CN113278911B - Method for greatly improving surface hardness of zirconium-based amorphous alloy by laser irradiation - Google Patents
Method for greatly improving surface hardness of zirconium-based amorphous alloy by laser irradiation Download PDFInfo
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- CN113278911B CN113278911B CN202110576475.5A CN202110576475A CN113278911B CN 113278911 B CN113278911 B CN 113278911B CN 202110576475 A CN202110576475 A CN 202110576475A CN 113278911 B CN113278911 B CN 113278911B
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- 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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/24—Nitriding
Abstract
The invention provides a method for greatly improving the surface hardness of a zirconium-based amorphous alloy through laser irradiation, belonging to the technical field of amorphous alloy surface modification. The method comprises the steps of carrying out nanosecond laser irradiation on the surface of the zirconium-based amorphous alloy in a nitrogen environment, introducing a zirconium nitride phase, optimizing laser parameters by utilizing orthogonal test design to regulate and control the content of the zirconium nitride phase, further controlling the surface hardness of the amorphous alloy, and greatly improving the surface hardness of the amorphous alloy after irradiation under the optimized experimental parameters. The method has the advantages of less test times of orthogonal test design, uniform data distribution and furthest reduction of test errors; the method has the advantages of high efficiency, simplicity, easy implementation, strong practicability and economy; the hardness can be regulated and controlled, the surface hardness of the zirconium-based amorphous alloy can be changed by regulating laser irradiation parameters, and the practical application of the zirconium-based amorphous alloy is enhanced.
Description
Technical Field
The invention relates to the technical field of amorphous alloy surface modification, in particular to a method for greatly improving the surface hardness of a zirconium-based amorphous alloy through laser irradiation. The orthogonal test design of the invention has the advantages of high efficiency, uniform data distribution, simple method, easy implementation, strong practicability and the like.
Background
The large cooling rate of the metal elements in the liquid phase enables the amorphous alloy to have no crystal atom structure and no crystal boundary and dislocation defects, so that the amorphous alloy has excellent properties, such as high strength, high elasticity and strong corrosion resistance. The characteristics lead the amorphous alloy to have potential application prospect in the fields of aerospace, precision machinery, military weapons and other fields. However, under tensile load, amorphous alloys are prone to highly localized shear band deformation, which limits their practical application as structural and engineering materials. Further, the high hardness of the amorphous alloy enables the amorphous alloy to be used as a functional contact material, and further improvement in the surface hardness is required for improving the applicability.
In recent years, laser nitriding has been applied to the improvement of the surface hardness of zirconium-based amorphous alloys. For example, Huang Hu et al in 2018 Journal of Alloys and Compounds 770-864-874 (The coupling effects of laser thermal shock and surface chemistry on mechanical properties of Zr-based metallic glass) achieved surface hardness enhancement by irradiating The surface of The zirconium-based amorphous alloy with nanosecond laser in a nitrogen atmosphere. However, up to now, this method only increases the surface hardness of the amorphous alloy by 15.7% because no parameter optimization is performed. Therefore, further systematic design experiment is urgently needed, laser parameters are optimized, and the surface hardness of the zirconium-based amorphous alloy is greatly improved so as to enhance the functional application of the amorphous alloy.
Disclosure of Invention
The invention aims to provide a method for greatly improving the surface hardness of a zirconium-based amorphous alloy through laser irradiation, which overcomes the problems in the prior art. The invention provides a method for greatly improving the surface hardness of a zirconium-based amorphous alloy by laser irradiation, which comprises the steps of carrying out nanosecond laser irradiation on the surface of the zirconium-based amorphous alloy in a nitrogen environment, introducing a zirconium nitride phase, optimizing laser parameters by using orthogonal test design to regulate and control the content of the zirconium nitride phase, further controlling the surface hardness of the amorphous alloy, and greatly improving the surface hardness of the amorphous alloy after irradiation under the optimized experimental parameters; the method comprises the following specific steps:
(1) mechanically grinding and polishing the surface of the zirconium-based amorphous alloy, cleaning by using alcohol, and then drying;
(2) a nanosecond pulse laser is used for irradiating the surface of the zirconium-based amorphous alloy in a nitrogen atmosphere, and laser parameters are changed through orthogonal test design, so that the surface hardness of the laser zirconium nitride-based amorphous alloy is regulated and controlled.
The nanosecond laser irradiation process parameters are as follows: the laser pulse width is 10ns, the wavelength is 1064nm, the repetition frequency is 600kHz, the spot diameter is 43 microns, the average laser power is 0.8-12.1W, the scanning speed is 10-80 mm/s, the overlapping rate of adjacent scanning lines is 10% -80%, and the laser irradiation frequency is 1-4.
After irradiation is carried out according to laser irradiation process parameters, the surface hardness of the amorphous alloy is remarkably improved, when the indentation load is 120mN, the surface hardness of the original amorphous alloy is 6.50GPa, the laser average power is 7.1W, the scanning speed is 10mm/s, the overlapping rate of adjacent scanning lines is 70%, the surface hardness can reach 24.68GPa at most after laser irradiation is carried out under the test condition that the laser irradiation frequency is 4, and the surface hardness is improved by 279% compared with the surface of the original amorphous alloy.
The laser irradiation process parameters are changed, and the surface hardness of the amorphous alloy can be regulated and controlled. The average laser power is adjusted in a range of 0.8-12.1W, the average surface hardness change range is 6.06-12.78 GPa, the scanning speed is adjusted in a range of 10-80 mm/s, the average surface hardness change range is 7.95-14.31 GPa, the overlapping rate of adjacent scanning lines is adjusted in a range of 10% -80%, the average surface hardness change range is 9.42-10.35 GPa, the laser irradiation frequency is adjusted in a range of 1-4, and the average surface hardness change range is 7.67-9.76 GPa.
The present invention belongs to the field of amorphous alloy surface modification technology. Specifically, the method comprises the steps of irradiating the surface of the amorphous alloy by nanosecond laser in a nitrogen atmosphere, and optimizing laser parameters by using orthogonal test design to regulate and control the content of zirconium nitride phase so as to control the surface hardness of the amorphous alloy. Compared with the prior art, the invention has the following characteristics:
the invention has the advantages of less test times, uniform data distribution and furthest reduced test errors.
The method has the advantages of high efficiency, simple method, easy implementation, strong practicability and economy.
The invention can realize the regulation and control of the surface hardness of the amorphous alloy by adjusting the laser irradiation parameters.
The nanosecond laser adopted by the invention can realize laser irradiation of various sizes and shapes by controlling the scanning path through a computer.
Based on the characteristics, the method is different from the prior art for improving the surface hardness of the amorphous alloy by laser nitridation, and is a novel, effective and practical technology capable of greatly improving the hardness of the amorphous alloy.
The purpose of the invention is realized by the following technical scheme:
firstly, grinding and polishing the surface of the amorphous alloy, and cleaning the surface of the amorphous alloy by using alcohol to obtain a smooth surface. According to the orthogonal test design, nanosecond laser is used for irradiating the surface of the amorphous alloy in a nitrogen atmosphere, nano indentations are used for testing the surface irradiated by different laser parameters, and the regulation and control of the surface hardness of the amorphous alloy can be realized by correlating the relation between the laser irradiation parameters and the surface hardness.
The invention provides a method for greatly improving the surface hardness of a zirconium-based amorphous alloy through laser irradiation, which comprises the following steps:
1. and grinding and polishing the amorphous alloy to obtain a smooth surface.
2. The amorphous alloy block is placed in a cuboid cavity into which nitrogen can be introduced, and laser processing is ensured to be carried out in the nitrogen.
3. Nanosecond laser is used, and a multi-line scanning mode is adopted.
4. And testing the surface hardness after laser irradiation by using a nanoindenter.
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 a schematic diagram of a nanosecond laser processing system according to the invention;
FIG. 2 is a comparison of the surface 1 of the zirconium-based amorphous alloy after laser irradiation in a nitrogen atmosphere according to the present invention with the original surface indentation curve;
FIG. 3 is a comparison of the surface 2 of the zirconium-based amorphous alloy after laser irradiation and the original surface indentation curve in a nitrogen atmosphere according to the present invention;
FIG. 4 is a comparison of the laser irradiated surface 3 of the zirconium-based amorphous alloy in the nitrogen atmosphere with the original surface indentation curve;
fig. 5 shows the comparison result of the laser irradiation of the surfaces 1, 2, 3 of the zirconium-based amorphous alloy in the nitrogen atmosphere with the x-ray diffraction (XRD) of the original surface.
Detailed Description
The details of the present invention and its embodiments are further described below with reference to the accompanying drawings.
The invention is further illustrated by the following specific examples, which, however, are to be construed as merely illustrative, and not limitative of the remainder of the disclosure in any way whatsoever.
Example 1
The embodiment is used for explaining the method for greatly improving the surface hardness of the zirconium-based amorphous alloy by laser irradiation.
Zr41.2Ti13.8Cu12.5Ni10Be22.5 amorphous alloy blocks with the thickness of 2 mm are selected, the surfaces of the amorphous alloy blocks are ground, No. 400, No. 800, No. 1200 and No. 2000 abrasive paper are used for grinding in sequence, then 0.5 micron diamond particle polishing paste is used for polishing until the mirror surfaces are smooth, and the surfaces are cleaned by alcohol. The block sample is placed in a cuboid cavity which can be filled with nitrogen, the mirror surface faces upwards, a nanosecond laser is used, the wavelength of the nanosecond laser is 1064nm, the diameter of a focusing light spot is 43 mu m, the pulse width is 10ns, and the nanosecond laser is processed in the nitrogen according to the orthogonal test design.
Fig. 2 shows the indentation curve and the hardness value of the irradiated surface and the original surface obtained after laser irradiation under the test conditions that the average laser power is 12.1W, the scanning speed is 10mm/s, the overlapping rate of adjacent scanning lines is 10%, and the laser irradiation frequency is 3, and it can be seen that when the indentation load is 120mN, the hardness value obtained by irradiating the surface in a nitrogen atmosphere is 15.43GPa, which is improved by 137% compared with the hardness of the original surface of 6.50 GPa.
Fig. 3 shows the indentation curve and the hardness value of the irradiated surface and the original surface obtained after laser irradiation is performed under the test conditions that the average laser power is 10.5W, the scanning speed is 10mm/s, the overlapping rate of adjacent scanning lines is 30%, and the laser irradiation frequency is 2, and it can be seen that when the indentation load is 120mN, the hardness value obtained by irradiating the surface in a nitrogen atmosphere is 19.72GPa, which is improved by 203% compared with the hardness of the original surface being 6.50 GPa.
Fig. 4 shows the indentation curve and the hardness value of the irradiated surface and the original surface obtained after laser irradiation is performed under the test conditions that the average laser power is 7.1W, the scanning speed is 10mm/s, the overlapping rate of adjacent scanning lines is 70%, and the laser irradiation frequency is 4, and it can be seen that when the indentation load is 120mN, the hardness value obtained by the irradiated surface in a nitrogen atmosphere is 24.68GPa, which is improved by 279% compared with the hardness of the original surface of 6.50GPa, which indicates that the surface hardness of the zirconium-based amorphous alloy surface is significantly improved after laser irradiation is performed on the zirconium-based amorphous alloy surface by using the optimized parameters of the orthogonal test design.
Fig. 5 shows the comparison result of x-ray diffraction (XRD) of the surface after laser irradiation and the original surface obtained under the test conditions of fig. 2, fig. 3 and fig. 4, and it can be seen that the laser irradiation induces the zirconium nitride phase to be generated on the surface of the zirconium-based amorphous alloy in the nitrogen atmosphere, further proving the reason for the improvement of the surface hardness.
The above examples show that the orthogonal test design greatly improves the surface hardness of the zirconium-based amorphous alloy and the effectiveness and feasibility of surface hardness regulation under laser irradiation. The method is suitable for improving the surface hardness of the amorphous alloy samples with different sizes and shapes, and further enhances the applicability of the amorphous alloy samples.
Although the present invention has been described to a certain extent, it is apparent that appropriate changes in the respective conditions may be made without departing from the spirit and scope of the present invention. It is to be understood that the invention is not limited to the described embodiments, but is to be accorded the scope consistent with the claims, including equivalents of each element described.
Claims (2)
1. A method for greatly improving the surface hardness of a zirconium-based amorphous alloy through laser irradiation is characterized by comprising the following steps: the method comprises the steps of carrying out nanosecond laser irradiation on the surface of the zirconium-based amorphous alloy in a nitrogen environment, introducing a zirconium nitride phase, optimizing laser parameters by using orthogonal test design to regulate and control the content of the zirconium nitride phase, and further controlling the surface hardness of the amorphous alloy, and comprises the following specific steps:
(1) mechanically grinding the surface of the zirconium-based amorphous alloy, sequentially grinding with No. 400, No. 800, No. 1200 and No. 2000 abrasive paper, then polishing with 0.5 micron diamond particle polishing paste to obtain a smooth mirror surface, cleaning the surface by using alcohol, and then drying;
(2) according to the orthogonal test design, nanosecond laser is used for irradiating the surface of the amorphous alloy in a nitrogen atmosphere, nano indentations are used for testing the surface irradiated by different laser parameters, and the regulation and control of the surface hardness of the amorphous alloy can be realized by correlating the relation between the laser irradiation parameters and the surface hardness;
(3) after irradiation is carried out according to laser irradiation process parameters, the surface hardness of the amorphous alloy is remarkably improved, when the indentation load is 120mN, the surface hardness of the original amorphous alloy is 6.50GPa, the laser average power is 7.1W, the scanning speed is 10mm/s, the overlapping rate of adjacent scanning lines is 70%, the surface hardness can reach 24.68GPa after laser irradiation is carried out under the test condition that the laser irradiation frequency is 4, and the surface hardness is improved by 279% compared with the surface of the original amorphous alloy.
2. The method for greatly improving the surface hardness of the zirconium-based amorphous alloy through laser irradiation according to claim 1, wherein the method comprises the following steps: the nanosecond laser irradiation process parameters are as follows: the laser pulse width is 10ns, the wavelength is 1064nm, the repetition frequency is 600kHz, and the spot diameter is 43 μm.
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