CN115717231B - Paracrystalline metal material, preparation method and application thereof - Google Patents
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Abstract
The invention relates to the technical field of materials, and particularly provides a secondary crystal metal material, a preparation method and application thereof; the secondary crystal metal material comprises a metal material and a secondary crystal phase formed on the metal material; an amorphous interlayer is arranged between adjacent secondary crystals in the secondary crystal phase state; the secondary crystal phase state and the amorphous phase state are in space discretized mosaic distribution; the interior of each of the secondary crystals is defect-free; in the secondary crystal metal material, the secondary crystal phase state has small size and high density, and forms a space mosaic distribution state with an amorphous phase state; the material has extremely stable intrinsic low surface energy, and greatly prolongs the super-hydrophobic property of the material surface; furthermore, the coating has excellent anti-corrosion effect.
Description
Technical Field
The invention relates to the technical field of secondary crystal metal materials, in particular to a secondary crystal metal material, a preparation method and application thereof.
Background
In recent years scientists around the world have been striving to improve the intrinsic properties of materials by changing their chemical composition and organization, for example: material hardness and plasticity, etc. Nanocrystalline and amorphous metals are widely recognized as one of the research hotspots in materials science and its application fields as an emerging metastable material. For nanocrystalline metals, as the average particle size thereof decreases, the mechanical strength and hardness of the material will correspondingly increase, resulting in wide application prospects. Although the nanocrystalline formation is a low-energy state which is theoretically thermodynamically stable, its geometric dimensions are generally large (10 or more nm), and therefore, many internal defects such as dislocation, twin crystal and vacancy are usually accompanied, and not only the bulk material constructed based on close contact therebetween will bring about abnormally abundant grain boundary energy due to the presence of a large number of nano grain boundaries, so that the material as a whole exhibits a thermodynamically unstable state with high free energy.
For amorphous materials, the atomic arrangement does not have long-range periodicity, so that the amorphous material has the characteristic of isotropy in a macroscopic sense, and has the advantages of good toughness, high hardness, corrosion resistance and the like of common polycrystalline metals and glasses. On the other hand, the entropy value of the surface of the material is increased due to the long-range disorder of the atomic arrangement, and the material presents a high free energy state which is unstable thermodynamically. It is important to find a special phase state between amorphous and nanocrystalline to effectively reduce the surface energy of the material.
Recently, researchers at the Beijing high-pressure scientific research center have successfully prepared diamond materials composed of sub-nanometer scale sub-crystals that exhibit an ordered arrangement over a few atomic ranges using a high-temperature and high-pressure environment. Although the new form similar to the microcrystalline glass fills the missing link in the atomic arrangement scale between the amorphous structure and the crystal structure, the research on the secondary crystal material is still in the starting stage at present, and particularly the formation of the secondary crystal phase state on the metal material is not found yet.
Disclosure of Invention
The invention aims to solve the problems and provides a novel secondary crystallization low-surface-energy metal material which forms a secondary crystal phase state on the basis of the metal material, and a preparation method and application thereof.
The invention provides a secondary crystal metal material, which comprises a metal material and secondary crystal phases formed on the metal material, wherein an amorphous phase interlayer is arranged between adjacent secondary crystals in the secondary crystal phases; the secondary crystal phase state and the amorphous phase state are in space discretized mosaic distribution; each of the paracrystalline phases is internally defect-free.
Preferably, the size of the secondary crystals in the secondary crystal phase is in the range of 0.3nm to 1nm, and the density of the secondary crystals is 1×10 4 Individual/μm 2 ～3×10 4 Individual/μm 2 。
Preferably, the thickness of the amorphous interlayer between the adjacent secondary crystals is 0.2-nm-30 nm; the depth of the space distribution of the paracrystalline amorphous mosaic phase is 5-10 mu m.
The invention provides a preparation method of the paracrystalline metal material, which comprises the following steps:
s1, ablating the metal material by using ultrafast laser to generate a supernano crystalline phase and an amorphous phase on the metal material, and forming an initial micro-nano structure surface;
s2, irradiating again through ultrafast laser, doping a doping substance into the surface of the initial microstructure, so that the state of the supernano crystal phase is crushed into an amorphous phase, and the surface of the micro-nano structure is obtained;
s3, carrying out low-temperature annealing treatment on the surface of the micro-nano structure to form a secondary crystal phase state, wherein an amorphous phase interlayer is formed between adjacent secondary crystals of the secondary crystal phase state; and as the time of the low-temperature annealing treatment increases, the density of the secondary crystals increases, the size of the secondary crystals decreases, and the thickness of the amorphous interlayer decreases, so that the secondary crystal metal material is obtained.
Preferably, the metal material is aluminum alloy, and the supernanocrystalline component and the amorphous component are both aluminum oxide; the pulse width of the ultrafast laser is 40fs, and the ultrafast laser isThe heart wavelength is 800nm, and the pulse frequency of the ultrafast laser is 1kHz; the doping substance is SiO 2 、CO 2 Gas, calcium fluoride crystals or optically transparent substances.
Preferably, in the step S2, the thickness of the amorphous interlayer between the adjacent secondary crystals is 1 nm-50 nm; the space distribution depth of the paracrystalline amorphous mosaic phase is 5-10 mu m.
Preferably, in the step S3, the temperature range of the low-temperature annealing treatment is 150 ℃ to 300 ℃, and the time range of the low-temperature annealing treatment is 3 hours to 23 hours.
The invention also provides other preparation methods of the secondary crystal metal material, wherein the preparation methods comprise a magnetron sputtering method, a laser cladding method or a high-temperature high-pressure method.
The invention also provides application of the secondary crystal metal material, and the secondary crystal metal material is applied to the corrosion resistance field, the super-hydrophobic field, the self-cleaning field, the biofouling prevention field, the icing resistance field or the water resistance reduction field.
In the paracrystalline low-surface-energy paracrystalline metal material prepared by the method, the paracrystalline phase is small in size and large in density, and forms a space mosaic distribution state with an amorphous phase; the material has extremely stable intrinsic low surface energy, and greatly prolongs the super-hydrophobic property of the material surface; moreover, the coating has high stable superhydrophobic effect and excellent anti-corrosion effect.
Drawings
FIG. 1 is a scanning electron micrograph of a micro-nano structure prepared in example 1 of the present invention.
FIG. 2 is a scanning electron micrograph of a micro-nano structure prepared in example 2 of the present invention.
Fig. 3 is a high-definition transmission electron TEM micrograph of the surface of the paracrystalline low surface energy paracrystalline metal material prepared in example 1 of the present invention.
Fig. 4 is an inverse fourier transform IFFT image of the paracrystalline low surface energy paracrystalline metal material prepared in example 1 of the present invention.
Fig. 5 is a high-definition transmission electron TEM micrograph of the surface of the paracrystalline low surface energy paracrystalline metal material prepared in example 2 of the present invention.
Fig. 6 is an inverse fourier transform IFFT image of the paracrystalline low surface energy paracrystalline metal material prepared in example 2 of the present invention.
FIG. 7 is a bar graph of the statistical distribution of the paracrystalline layer of the paracrystalline low surface energy paracrystalline metal material prepared in example 1 of the present invention.
Fig. 8 is a bar graph of the statistical distribution of the amorphous interlayer of the paracrystalline low surface energy paracrystalline metallic material prepared in example 1 of the present invention.
Fig. 9 is a bar graph of the statistical distribution of the paracrystalline metal material paracrystalline layer of the paracrystalline low surface energy produced in example 2 of the present invention.
Fig. 10 is a bar graph of the statistical distribution of the amorphous interlayer of the paracrystalline low surface energy paracrystalline metallic material prepared in example 2 of the present invention.
Fig. 11 is a graph showing the variation of contact angle of the paracrystalline low surface energy paracrystalline metal material prepared in example 1 and example 2 according to the present invention in a seawater immersion environment.
Fig. 12 is the electrochemical test results of the paracrystalline low surface energy paracrystalline metal material prepared in example 1 and example 2 of the present invention in seawater.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not to be construed as limiting the invention.
The invention provides a secondary crystal metal material, which comprises a metal material and secondary crystal phase states formed on the metal material, wherein an amorphous phase interlayer is arranged between adjacent secondary crystals in the secondary crystal phase states; the secondary crystal phase state and the amorphous phase state are in space discretization mosaic distribution; each of the paracrystalline phases is internally defect-free. Specifically, the size of the secondary crystals in the secondary crystal phase is in the range of 0.3nm to 1nm, and the density of the secondary crystals is 1×10 4 Individual/μm 2 ～3×10 4 Individual/μm 2 The method comprises the steps of carrying out a first treatment on the surface of the The thickness of the amorphous interlayer between the adjacent secondary crystals is 0.2nm to the whole width30nm; the space distribution depth of the paracrystalline amorphous mosaic phase is 5-10 mu m.
The invention further provides a preparation method of the paracrystalline metal material, which comprises the following steps:
s1, ablating the metal material by using ultrafast laser to convert the metal material from a polycrystalline phase state to a supernanocrystalline phase state and an amorphous phase state, generating the supernanocrystalline phase state and the amorphous phase state on the metal material, and forming an initial micro-nano structure surface to enable the material to be in a super-hydrophilic state with high surface energy; the metal material can be aluminum alloy, and the supernanocrystalline component and the amorphous component are aluminum oxide; the metal material may be magnesium alloy, stainless steel or the like in addition to aluminum alloy; the tight embedding of a large number of secondary crystals and ultrathin amorphous interlayers and the space discretization distribution of the secondary crystals and the ultrathin amorphous interlayers can be generated; specifically, the ultrafast laser may be a femtosecond laser, the pulse width of the ultrafast laser is 40fs, the center wavelength of the ultrafast laser is 800nm, and the pulse frequency of the ultrafast laser is 1kHz; focusing the light beam of the ultrafast laser to the surface of the metal material by using a lens for ablation; the material low-energy surface based on the secondary crystal and amorphous mosaic distribution characteristics is formed by firstly preparing a large number of supernano crystals and amorphous phases on the surface of the aluminum alloy by using ultra-fast laser.
S2, irradiating again through ultrafast laser, doping a doping substance into the surface of the initial microstructure, so that the state of the supernano crystal phase is crushed into an amorphous phase, and the surface of the micro-nano structure is obtained; the amorphous phase is usually metastable and has high thermodynamic free energy, so that the surface of the micro-nano structure of the material presents super-hydrophilic performance, and the corrosion resistance to seawater is poor; the doping substance is SiO 2 、CO 2 Gas, calcium fluoride crystals or optically transparent substances; after the step, only a small amount of secondary crystals exist on the surface of the micro-nano structure, the size range of the secondary crystals in the secondary crystal phase is 1 nm-2 nm, and the density of the secondary crystals is 1 multiplied by 10 3 Individual/μm 2 ～9×10 3 Individual/μm 2 The method comprises the steps of carrying out a first treatment on the surface of the Thickness of amorphous interlayer between adjacent sub-crystals1nm to 50nm, and the secondary crystal has no defect inside; at this time, the surface of the material contains a large number of unordered amorphous phases, the space distribution depth of the secondary amorphous mosaic phase is 5-10 mu m, and therefore the surface of the material still presents a super-hydrophilic state with high energy instability.
S3, carrying out low-temperature annealing treatment on the surface of the micro-nano structure to form a secondary crystal phase state, wherein an amorphous phase interlayer is formed between adjacent secondary crystals of the secondary crystal phase state; with the increase of the time of the low-temperature annealing treatment, the density of the secondary crystals is increased, the size of the secondary crystals is reduced, the thickness of the amorphous phase interlayer is reduced, and finally the secondary crystal metal material is obtained; the temperature range of the low-temperature annealing treatment is 150-300 ℃, and the time range of the low-temperature annealing treatment is 3-23 hours; the low-temperature annealing treatment leads a large amount of disordered amorphous state on the surface of the material micro-nano structure to be converted into secondary crystal phase which is arranged in a medium range order; at this time, the size range of the secondary crystals in the secondary crystal phase state is reduced to 0.3-nm-1 nm, and the density of the secondary crystals is increased to 1×10 4 Individual/μm 2 ～3×10 4 Individual/μm 2 The method comprises the steps of carrying out a first treatment on the surface of the The thickness of the amorphous phase interlayer between the adjacent secondary crystals is reduced to 0.2-nm-30 nm; the surface of the material is integrally formed by embedding a large number of secondary crystals and thin amorphous phases, the space distribution depth of the secondary crystal amorphous embedded phases is 5-10 mu m, and the surface of the material correspondingly presents a low-energy stable super-hydrophobic state independently.
The secondary crystal metal material combines ultra-fast laser ablation processing and SiO 2 After element doping and low-temperature annealing treatment, the surface of the material with high-density secondary crystal and amorphous mosaic distribution is endowed with an intrinsic thermodynamic low-energy characteristic, so that a durable, stable and efficient super-hydrophobic corrosion-resistant effect is macroscopically shown.
The invention further provides other preparation methods of the secondary crystal metal material, wherein the preparation methods comprise a magnetron sputtering method, a laser cladding method or a high-temperature high-pressure method.
The invention further provides application of the secondary crystal metal material in the corrosion resistance field, the super-hydrophobic field, the self-cleaning field, the biofouling prevention field, the ice coating resistance field or the water resistance reduction field.
In the paracrystalline metal material prepared by the invention, the paracrystalline phase has small size and high density, and forms a space mosaic distribution state with an amorphous phase; the material has extremely stable intrinsic low surface energy, and greatly prolongs the super-hydrophobic property of the material surface; moreover, the coating has high stable superhydrophobic effect and excellent anti-corrosion effect.
Further description of the embodiments is provided below.
Example 1
The invention provides a secondary crystal metal material and a preparation method thereof, wherein the secondary crystal metal material comprises the following steps:
s1, polishing the 6061 aluminum alloy surface by using sand paper, then ultrasonically cleaning the 6061 aluminum alloy surface by using deionized water, and drying by using nitrogen.
S2, placing a 6061 aluminum alloy sample on a precise three-dimensional moving platform, setting the ultrafast laser power to be 600 mW, the scanning speed to be 1 mm/S, and forming a supernano crystal and amorphous mosaic structure by focusing femtosecond laser ablation on the surface of the aluminum alloy;
s3, placing quartz glass on the high surface energy aluminum alloy obtained in the step S2, and then adopting the laser power and the processing speed parameters determined in the step S2 to carry out amorphous SiO 2 Doping to the surface of the material micro-nano structure as shown in figure 1;
s4, ultrasonically cleaning the surface of the 6061 aluminum alloy obtained in the step S3 by using deionized water for 30 minutes, and then carrying out annealing treatment on the surface of the 6061 aluminum alloy, wherein the annealing temperature is 200 ℃, and the annealing time is 3 hours; at this time, a large amount of amorphous phase on the surface of the material in the step S3 is converted into a secondary crystalline phase with a medium range ordered arrangement through the process of structure relaxation and stress release, and the single average size is 1.025 nm, so that the density is 2×10 3 Individual/μm 2 The method comprises the steps of carrying out a first treatment on the surface of the The average thickness of the amorphous interlayer between adjacent sub-crystalline phases is 22.84 nm, as shown in fig. 3-4 and fig. 7-8.
Subsequently, the secondary-crystallized low-surface-energy aluminum alloy sample prepared in the embodiment is soaked in the concentrated solutionAfter 35 days in a 3.5% NaCl solution, the surface of the material can still maintain good hydrophobic performance, as shown in FIG. 11. Moreover, as shown in FIG. 12, the electrochemical test results of the secondary-crystallized low-surface-energy aluminum alloy sample prepared in this example, in which the corrosion current of the raw aluminum alloy sample was 0.315. Mu.A, while the corrosion current of the secondary-crystallized secondary-metal material surface prepared in this example was less than 3.17X10 -4 Mu A is reduced by at least 3 orders of magnitude compared with the former, which shows that the surface of the paracrystalline metal material prepared by the embodiment also has excellent corrosion resistance.
Example 2
The invention provides a secondary crystal metal material and a preparation method thereof, wherein the secondary crystal metal material comprises the following steps:
s1, polishing the 6061 aluminum alloy surface by using sand paper, then ultrasonically cleaning the 6061 aluminum alloy surface by using deionized water, and drying by using nitrogen.
S2, placing a 6061 aluminum alloy sample on a precise three-dimensional moving platform, setting the ultrafast laser power to be 600 mW, setting the scanning speed to be 1 mm/S, and forming a high-energy surface consisting of supernano crystals and amorphous crystals by ablating the surface of the aluminum alloy through focusing femtosecond laser.
S3, placing quartz glass on the high surface energy aluminum alloy obtained in the step S2, and then adopting the laser power and the processing speed parameters determined in the step S2 to carry out amorphous SiO 2 Doped to the material micro-nano structure surface as shown in figure 2.
And S4, ultrasonically cleaning the surface of the 6061 aluminum alloy obtained in the step S3 for 30 minutes by using deionized water, and then carrying out annealing treatment on the surface of the 6061 aluminum alloy at the annealing temperature of 200 ℃ for 23 hours. At this time, a large amount of amorphous phase on the surface of the material in step S3 is converted into a secondary crystalline phase with a medium range ordered arrangement through the process of structure relaxation and stress release, and the average size is 0.68 nm, and the density is increased by 2.5×10 4 Individual/μm 2 The method comprises the steps of carrying out a first treatment on the surface of the The average thickness of the amorphous interlayer between adjacent sub-crystalline phases is reduced to 2.09 and nm, as shown in fig. 5-6 and 9-10.
Subsequently, the secondary-crystallized low-surface-energy aluminum alloy sample prepared in the embodiment is soaked in the concentrationAfter 100 days in 3.5% NaCl solution, the surface of the material can still maintain good hydrophobic performance, as shown in FIG. 11. Moreover, as shown in FIG. 12, the electrochemical test results of the secondary-crystallized low-surface-energy aluminum alloy sample prepared in this example, in which the corrosion current of the raw aluminum alloy sample was 0.315. Mu.A, while the corrosion current of the secondary-crystallized metal material surface prepared in this example was less than 2.24X10 -4 Mu A is reduced by at least 3 orders of magnitude compared with the former, which shows that the surface of the paracrystalline metal material prepared by the embodiment also has excellent corrosion resistance.
While embodiments of the present invention have been illustrated and described above, it will be appreciated that the above described embodiments are illustrative and should not be construed as limiting the invention. Variations, modifications, alternatives and variations of the above-described embodiments may be made by those of ordinary skill in the art within the scope of the present invention.
The above embodiments of the present invention do not limit the scope of the present invention. Any other corresponding changes and modifications made in accordance with the technical idea of the present invention shall be included in the scope of the claims of the present invention.
Claims (4)
1. A paracrystalline metal material, characterized in that the paracrystalline metal material comprises a metal material and a paracrystalline phase formed on the metal material; an amorphous interlayer is arranged between adjacent secondary crystals in the secondary crystal phase state; the secondary crystal phase and the amorphous phase interlayer are in space discretization mosaic distribution; the interior of each of the paracrystalline phases is defect-free; the size of the secondary crystal in the secondary crystal phase state ranges from 0.3nm to 1nm, and the density of the secondary crystal is 1 multiplied by 10 4 Individual/μm 2 ～3×10 4 Individual/μm 2 The method comprises the steps of carrying out a first treatment on the surface of the The thickness of the amorphous phase interlayer between the adjacent secondary crystals is 0.2 nm-30 nm; the depth of the space distribution of the paracrystalline amorphous mosaic phase is 5-10 mu m.
2. A method of producing the paracrystalline metal material as described in claim 1, characterized in that the method comprises the steps of:
s1, ablating the metal material by using ultrafast laser to generate a supernano crystalline phase and an amorphous phase on the metal material, and forming an initial micro-nano structure surface;
s2, irradiating again through ultrafast laser, doping a doping substance into the surface of the initial micro-nano structure, so that the ultra-nano crystal phase is crushed into the amorphous phase, and the surface of the micro-nano structure is obtained;
s3, carrying out low-temperature annealing treatment on the surface of the amorphous structure to form the secondary crystal phase state, wherein an amorphous phase interlayer is formed between adjacent secondary crystals in the secondary crystal phase state; the temperature range of the low-temperature annealing treatment is 150-300 ℃, and the time range of the low-temperature annealing treatment is 3-23 hours; as the time of the low-temperature annealing treatment increases, the density of the secondary crystals increases, the size of the secondary crystals decreases, and the thickness of the amorphous interlayer decreases, so as to obtain the secondary crystal metal material;
the metal material is aluminum alloy, and the supernanocrystalline component and the amorphous component are aluminum oxide; the pulse width of the ultrafast laser is 40fs, the central wavelength of the ultrafast laser is 800nm, and the pulse frequency of the ultrafast laser is 1kHz; the doping substance is SiO 2 、CO 2 A gas or an optically transparent substance.
3. The method for producing a secondary crystal metallic material as defined in claim 2, wherein in said S2, only a small amount of secondary crystals exist in an amorphous phase, the size of the secondary crystals in said secondary crystal phase ranges from 1nm to 2nm, and the density of the secondary crystals is 1X 10 3 Individual/μm 2 ～9×10 3 Individual/μm 2 The thickness of the amorphous phase interlayer between the adjacent secondary crystals is 1 nm-50 nm.
4. Use of the paracrystalline metal material according to claim 1, characterized in that the paracrystalline metal material is applied in the anti-corrosion field, the super-hydrophobic field, the self-cleaning field, the anti-biofouling field, the anti-icing field or the water-resistance-reducing field.
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