CN112025098B - Preparation method of titanium alloy surface with low reflectivity to visible light - Google Patents
Preparation method of titanium alloy surface with low reflectivity to visible light Download PDFInfo
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- CN112025098B CN112025098B CN202010861142.2A CN202010861142A CN112025098B CN 112025098 B CN112025098 B CN 112025098B CN 202010861142 A CN202010861142 A CN 202010861142A CN 112025098 B CN112025098 B CN 112025098B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/352—Working by laser beam, e.g. welding, cutting or boring for surface treatment
- B23K26/354—Working by laser beam, e.g. welding, cutting or boring for surface treatment by melting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/60—Preliminary treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
Abstract
The invention belongs to the field of laser processing, and particularly relates to a method for preparing a titanium alloy surface with low reflectivity to visible light, which comprises the following steps: (1) Cleaning and pretreating the surface of a titanium alloy sample to be treated; (2) Preparing a pit-shaped milli-micro-nano tertiary structure on the surface of the titanium alloy by nanosecond laser: (3) Fluoridizing with hydrofluoric acid to strengthen the surface nano texture: and (3) placing the titanium alloy sample treated in the step (2) in a hydrofluoric acid solution for a certain time, taking out, cleaning and drying to obtain the titanium alloy surface with low reflectivity to visible light. The titanium alloy surface prepared by the preparation method of the invention realizes the reflectivity lower than 3% in the visible spectrum of 300-800nm, thereby having very good anti-reflection performance. The preparation method can simultaneously obtain a milli-micro-nano three-level structure on the surface of the titanium alloy, and has the advantages of simple process, convenient operation, high efficiency, less energy consumption and low cost.
Description
Technical Field
The invention belongs to the field of laser processing, and particularly relates to a method for preparing a titanium alloy surface with low reflectivity for visible light.
Background
Titanium is a young metal to be placed on the industrial stage of the world after world war II, and is a new star in the kingdom of metal materials. The mass percentage of titanium in the earth crust is 0.6%, and the structural metal is second to aluminum, iron and magnesium and is fourth. Titanium has excellent performance and abundant reserves, is inferior to iron and aluminum in terms of industrial value, resource life and development prospect, and is known as a third metal which is being developed. Titanium and its alloy have the comprehensive excellent properties of large strength, light weight and strong heat resistance, and when it is used to replace other metals in the manufacture of airplane, it not only can prolong the service life of airplane, but also can reduce its weight so as to greatly raise its flying property. Titanium is therefore one of the most promising structural materials in the aerospace industry and aeronautics. In addition, titanium and its alloys are also used as the main material of cameras outside the ship, and therefore, it is important to increase the light absorption performance of the surface.
Meanwhile, the phenomenon that the antireflection of the titanium alloy surface treatment changes the optical characteristics of the surface attracts considerable attention in the military and civil fields. Such as optical imaging and sensing, camouflage and stealth, countermeasures, solar absorbers, solar cells, solar water heaters, solar heating equipment, solar air conditioners, high-radiation heat exchange equipment, building wave-absorbing materials, mechanical equipment information acquisition, identification, carving, biomedicine and the like can be widely applied to reflection prevention, so that the characteristic of light absorption performance is improved.
Many techniques have been developed in recent years to reduce the surface reflectivity of titanium alloy materials. Such as chemical etching, ultrafast laser etching, mechanical grooving, and Reactive Ion Etching (RIE), wherein the chemical etching may pollute the environment, the mechanical grooving and the Reactive Ion Etching (RIE) may damage the titanium alloy surface, the manufacturing process is complicated, and the equipment cost of the ultrafast laser etching is high, so that the physical method and the chemical method have defects.
In conclusion, the method which is simple in process, high in preparation efficiency and suitable for industrialization and realizes the low reflectivity of the titanium alloy surface to visible light has important significance for advanced research, efficiency improvement, energy consumption reduction and environment protection, so that the rapid development of society and economy is promoted.
Disclosure of Invention
The invention aims to provide a method for preparing a titanium alloy surface with low reflectivity for visible light, which has the advantages of simple process and high preparation efficiency and is suitable for industrialization.
The scheme adopted by the invention for realizing the purpose is as follows: a method for preparing a titanium alloy surface with low reflectivity to visible light comprises the following steps:
(1) Cleaning and pretreating the surface of a titanium alloy sample to be treated;
(2) Preparing a pit-shaped milli-micro-nano tertiary structure on the surface of the titanium alloy by nanosecond laser:
(a) Scanning a focused laser beam on the surface of the titanium alloy sample treated in the step (1) along the X-axis direction, wherein the laser wavelength is 1064nm, the pulse width is 350-450ns, and the adjacent interval is 0.10-0.18mm;
(b) Scanning the surface of the titanium alloy sample obtained in the step (a) by focusing laser beams along the Y-axis direction, wherein the laser wavelength is 1064nm, the pulse width is 350-450ns, and the adjacent interval is 0.05-0.10mm;
(3) Fluoridizing with hydrofluoric acid to strengthen the surface nano texture:
and (3) placing the titanium alloy sample treated in the step (2) in a hydrofluoric acid solution for a certain time, taking out, cleaning and drying to obtain the titanium alloy surface with low reflectivity to visible light.
Preferably, in the step (1), the titanium alloy sample is a TC4 titanium alloy sample.
Preferably, in the step (2), in the step (a), the single pulse energy of the laser is 0.5mJ, the focused spot is 20 μm, the scanning speed is 1800-2400mm/s, and the scanning times are 200-250.
Preferably, in the step (2), in the step (b), the single pulse energy of the laser is 1mJ, the focused spot is 20 μm, the scanning speed is 8500-9500mm/s, and the scanning times are: 400-700 times.
Preferably, in the step (3), the concentration of the hydrofluoric acid solution is 30wt%, and the soaking time in the hydrofluoric acid solution is 3-10s.
The invention has the following advantages and beneficial effects:
the preparation method provided by the invention is mainly used for processing the surface of the titanium alloy by using the nanosecond laser technology, and the nanosecond laser processing technology has the advantages of simplicity, strong controllability, high processing precision, low cost, high efficiency, environmental friendliness and the like, and is one of ideal manufacturing technologies for preparing the surface of the low-reflectivity structure.
The preparation method of the invention not only overcomes the surface damage problem caused by mechanical grooving and RIE, but also overcomes the problems of high cost and low efficiency of ultrafast laser, and is convenient for realizing the large-area titanium alloy surface structure with low reflectivity to visible light.
The titanium alloy surface prepared by the preparation method of the invention realizes the reflectivity lower than 3% in the visible spectrum of 300-800nm, thereby having very good anti-reflection performance.
The preparation method provided by the invention mainly adopts nanosecond laser for preparation, can simultaneously obtain a milli-micro-nano three-level structure on the surface of the titanium alloy, and has the advantages of simple process, convenience in operation, high efficiency, low energy consumption and low cost.
The titanium alloy surface prepared by the preparation method provided by the invention has stable absorption performance on visible light, has excellent anti-reflection performance, and greatly expands the application range of the titanium alloy in the field of optical components.
Drawings
FIG. 1 is a photograph of a titanium alloy surface after nanosecond laser processing in example 1 of the invention;
FIG. 2 is a scanning electron microscope photomicrograph of the surface of the titanium alloy after nanosecond laser treatment in example 1 of the invention;
FIG. 3 is a high power scanning electron micrograph of the titanium alloy surface after hydrofluoric acid solution treatment according to example 1 of the present invention; the micron-sized holes and the nano-scale loose texture at the periphery of the holes can be seen in the figure;
FIG. 4 is a graph of the absorption rate of the titanium alloy surface prepared by the present invention in the visible light band.
Detailed Description
The following examples are provided to further illustrate the present invention for better understanding, but the present invention is not limited to the following examples.
Example 1
A method for preparing a titanium alloy surface with low reflectivity to visible light comprises the following steps:
(1) Surface cleaning pretreatment:
cleaning a TC4 titanium alloy sample to be treated in an ultrasonic cleaning instrument filled with deionized water, then cleaning with absolute ethyl alcohol (purity is more than 99.8%), drying the surface of the titanium alloy sample with compressed air or naturally drying at room temperature, and keeping the titanium alloy sample clean and dustproof to obtain a clean titanium alloy sample for later use.
(2) Preparing a pit-shaped milli-micro-nano tertiary structure on the surface of the titanium alloy by nanosecond laser:
(a) And (3) putting up and flatly placing four corners of the titanium alloy sample on a workbench, wherein air is arranged between the bottom surface of the titanium alloy sample and the workbench. Firstly, scanning a focused laser beam on the surface of a sample along the X direction, wherein the laser wavelength is 1064nm, the pulse width is 400ns, the single-pulse energy is 0.5mJ, the focused light spot is 20 mu m, the scanning speed is 2000mm/s, the adjacent interval is 0.15mm, and the scanning times are as follows: 200 times.
(b) And (2) scanning the surface of the sample by focusing a laser beam along the Y direction, wherein the laser wavelength is 1064nm, the pulse width is 400ns, the single-pulse energy is 1mJ, the focusing light spot is 20 mu m, the scanning speed is 9000mm/s, the adjacent interval is 0.09mm, and the scanning times are as follows: 500 times.
(3) Fluoridizing with hydrofluoric acid to strengthen the surface nano texture:
and (3) placing the titanium alloy sample piece prepared by the laser in a hydrofluoric acid solution, wherein the concentration of the hydrofluoric acid solution is 30%. And (3) taking out after standing for 5 seconds, washing with clear water for 1 minute, cleaning in an ultrasonic cleaning instrument filled with deionized water, and blow-drying with compressed air or naturally drying at room temperature.
FIG. 1 is a photograph of the surface of the titanium alloy after nanosecond laser processing according to the present embodiment; as can be seen from the figure: the titanium alloy surface appears pure black, and after visible light is irradiated on the titanium alloy surface, the reflected and scattered light is very little.
FIG. 2 is a scanning electron microscope photograph of the surface of the titanium alloy after the nanosecond laser treatment in the embodiment; as can be seen from the figure: the surface of the alloy presents regular pits, the diameter of each pit is slightly smaller than 100 micrometers, and the light trapping effect is good.
FIG. 3 is a scanning electron microscope photograph of the titanium alloy surface treated with the hydrofluoric acid solution according to the embodiment; the graph shows that the micron-sized holes and the nano-sized loose texture around the holes can further increase the light trapping effect.
Example 2
A method for preparing a titanium alloy surface with low reflectivity to visible light comprises the following steps:
(1) Surface cleaning pretreatment:
cleaning a TC4 titanium alloy sample to be treated in an ultrasonic cleaning instrument filled with deionized water, then cleaning with absolute ethyl alcohol (purity is more than 99.8%), drying the surface of the titanium alloy sample with compressed air or naturally drying at room temperature, and keeping the titanium alloy sample clean and dustproof to obtain a clean titanium alloy sample for later use.
(2) Preparing a pit-shaped milli-micro-nano tertiary structure on the surface of the titanium alloy by nanosecond laser:
(a) And (3) putting up and flatly placing four corners of the titanium alloy sample on a workbench, wherein air is arranged between the bottom surface of the titanium alloy sample and the workbench. Firstly, scanning a focused laser beam on the surface of a sample along the X direction, wherein the laser wavelength is 1064nm, the pulse width is 400ns, the single-pulse energy is 0.5mJ, the focused light spot is 20 mu m, the scanning speed is 2200mm/s, the adjacent interval is 0.15mm, and the scanning times are as follows: 250 times.
(b) And (2) scanning the surface of the sample by focusing laser beams along the Y direction, wherein the laser wavelength is 1064nm, the pulse width is 400ns, the single-pulse energy is 1mJ, the focusing light spot is 20 mu m, the scanning speed is 9500mm/s, the adjacent interval is 0.09mm, and the scanning times are as follows: 650 times.
(3) Fluoridizing with hydrofluoric acid to strengthen the surface nano texture:
and (3) placing the titanium alloy sample piece prepared by the laser in a hydrofluoric acid solution, wherein the concentration of the hydrofluoric acid solution is 30%. And (3) taking out after standing for 5 seconds, washing with clear water for 1 minute, cleaning in an ultrasonic cleaning instrument filled with deionized water, and blow-drying with compressed air or naturally drying at room temperature.
The pattern of the samples prepared in this example is identical to the pattern of the samples prepared in example 1.
Example 3
A method for preparing a titanium alloy surface with low reflectivity to visible light comprises the following steps:
(1) Surface cleaning pretreatment:
cleaning a TC4 titanium alloy sample to be treated in an ultrasonic cleaning instrument filled with deionized water, then cleaning with absolute ethyl alcohol (purity is more than 99.8%), drying the surface of the titanium alloy sample with compressed air or naturally drying at room temperature, and keeping the titanium alloy sample clean and dustproof to obtain a clean titanium alloy sample for later use.
(2) Preparing a pit-shaped milli-micro-nano tertiary structure on the surface of the titanium alloy by nanosecond laser:
(a) And (3) laying the four corners of the titanium alloy sample on a workbench, wherein air is arranged between the bottom surface of the titanium alloy sample and the workbench. Firstly, scanning a focused laser beam on the surface of a sample along the X direction, wherein the laser wavelength is 1064nm, the pulse width is 350ns, the single-pulse energy is 0.5mJ, the focused light spot is 20 mu m, the scanning speed is 1800mm/s, the adjacent interval is 0.10mm, and the scanning times are as follows: 220 times.
(b) And (2) scanning the surface of the sample by focusing a laser beam along the Y direction, wherein the laser wavelength is 1064nm, the pulse width is 350ns, the single-pulse energy is 1mJ, the focusing light spot is 20 mu m, the scanning speed is 8500mm/s, the adjacent interval is 0.05mm, and the scanning times are as follows: 400 times.
(3) Fluoridizing with hydrofluoric acid to strengthen the surface nano texture:
and (3) placing the titanium alloy sample piece prepared by the laser in a hydrofluoric acid solution, wherein the concentration of the hydrofluoric acid solution is 30%. And (3) taking out after standing for 5 seconds, washing with clear water for 1 minute, cleaning in an ultrasonic cleaning instrument filled with deionized water, and blow-drying with compressed air or naturally drying at room temperature.
The pattern of the samples prepared in this example is identical to the pattern of the samples prepared in example 1.
Example 4
A method for preparing a titanium alloy surface with low reflectivity to visible light comprises the following steps:
(1) Surface cleaning pretreatment:
cleaning a TC4 titanium alloy sample to be treated in an ultrasonic cleaning instrument filled with deionized water, then cleaning with absolute ethyl alcohol (the purity is more than 99.8%), blow-drying the surface of the titanium alloy sample with compressed air or naturally drying at room temperature, and paying attention to cleanness and dust prevention to obtain a clean titanium alloy sample for later use.
(2) Preparing a pit-shaped milli-micro-nano tertiary structure on the surface of the titanium alloy by nanosecond laser:
(a) And (3) putting up and flatly placing four corners of the titanium alloy sample on a workbench, wherein air is arranged between the bottom surface of the titanium alloy sample and the workbench. Firstly, scanning a focused laser beam on the surface of a sample along the X direction, wherein the laser wavelength is 1064nm, the pulse width is 450ns, the single-pulse energy is 0.5mJ, the focused light spot is 20 mu m, the scanning speed is 2400mm/s, the adjacent interval is 0.18mm, and the scanning times are as follows: 250 times.
(b) And (2) scanning the surface of the sample by focusing a laser beam along the Y direction, wherein the laser wavelength is 1064nm, the pulse width is 450ns, the single-pulse energy is 1mJ, the focusing light spot is 20 mu m, the scanning speed is 9500mm/s, the adjacent interval is 0.10mm, and the scanning times are as follows: and 700 times.
(3) Fluoridizing with hydrofluoric acid to strengthen the surface nano texture:
and (3) placing the titanium alloy sample piece prepared by the laser in a hydrofluoric acid solution, wherein the concentration of the hydrofluoric acid solution is 30%. And (3) taking out after standing for 5 seconds, washing with clear water for 1 minute, cleaning in an ultrasonic cleaning instrument filled with deionized water, and blow-drying with compressed air or naturally drying at room temperature.
The sample plots prepared in this example are identical to those prepared in example 1.
Comparative example 1
A method for preparing a titanium alloy surface with low reflectivity to visible light comprises the following steps:
(1) Surface cleaning pretreatment:
cleaning a TC4 titanium alloy sample to be treated in an ultrasonic cleaning instrument filled with deionized water, then cleaning with absolute ethyl alcohol (purity is more than 99.8%), drying the surface of the titanium alloy sample with compressed air or naturally drying at room temperature, and keeping the titanium alloy sample clean and dustproof to obtain a clean titanium alloy sample for later use.
(2) Preparing a pit-shaped milli-micro-nano tertiary structure on the surface of the titanium alloy by nanosecond laser:
(a) And (3) putting up and flatly placing four corners of the titanium alloy sample on a workbench, wherein air is arranged between the bottom surface of the titanium alloy sample and the workbench. Firstly, scanning a focused laser beam on the surface of a sample along the X direction, wherein the laser wavelength is 1064nm, the pulse width is 400ns, the single-pulse energy is 0.5mJ, the focused light spot is 20 mu m, the scanning speed is 2000mm/s, the adjacent interval is 0.15mm, and the scanning times are as follows: 200 times.
(b) And (2) scanning the surface of the sample by focusing a laser beam along the Y direction, wherein the laser wavelength is 1064nm, the pulse width is 400ns, the single-pulse energy is 1mJ, the focusing light spot is 20 μm, the scanning speed is 9000mm/s, the adjacent interval is 0.09mm, and the scanning times are as follows: 500 times.
(3) And (3) washing the titanium alloy sample prepared by the laser for 1 minute by using clean water, then putting the titanium alloy sample into an ultrasonic cleaning instrument filled with deionized water for cleaning, and then blowing the titanium alloy sample to dry by using compressed air or naturally drying the titanium alloy sample at room temperature.
FIG. 4 is a comparison result of the light absorption rate test of the titanium alloy surfaces prepared in examples 1-2 of the present invention and comparative example 1 in the visible light band. Wherein, the fluorination treatment a is the light absorption curve of the titanium alloy surface prepared in the example 1 in the visible light band, the fluorination treatment B is the light absorption curve of the titanium alloy surface prepared in the example 2 in the visible light band, and the air non-fluorination treatment is the light absorption curve of the titanium alloy surface prepared in the comparative example 1 in the visible light band, as can be seen from the figure: after the laser emitting method is adopted, the reflectivity of the surface of the titanium alloy is greatly reduced from more than or equal to 20 percent to about 2 percent. Then the skin care treatment is adopted, and the skin can be further reduced to about 1.5 percent. And after the fluorination treatment is adopted, the reflectivity result is good in stability and tends to be consistent.
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (3)
1. A method for preparing a titanium alloy surface with low reflectivity to visible light is characterized by comprising the following steps:
(1) Cleaning and pretreating the surface of a titanium alloy sample to be treated;
(2) Preparing a pit-shaped milli-micro-nano tertiary structure on the surface of the titanium alloy by nanosecond laser:
(a) Firstly, scanning a focused laser beam on the surface of a titanium alloy sample treated in the step (1) along the X-axis direction, wherein the laser wavelength is 1064nm, the pulse width is 350-450ns, the adjacent interval is 0.10-0.18mm, the single pulse energy of the laser is 0.5mJ, the focused light spot is 20 mu m, the scanning speed is 1800-2400mm/s, and the scanning times are 200-250;
(b) And (b) scanning the titanium alloy sample obtained in the step (a) by focusing laser beams on the surface of the sample along the Y-axis direction, wherein the laser wavelength is 1064nm, the pulse width is 350-450ns, the adjacent interval is 0.05-0.10mm, the single pulse energy of the laser is 1mJ, the focusing light spot is 20 mu m, the scanning speed is 8500-9500mm/s, and the scanning times are as follows: 400-700 times;
(3) Fluoridizing with hydrofluoric acid to strengthen the surface nano texture:
and (3) placing the titanium alloy sample treated in the step (2) into a hydrofluoric acid solution, soaking for 3-10s, taking out, cleaning and drying to obtain the titanium alloy surface with low reflectivity to visible light.
2. The method for preparing a titanium alloy surface having a low reflectance to visible light according to claim 1, wherein: in the step (1), the titanium alloy sample is any one of TC4, TA2 and TA15 titanium alloy samples.
3. The method for preparing a titanium alloy surface having a low reflectance to visible light according to claim 1, wherein: in the step (3), the concentration of the hydrofluoric acid solution is 30wt%.
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