CN113118633B - Method for preparing periodic microstructure on surface of titanium alloy through nanosecond laser irradiation - Google Patents
Method for preparing periodic microstructure on surface of titanium alloy through nanosecond laser irradiation Download PDFInfo
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- CN113118633B CN113118633B CN202110429325.1A CN202110429325A CN113118633B CN 113118633 B CN113118633 B CN 113118633B CN 202110429325 A CN202110429325 A CN 202110429325A CN 113118633 B CN113118633 B CN 113118633B
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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
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- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
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Abstract
The invention relates to a method for preparing a periodic microstructure on a titanium alloy surface by nanosecond laser irradiation, and belongs to the field of laser surface modification. The method 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, and vertically irradiating the focused laser beam on the surface of the titanium alloy sample through silica glass; by controlling laser parameters, a periodic microstructure is prepared on the surface of the titanium alloy, and the effect of laser nitridation is achieved. The invention can not only improve the wetting property of the titanium alloy surface, but also realize the regulation and control of the surface color, and in addition, the hardness and the wear resistance of the titanium alloy surface after laser irradiation are improved due to the action of laser nitridation. The surface microstructure provided by the invention is simple in preparation method and good in 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)
1. A method for preparing a periodic microstructure on the surface of a titanium alloy by nanosecond laser irradiation is characterized by comprising the following steps: firstly, the surface of the titanium alloy is pretreated, the pretreated titanium alloy sample is placed in a gas cavity, nitrogen is conveyed through the air inlet to fill the air cavity with the nitrogen, after the pre-air conveying for 10 to 15 seconds, opening the nanosecond fiber laser, vertically irradiating the focused laser beam on the surface of the titanium alloy sample through silica glass, controlling laser parameters, 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 the laser scanning lines is 5-20 μm, the central wavelength is 1064nm, the diameter of the Gaussian spot is 42 μm, preparing a periodic microstructure with modulation depth of 50-200nm and space period of 0.9-1.2 mu m on the surface of the titanium alloy, and simultaneously playing a role in laser nitridation.
2. The method for preparing the periodic microstructure on the surface of the titanium alloy by nanosecond laser irradiation, which is characterized in that 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.
3. The method for preparing the periodic microstructure on the surface of the titanium alloy through nanosecond laser irradiation, as claimed in claim 2, wherein the mechanical grinding is sequentially performed by using 200#, 400#, 800#, 1200#, 1500#, 2000# sandpaper, and then the mechanical polishing is performed by using diamond abrasive pastes of W5, W3, W1, the cleaning temperature of the ultrasonic cleaning is set to be 50-60 ℃, the cleaning time is 5-10min, and the titanium alloy is naturally dried in the air.
4. The method for preparing the periodic microstructure on the surface of the titanium alloy through nanosecond laser irradiation, as claimed in claim 1, wherein the laser for preparing the periodic microstructure is a nanosecond fiber laser.
5. The method for preparing the periodic microstructure on the surface of the titanium alloy through nanosecond laser irradiation, as claimed in claim 1, wherein the nitrogen gas is high-purity nitrogen gas, and the gas flow rate is 5-15L/min.
6. The method for preparing the periodic microstructure on the surface of the titanium alloy by nanosecond laser irradiation, as claimed in claim 1, wherein the periodic surface microstructure can change the wetting property of the surface of the titanium alloy, and has two or more colors, the surface hardness of the periodic surface microstructure is 6-15GPa, and the friction coefficient under the scratch load of 5-15N is 0.08-0.12.
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