (en) * | 2019-12-03 | 2020-02-28 | 浙江天阳钢管有限公司 | Precise stainless steel pipe electrolytic polishing process and electrolyte thereof |
| CN114211209A (en) * | 2021-12-27 | 2022-03-22 | 众至达精密机械科技(昆山)有限公司 | Surface processing technology for high-finish electronic metal structural part |
Non-Patent Citations (1)
| Title |
|---|
| 中国大百科全书出版社编辑部编: "《机械工程材料及机械制造基础》", 中国大百科全书出版社 * |
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