CN113118633B - Method for preparing periodic microstructure on surface of titanium alloy through nanosecond laser irradiation - Google Patents
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 59
- 230000000737 periodic effect Effects 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000007789 gas Substances 0.000 claims abstract description 19
- 239000000835 fiber Substances 0.000 claims abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000009736 wetting Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims description 9
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000005498 polishing Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- 229910003460 diamond Inorganic materials 0.000 claims description 3
- 239000010432 diamond Substances 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims 4
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 14
- 238000002360 preparation method Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract description 3
- 230000004048 modification Effects 0.000 abstract description 3
- 230000033228 biological regulation Effects 0.000 abstract description 2
- 238000005121 nitriding Methods 0.000 abstract description 2
- 229910000883 Ti6Al4V Inorganic materials 0.000 description 17
- 238000012545 processing Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 6
- 239000003086 colorant Substances 0.000 description 4
- 238000007373 indentation Methods 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 3
- 230000001678 irradiating effect Effects 0.000 description 3
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000013532 laser treatment Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012935 Averaging Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 230000003075 superhydrophobic effect Effects 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
- B23K26/355—Texturing
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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
- 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
- B23K26/70—Auxiliary operations or equipment
- B23K26/702—Auxiliary equipment
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Abstract
本发明涉及一种纳秒激光辐照制备钛合金表面周期性微结构的方法，属于激光表面改性领域。该方法为：先对钛合金表面进行预处理，将预处理后的钛合金样品放置于气体腔中，通过进气口输送氮气，使氮气充满气体腔，氮气流量为1‑20L/min；经过10‑15s的预送气后，打开纳秒光纤激光器，将聚焦后的激光束经过二氧化硅玻璃垂直照射于钛合金样品表面；通过控制激光参数，在钛合金表面制备周期性微结构，同时起到激光氮化的作用。本发明不仅可以改善钛合金表面的湿润性能，并且可以实现表面颜色的调控，此外由于激光氮化的作用，激光辐照后钛合金表面的硬度和耐磨性得到提高。本发明提供的表面微结构制备方法简单，重复性好，且制备的结构具有优异的耐久性。
The invention relates to a method for preparing a periodic microstructure of a titanium alloy surface by nanosecond laser irradiation, and belongs to the field of laser surface modification. The method is as follows: first pretreating the surface of the titanium alloy, placing the pretreated titanium alloy sample in a gas chamber, conveying nitrogen through the air inlet to fill the gas chamber with nitrogen, and the nitrogen flow rate is 1-20L/min; After 10-15s of pre-gassing, the nanosecond fiber laser was turned on, and the focused laser beam was irradiated vertically on the surface of the titanium alloy sample through the silica glass; by controlling the laser parameters, periodic microstructures were prepared on the surface of the titanium alloy, and at the same time to the effect of laser nitridation. The invention can not only improve the wetting performance of the titanium alloy surface, but also realize the regulation of the surface color, and in addition, due to the effect of laser nitriding, the hardness and wear resistance of the titanium alloy surface after laser irradiation are improved. The preparation method of the surface microstructure provided by the invention is simple and has good repeatability, and the prepared structure has excellent durability.
Description
Technical Field
The invention relates to the technical field of metal surface modification, in particular to a method for preparing a periodic microstructure on a titanium alloy surface by nanosecond laser irradiation.
Background
Titanium alloys have excellent mechanical, physical and chemical properties, such as high specific strength, low density, good high temperature retention, and excellent corrosion resistance and biocompatibility, and are widely used in the fields of national defense, aerospace, biomedicine and others. But its inherent disadvantages, such as high friction coefficient, low hardness and wear resistance, limit the industrial application range to some extent.
The preparation of the material surface microstructure can improve the surface wettability, the optical characteristics, the biocompatibility, the friction and wear performance and the like, and obviously, the preparation of the microstructure on the titanium alloy surface can provide larger development space and application potential for the titanium alloy. However, most of the surface microstructures have extremely poor durability and short service life, and the surface microstructures prepared in a special way are easily affected by environmental factors such as optics, temperature and the like, so that the surface microstructures are easily damaged (Li Xiao, Limni, Wang Yuxuan, research progress of multifunctional and durable superhydrophobic surfaces, Nature science of university in Hunan province, 2020).
Therefore, how to prepare the multifunctional and high-durability surface microstructure is of great significance.
Titanium nitride has high hardness, good chemical stability and excellent wear resistance and corrosion resistance, is a common coating material, and is used as a cutter coating to improve the hardness and wear resistance of the cutter. Aiming at poor wear resistance and the like of titanium alloy, an attempt can be made to prepare a layer of titanium nitride on the surface of the titanium alloy in a nitriding manner (Qinxiang, Huangting, Shoulongshi, Ti surface microstructure preparation and application research progress, electromachining and die, 2019, (4): 1-9).
Laser processing is used as a high-precision, flexible and pollution-free mode, is suitable for most materials, and can expose corners in the aspect of preparation of micro-nano structures. The laser devices are various, and the nanosecond laser device is low in cost, can give consideration to both processing efficiency and processing quality, and is successfully applied to industrialization at present. For the interaction of nanosecond laser and material, the heat effect is inevitable, which causes uncontrollable local flow and evaporation of the melt, and it is difficult to prepare a relatively regular periodic structure on the surface of the material. Therefore, there is a need for a simple, efficient and durable method for producing periodic microstructures on a surface.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for preparing a periodic microstructure on the surface of a titanium alloy by nanosecond laser irradiation, which can improve the wetting property of the surface of the titanium alloy and also play a role in color regulation, and in addition, due to the action of laser nitridation, the surface shows higher surface hardness and better frictional wear performance, the preparation method is simple, the repeatability is better, and the prepared structure has excellent durability.
The above object of the present invention is achieved by the following technical solutions:
a method for preparing a periodic microstructure on a titanium alloy surface by nanosecond laser irradiation comprises the following steps: firstly, pretreating the surface of a titanium alloy, placing a pretreated titanium alloy sample in a gas cavity, and conveying nitrogen through a gas inlet to fill the gas cavity with the nitrogen, wherein the flow rate of the nitrogen is 1-20L/min; after pre-feeding gas for 10-15s, turning on a nanosecond fiber laser, vertically irradiating the focused laser beam on the surface of a titanium alloy sample through silica glass, and preparing a periodic surface microstructure on the surface of the titanium alloy by controlling laser parameters and playing a role in laser nitridation.
The pretreatment mode of the titanium alloy is as follows: and (3) mechanically grinding and polishing the titanium alloy sample subjected to wire cutting, putting the titanium alloy sample into absolute ethyl alcohol for ultrasonic cleaning, and drying.
The mechanical grinding is carried out by sequentially using 200#, 400#, 800#, 1200#, 1500#, 2000# sandpaper, then mechanically polishing by using diamond grinding pastes of W5, W3, W1, and naturally drying in air, wherein the cleaning temperature of ultrasonic cleaning is 50-60 ℃, and the cleaning time is 5-10 min.
The laser for preparing the periodic surface microstructure is a nanosecond fiber laser.
Preferably, the method comprises the following steps: the nitrogen is high-purity nitrogen, and the gas flow rate is 5-15L/min.
Preferably, the method comprises the following steps: the laser processing parameters comprise laser power, laser scanning speed, laser repetition frequency, laser pulse width, central wavelength and spot diameter, wherein the laser power is 4.04-5.21W, the laser scanning speed is 5-15mm/s, the laser repetition frequency is 500-1000kHz, the laser pulse width is 7-20ns, the spacing of laser scanning lines is 5-20 mu m, the central wavelength is 1064nm, and the diameter of a Gaussian spot is 42 mu m. By adopting the mode, a regular periodic surface structure can be prepared on the surface of the titanium alloy, and the titanium alloy has the functions of improving the wetting property, regulating and controlling the color and improving the surface hardness and the frictional wear property.
Preferably, the method comprises the following steps: after the laser processing parameters are adjusted, the structure modulation depth of the periodic surface structure prepared on the surface of the titanium alloy is 50-200nm, and the space period of the periodic surface structure is 0.9-1.2 mu m.
Preferably, the method comprises the following steps: the periodic surface microstructure can change the wetting property of the titanium alloy surface, has more than two colors, has the surface hardness of 6-10GPa and the friction coefficient of 0.08-0.12 under the scratch load of 5-15N.
Compared with the prior art, the invention has the following remarkable advantages:
the invention adopts nanosecond laser irradiation to induce the titanium alloy to form the multifunctional periodic surface microstructure, has simple operation, low processing cost, high efficiency, good repeatability, no pollution and can be used for large-scale industrial production. The surface structure can be adjusted by designing different laser processing parameters, so that a multifunctional and high-durability periodic surface microstructure can be realized on a titanium alloy sample, and the surface microstructure has a wide application prospect.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention.
FIG. 1 is an SEM image of a periodic surface microstructure of a Ti6Al4V sample and a cross-sectional image of the corresponding structure;
FIG. 2 is an image of the periodic surface microstructure of Ti6Al4V sample showing different colors at different camera angles;
FIG. 3 is a schematic diagram of the contact angles of the original surface and the laser-machined surface of the Ti6Al4V sample;
FIG. 4 is a schematic diagram of the hardness of the original surface and the laser processed surface of a Ti6Al4V sample under different indentation loads, and the corresponding indentation curve under the indentation load of 600 mN;
fig. 5 is a graph of the coefficient of friction of the original surface of the Ti6Al4V sample and the laser machined surface at a scratch load of 15N.
Detailed Description
The details and embodiments of the present invention are further described below with reference to the examples and the drawings, but the present invention is not limited thereto, and the experimental methods are conventional methods unless otherwise specified, and the materials and reagents can be obtained from ordinary sources unless otherwise specified.
A method for preparing a periodic microstructure on a titanium alloy surface by nanosecond laser irradiation comprises the following specific implementation steps: firstly, pretreating the surface of a titanium alloy, placing a pretreated titanium alloy sample in a gas cavity, and conveying nitrogen through a gas inlet to fill the gas cavity with the nitrogen, wherein the flow rate of the nitrogen is 1-20L/min; after pre-feeding gas for 10-15s, turning on a nanosecond fiber laser, vertically irradiating the focused laser beam on the surface of a titanium alloy sample through silica glass, and preparing a periodic surface microstructure on the surface of the titanium alloy by controlling laser parameters and playing a role in laser nitridation.
In a further embodiment, the pretreatment method of the titanium alloy is as follows: and (3) mechanically grinding and polishing the titanium alloy sample subjected to wire cutting, putting the titanium alloy sample into absolute ethyl alcohol for ultrasonic cleaning, and drying.
In a further embodiment, the mechanical grinding is carried out by sequentially using 200#, 400#, 800#, 1200#, 1500#, 2000# sandpaper, then the mechanical polishing is carried out by using diamond grinding pastes of W5, W3, W1, the cleaning temperature of ultrasonic cleaning is set to be 50-60 ℃, the cleaning time is 5-10min, and the abrasive is naturally dried in the air.
In a further embodiment, the laser used is a nanosecond fiber laser.
In a further embodiment, the nitrogen used is high purity nitrogen at a gas flow rate of 5-15L/min.
In a further embodiment, the laser processing parameters include laser power, laser scanning speed, laser repetition frequency, laser pulse width, center wavelength, and spot diameter, wherein the laser power is 4.04-5.21W, the laser scanning speed is 5-15mm/s, the laser repetition frequency is 500-1000kHz, the laser pulse width is 7-20ns, the spacing between laser scanning lines is 5-20 μm, the center wavelength is 1064nm, and the diameter of the Gaussian spot is 42 μm.
In a further embodiment, by adjusting laser processing parameters, the modulation depth of the periodic surface structure prepared on the surface of the titanium alloy is 50-200nm, and the spatial period is 0.9-1.2 μm.
In further embodiments, the prepared periodic surface microstructure can change the wetting property of the titanium alloy surface, has more than two colors, has the surface hardness of 6-15GPa and the friction coefficient of 0.08-0.12 under the scratch load of 5-15N.
Example 1:
the following titanium alloy is preferably Ti6Al4V, which is one of the most widely used titanium alloys currently used in the fields of machinery, aerospace, biomedicine, etc., but other types of titanium alloys may also be used.
(1) The Ti6Al4V raw material is cut into square samples with the size of 20mm multiplied by 3mm by a linear cutting mode, the Ti6Al4V samples are subjected to mechanical grinding and polishing treatment, and ultrasonic cleaning is carried out for 5min by using absolute ethyl alcohol, the cleaning temperature of the ultrasonic cleaning is 50 ℃, and the samples are naturally dried in the air.
(2) Placing the treated Ti6Al4V sample in a gas cavity, opening a gas valve, introducing high-purity nitrogen at a gas flow rate of 5L/min, pre-feeding gas for 10-15s, opening a nanosecond laser, and vertically irradiating the focused laser beam on the surface of the titanium alloy sample through silicon dioxide glass.
(3) Adjusting nanosecond laser parameters, setting the laser power to be 4.46W through control software, setting the laser scanning speed to be 10mm/s, setting the laser repetition frequency to be 700kHz, setting the laser pulse width to be 7ns, setting the laser scanning line interval to be 15 mu m, setting the central wavelength to be 1064nm and setting the Gaussian spot diameter to be 42 mu m, carrying out continuous line scanning, setting the modulation depth of a periodic surface structure prepared on the titanium alloy surface to be 100nm, setting the space period to be 1 mu m, and referring to the detailed structure in figure 1.
(4) Observation and experiment were performed on the Ti6Al4V sample after laser processing. By changing the observation angle, the Ti6Al4V surface appears different colors, as can be seen in fig. 2. The average contact angle was measured by 5 times averaging 5 μ L of deionized water dropped on different positions of the surface using a contact angle measuring instrument, and the average contact angle of the laser-processed Ti6Al4V surface was 45 °, which was 17 ° smaller than the polished surface, and slightly increased its hydrophilic properties, as shown in fig. 3.
(5) The laser processed Ti6Al4V surface was polished to remove surface structure and the hardness of the surface was characterized using a nanoindenter, see fig. 4, with the laser processed surface hardness at different indentation loads ranging from 5.8 GPa to 7.7GPa, an increase of 2-4GPa over the original surface hardness (3.6 GPa).
(6) See fig. 5, which is a graph of the coefficient of friction of the Ti6Al4V surface before and after nanosecond laser machining at different scratch loads. The results show that the surface friction coefficient of Ti6Al4V after laser treatment at a scratch load of 15N was 0.12 ± 0.01, while the surface friction coefficient of Ti6Al4V before laser treatment at a scratch load of 15N was between 0.38 and 0.42, greatly improving the friction properties of the Ti6Al4V surface.
The foregoing is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Obvious variations or modifications which are within the spirit of the invention are possible within the scope of the invention.
Claims (6)
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| CN114160807B (en) * | 2021-12-02 | 2023-08-29 | 吉林大学 | Method for nanosecond laser lifting forming of amorphous alloy surface |
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| CN104985328A (en) * | 2015-05-28 | 2015-10-21 | 湖北工业大学 | Method for preparing titanium alloy super-hydrophobic anti-frost surface using short pulse laser |
| CN110257765A (en) * | 2019-06-05 | 2019-09-20 | 中国船舶重工集团公司第七二五研究所 | A kind of preparation method of titanium alloy super-hydrophobic structure |
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| CN107345289B (en) * | 2017-06-07 | 2019-09-17 | 暨南大学 | A kind of method that laser prepares titanium alloy nitrogen titanium coating textured surfaces |
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