CN115679432A - Titanium alloy super-corrosion-resistant surface modification method - Google Patents
Titanium alloy super-corrosion-resistant surface modification method Download PDFInfo
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- CN115679432A CN115679432A CN202211378413.4A CN202211378413A CN115679432A CN 115679432 A CN115679432 A CN 115679432A CN 202211378413 A CN202211378413 A CN 202211378413A CN 115679432 A CN115679432 A CN 115679432A
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Abstract
The invention discloses a method for modifying a super-corrosion-resistant surface of a titanium alloy, which comprises the following specific steps: firstly, carrying out mechanical grinding and polishing treatment on the surface of a titanium alloy sample to remove mechanical processing traces and oil stains on the surface of the sample, then carrying out electrolytic polishing treatment on the surface of the titanium alloy sample to obtain a clean sample surface, and finally bombarding the surface of the titanium alloy sample by using electron beams to carry out surface modification treatment to obtain the surface of the titanium alloy sample with super corrosion resistance. According to the invention, the surface of the titanium alloy sample is subjected to surface modification treatment by a three-step method of mechanical grinding and polishing, electrolytic polishing and electron beam bombardment, so that the super-corrosion resistance of the surface of the titanium alloy sample is realized, and the reaction between the surface of the titanium alloy sample and an acid medium is prevented, so that the titanium alloy sample is protected from being corroded and damaged by the acid medium, and the prepared titanium alloy sample has good surface corrosion resistance and can be widely applied to titanium alloy corrosion protection.
Description
Technical Field
The invention relates to the technical field of material surface modification, in particular to a titanium alloy super-corrosion-resistant surface modification method.
Background
The titanium alloy has the characteristics of small density, high specific strength, good corrosion resistance, good biocompatibility and the like, so that the titanium alloy is widely applied to the fields of aerospace, ocean engineering, petrochemical industry, biomedical treatment and the like. In the service process, the surface of the titanium alloy sample is often contacted with other media, particularly acidic media, so that the surface of the sample is subjected to contact corrosion, the surface integrity of the titanium alloy sample is influenced, and even the service life is threatened.
The surface modification is one of important technical means in the field of titanium alloy corrosion protection. Currently, in surface modification, a mechanical polishing step is usually performed first, which can remove mechanical processing marks, oil stains and the like on the surface of a sample, and improve the basic morphology of the surface. And then, carrying out surface modification, wherein an electrolytic polishing surface treatment technology is adopted, but the technology only can improve the roughness of the surface and is difficult to realize effective titanium alloy surface corrosion protection, and more commonly used titanium alloy surface modification methods comprise ultrasonic surface rolling nanocrystallization, a surface laser remelting technology, an ultrasonic shot blasting surface modification technology and a laser impact surface modification technology. The technologies can realize corrosion protection of the surface of the titanium alloy, but have great technical difficulty and high process cost, and meanwhile, because the technology realizes surface modification by changing the microstructure of the surface layer of the titanium alloy, the microstructure difference between the core part and the surface layer of the titanium alloy sample is caused, and the difference between the mechanical properties of the core part and the surface layer of the titanium alloy sample is easy to be larger due to the difference between the microstructure of the core part and the microstructure of the surface layer of the titanium alloy sample, so that the properties of the core part and the surface layer of the titanium alloy sample are disordered, and the overall service capacity and the service life of the titanium alloy sample are finally influenced.
In conclusion, the research on the corrosion protection of the surface of the titanium alloy is very important, an advanced corrosion protection technology of the surface of the titanium alloy is developed, the corrosion resistance of the surface of the titanium alloy is improved, the surface performance of the titanium alloy is enhanced, the service life of the titanium alloy is prolonged, and the method has very important engineering application value and significance.
Disclosure of Invention
The invention provides a method for modifying a super-corrosion-resistant surface of a titanium alloy, which aims to solve the problems of high technical difficulty, high process cost and performance imbalance between a core part and a surface layer of a titanium alloy sample in the prior art.
In order to solve the technical problems, the invention adopts the technical scheme that: a method for modifying the super-anticorrosion surface of Ti alloy includes such steps as
Firstly, mechanically polishing and cleaning the surface of a titanium alloy sample: sequentially grinding the surfaces of the titanium alloy samples by adopting metallographic abrasive paper of different models, then mechanically polishing, and then ultrasonically cleaning and drying by adopting ethanol;
step two, electropolishing the surface of the titanium alloy sample: performing electrolytic polishing on the surface of the titanium alloy sample dried in the step one, then performing ultrasonic cleaning by using ethanol, and drying to obtain a clean surface of the titanium alloy sample;
step three, modifying the surface of a titanium alloy sample bombarded by electron beams: and E, performing electron beam bombardment on the surface of the clean titanium alloy sample obtained in the step II in a vacuum environment to obtain the surface modified titanium alloy sample surface.
Further, in the third step, in the bombardment of the electron beam, the titanium alloy sample with a clean surface obtained by the electrolytic polishing treatment in the second step is placed in a vacuum environment with the vacuum degree of 5 x 10 < -5 > Pa, the electron beam scans the bombarded area in an array manner, the incident direction of the electron beam and the surface of the sample form an included angle of 60 to 70 degrees, the acceleration voltage of the electron beam is 15 to 20kV, the scanning step length of the electron beam is 3 to 5 mu m, and the bombardment of the electron beam is finished to obtain the titanium alloy sample with a modified surface.
Further, when polishing is carried out in the first step, metallographic abrasive paper of 320#, 400#, 800#, 1000#, 2000# and 3000# is sequentially adopted to polish the surface of the titanium alloy sample, each type of abrasive paper is polished for 3-5 min, and the sample is rotated clockwise by 90 degrees when the type of the metallographic abrasive paper is changed and then is continuously polished; and during mechanical polishing, using Al2O3 turbid liquid as polishing liquid, and mechanically polishing on flannelette for 15-20 min.
Further, the electrolytic polishing solution in the second step is prepared by mixing a perchloric acid solution with a mass concentration of 71% and a glacial acetic acid solution with a mass concentration of 99.5% according to a volume ratio of 1: 15, wherein the voltage used in electrolytic polishing is 50-58V, the electrolytic polishing current is 0.8-1.2 mA, the polishing time is 10-15 s, and the temperature is-15 ℃.
Further, the temperature of the ultrasonic cleaning is 20 ℃, and the time of the ultrasonic cleaning is 20min.
Compared with the prior art, the invention has the following advantages:
1. the surface modification treatment of the titanium alloy sample surface by the three-step method of mechanical grinding and polishing, electrolytic polishing and electron beam bombardment is organically combined, so that the super-corrosion resistance of the titanium alloy sample surface to an acid medium is realized, the reaction of the titanium alloy sample surface and the acid medium is effectively prevented, and the titanium alloy sample is protected from being corroded and damaged by the acid medium. The experimental results show that after corrosion by acid medium, the modified area of the Ti-4Nb titanium alloy sample surface is 0.43 μm higher than the unmodified area, and the modified area of the Ti80 titanium alloy sample surface is 1.8 μm higher than the unmodified area.
2. As can be seen from FIG. 3, after being corroded by the acid medium, the surface modified area of the Ti-4Nb titanium alloy sample surface layer is a convex platform, and the area which is not subjected to surface modification is corroded to be a concave platform. As can be seen from fig. 5, the surface modified areas of the Ti80 titanium alloy sample surface after being corroded by the acid medium are convex plateaus, and the areas which are not subjected to surface modification are corroded to be concave plateaus. Therefore, the surface modification method for the titanium alloy sample can be used for modifying the surface of the titanium alloy sample, the microstructure of the surface layer of the sample cannot be changed, the balance of the core part and the surface layer structure and the performance of the titanium alloy sample can be maintained, and the service capacity of the titanium alloy sample is improved.
3. The mechanical grinding and polishing, the electrolytic polishing and the electron beam bombardment are all conventional technical means, so the technical difficulty is small, the process is simple, the process of organically combining the three for surface modification is controllable, and the method can be widely applied to corrosion protection of titanium alloy and other nonferrous metals. The prepared titanium alloy sample has good corrosion resistance to acid medium on the surface, and can be widely applied to corrosion protection of titanium alloy.
Drawings
FIG. 1 is an optical metallographic observation image of the surface of a Ti-4Nb titanium alloy sample subjected to surface modification in example 1 of the present invention, which is corroded by an acid medium.
FIG. 2 is an AFM observation of the surface of a Ti-4Nb titanium alloy sample of example 1 of the present invention after being corroded by an acid medium.
FIG. 3 is a graph showing the measurement of the difference in height of the surface of a Ti-4Nb titanium alloy sample of example 1 of the present invention after being corroded by an acid medium.
FIG. 4 is an optical metallographic observation image of the surface of a Ti80 titanium alloy sample subjected to surface modification in example 2 of the present invention, which is corroded by an acid medium.
FIG. 5 is an AFM observation of the surface of a Ti80 titanium alloy specimen in example 2 of the present invention after it has been corroded by an acid medium.
FIG. 6 is a graph showing the measurement of the difference in height of the surface of a Ti80 titanium alloy test piece corroded by an acid medium in example 2 of the present invention.
Detailed Description
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
firstly, mechanically polishing and cleaning the surface of a titanium alloy sample: the method comprises the steps of carrying out mechanical polishing treatment on the surface of a Ti-4Nb alloy sample, sequentially polishing the surface of the Ti-4Nb alloy sample by adopting metallographic abrasive paper of 320#, 400#, 800#, 1000#, 2000# and 3000#, polishing for 3min by each type of abrasive paper, continuously polishing after rotating the sample clockwise by 90 degrees when the type of the metallographic abrasive paper is changed, selecting Al2O3 turbid liquid as polishing liquid after polishing the surface of the titanium alloy sample by using the metallographic abrasive paper, and mechanically polishing on a flannel for 15min until the surface of the titanium alloy sample presents a mirror surface effect. And then ultrasonically cleaning the Ti-4Nb alloy sample subjected to mechanical polishing by using ethanol for 20min at the temperature of 20 ℃, and then drying. The method can remove machining traces and oil stains on the surface of the Ti-4Nb alloy sample.
Step two, electropolishing the surface of the titanium alloy sample: performing electrolytic polishing on the surface of the titanium alloy sample dried in the step one, then performing ultrasonic cleaning for 20min by using ethanol, and drying to obtain a clean and flat surface of the Ti-4Nb alloy sample; the electrolytic polishing solution adopted by the electrolytic polishing of the surface of the titanium alloy sample is prepared by mixing a perchloric acid solution with the mass concentration of 71% and a glacial acetic acid solution with the mass concentration of 99.5% according to the volume ratio of 1: 15, the voltage used in the electrolytic polishing is 52V, the electrolytic polishing current is 0.8mA, the polishing time is 10s, and the temperature is-15 ℃.
Step three, modifying the surface of a titanium alloy sample bombarded by electron beams: performing electron beam bombardment on the surface of the clean titanium alloy sample obtained in the step two in a vacuum environment to obtain the surface modified Ti-4Nb alloy sample surface; the environmental vacuum degree of the electron beam bombardment titanium alloy sample surface modification is 4 multiplied by 10 < -5 > Pa, the electron beam scans the bombarded area in an array manner, the included angle between the electron beam incidence direction and the sample surface is 70 degrees, the acceleration voltage of the electron beam is 20kV, the step length of the electron beam scanning is 3 mu m, and the modified Ti-4Nb alloy is obtained.
The modified Ti-4Nb alloy is subjected to an acid medium corrosion resistance test, and the test process and the test result are as follows:
the method comprises the following steps of testing the corrosion resistance of an acid-resistant medium on the surface of a Ti-4Nb alloy sample subjected to surface modification by using a titanium alloy metallographic corrosive solution, wherein the acid medium is the titanium alloy metallographic corrosive solution and is prepared by mixing a hydrofluoric acid solution with the relative molecular mass of 20.1%, a nitric acid solution with the relative molecular mass of 63.1% and purified water according to the volume ratio of 1: 3: 7, a soaking type corrosion mode is adopted in the test, and the corrosion time is 10s. And after the acid medium corrosion test is finished, carrying out ultrasonic cleaning on the surface of the Ti-4Nb alloy sample for 20min by using ethanol, and drying after cleaning. After the blow-drying, the surface appearance and the height difference measurement of the Ti-4Nb alloy sample subjected to surface modification in the embodiment after the corrosion in the acid medium are carried out by using an AxiovertA1 optical microscope and a Bruker RTESP-300 atomic force microscope.
As can be seen from FIG. 1, after the Ti-4Nb titanium alloy sample is corroded by the acid medium, a large optical contrast exists between the surface modified area and the area which is not subjected to surface modification on the surface layer of the Ti-4Nb titanium alloy sample, the bright area is the area which is not subjected to surface modification by the acid medium, and the black area is the area which is not subjected to surface modification and is corroded by the acid medium.
As can be seen from FIG. 2, after being corroded by the acid medium, the surface modified area of the Ti-4Nb titanium alloy sample surface layer is a convex platform, and the area which is not subjected to surface modification is corroded to be a concave platform.
It can be seen from fig. 3 that after corrosion by acid media, the surface modified regions of the Ti-4Nb titanium alloy sample surface were 0.43 μm higher than the regions that were not surface modified.
By combining and observing fig. 2 and fig. 3, the Ti-4Nb alloy sample in embodiment 1 of the present invention has a strong acid medium corrosion resistance after surface modification, which indicates that the surface modification treatment of the titanium alloy sample by the three-step method of "mechanical polishing + electropolishing + electron beam bombardment" can achieve the super-corrosion resistance of the titanium alloy sample surface and prevent the reaction between the titanium alloy sample surface and the acid medium, thereby protecting the titanium alloy sample from being corroded and damaged by the acid medium.
firstly, mechanically polishing and cleaning the surface of a titanium alloy sample: the method comprises the steps of carrying out mechanical polishing treatment on the surface of a Ti80 alloy sample, sequentially grinding the surface of the Ti80 alloy sample by adopting 320#, 400#, 800#, 1000#, 2000# and 3000# metallographic abrasive paper, grinding for 3min by each type of abrasive paper, continuously grinding after clockwise rotating the sample for 90 degrees when the type of the metallographic abrasive paper is changed, selecting Al2O3 turbid liquid as polishing liquid after finishing grinding the surface of the titanium alloy sample by the metallographic abrasive paper, and mechanically polishing on flannelette for 15min until the surface of the titanium alloy sample has a mirror surface effect. And then ultrasonically cleaning the Ti80 alloy sample subjected to mechanical polishing by using ethanol for 20min at the temperature of 20 ℃, and then drying. The step can remove machining traces and oil stains on the surface of the Ti80 alloy sample.
Step two, electropolishing the surface of the titanium alloy sample: performing electrolytic polishing on the surface of the titanium alloy sample dried in the step one, then performing ultrasonic cleaning for 20min by using ethanol, and drying to obtain a clean and flat surface of the Ti80 alloy sample; the electrolytic polishing solution adopted by the electrolytic polishing of the surface of the titanium alloy sample is prepared by mixing a perchloric acid solution with the mass concentration of 71% and a glacial acetic acid solution with the mass concentration of 99.5% according to the volume ratio of 1: 15, the voltage used in the electrolytic polishing is 55V, the electrolytic polishing current is 1.0mA, the polishing time is 10s, and the temperature is-15 ℃.
Step three, modifying the surface of a titanium alloy sample bombarded by electron beams: performing electron beam bombardment on the surface of the clean titanium alloy sample obtained in the step two in a vacuum environment to obtain the surface modified Ti80 alloy sample surface; the environmental vacuum degree of the modification of the surface of the titanium alloy sample bombarded by the electron beams is 5 multiplied by 10 < -5 > Pa, the electron beams scan the bombarded area in an array manner, the included angle between the incident direction of the electron beams and the surface of the sample is 70 degrees, the accelerating voltage of the electron beams is 20kV, and the step length of the electron beam scanning is 3 mu m, so that the modified Ti80 alloy is obtained.
The modified Ti80 alloy is subjected to an acid medium corrosion resistance test, and the test process and the test result are as follows:
and carrying out acid-medium corrosion resistance test on the surface of the Ti80 alloy sample subjected to surface modification by using a titanium alloy metallographic corrosive solution, wherein the acid medium is the titanium alloy metallographic corrosive solution and is prepared by mixing a hydrofluoric acid solution with the relative molecular mass of 20.1%, a nitric acid solution with the relative molecular mass of 63.1% and purified water according to the volume ratio of 1: 3: 7, soaking type corrosion is adopted in the test, and the corrosion time is 15s. And after the acid medium corrosion test is finished, ultrasonically cleaning the surface of the Ti80 alloy sample for 20min by using ethanol, and drying after cleaning. After the drying, the surface appearance of the Ti80 alloy sample subjected to surface modification in the embodiment after corrosion in an acid medium is observed and the height difference is measured by using an AxiovertA1 optical microscope and a Bruker RTESP-300 atomic force microscope.
As can be seen from FIG. 4, after the Ti80 titanium alloy sample is corroded by the acid medium, a large optical contrast exists between the surface modified area and the non-surface modified area of the surface layer of the Ti80 titanium alloy sample, the bright area is the non-corroded area subjected to the surface modification of the invention, and the black area is the corroded area by the acid medium not subjected to the surface modification.
As can be seen from fig. 5, the surface modified areas of the Ti80 titanium alloy sample surface after being corroded by the acid medium are convex plateaus, and the areas which are not subjected to surface modification are corroded to be concave plateaus.
As can be seen from FIG. 6, the surface-modified area of the Ti80 titanium alloy sample surface layer after etching by the acid medium was 1.8 μm higher than the area without surface modification.
By combining and observing fig. 5 and fig. 6, the Ti80 alloy sample in embodiment 2 of the present invention has a strong acid medium corrosion resistance after surface modification, which indicates that the surface modification treatment of the titanium alloy sample by the three-step method of "mechanical polishing + electropolishing + electron beam bombardment" can achieve the super-corrosion resistance of the titanium alloy sample surface, prevent the reaction between the titanium alloy sample surface and the acid medium, and thus protect the titanium alloy sample from being corroded and damaged by the acid medium.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modifications, alterations and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (5)
1. A method for modifying a super corrosion-resistant surface of a titanium alloy is characterized by comprising the following steps:
firstly, mechanically polishing and cleaning the surface of a titanium alloy sample: sequentially grinding the surfaces of the titanium alloy samples by adopting metallographic abrasive paper of different types, then mechanically polishing, and then ultrasonically cleaning and drying by adopting ethanol;
step two, electropolishing the surface of the titanium alloy sample: performing electrolytic polishing on the surface of the titanium alloy sample dried in the step one, then performing ultrasonic cleaning by using ethanol, and drying to obtain a clean surface of the titanium alloy sample;
step three, modifying the surface of a titanium alloy sample bombarded by electron beams: and E, performing electron beam bombardment on the surface of the clean titanium alloy sample obtained in the step II in a vacuum environment to obtain the surface modified titanium alloy sample surface.
2. The method for modifying the super corrosion-resistant surface of the titanium alloy according to claim 1, wherein: in the third step, electron beam bombardment is carried out, and the titanium alloy sample with clean surface obtained by the electrolytic polishing treatment in the second step is placed in a vacuum degree of 5 multiplied by 10 -5 In a Pa vacuum environment, electron beams scan a bombarded area in an array manner, the included angle between the incident direction of the electron beams and the surface of a sample is 60-70 degrees, the accelerating voltage of the electron beams is 15-20 kV, the step length of the electron beam scanning is 3-5 mu m, and the electron beam bombardment is finished to obtain the surface modificationAnd (3) a titanium alloy sample.
3. The method for modifying the super corrosion-resistant surface of the titanium alloy according to claim 2, wherein: when polishing is carried out in the first step, the surfaces of the titanium alloy samples are sequentially polished by adopting 320#, 400#, 800#, 1000#, 2000# and 3000#, each type of sand paper is polished for 3-5 min, and the samples are continuously polished after being rotated by 90 degrees clockwise when the types of the metallographic sand paper are changed; during the mechanical polishing, al is used 2 O 3 Taking the suspension as polishing solution, and mechanically polishing on the flannelette for 15-20 min.
4. The method of claim 3, wherein the titanium alloy is subjected to the modification of the super-corrosion-resistant surface, and the method comprises the following steps: and step two, the electrolytic polishing solution is prepared by mixing a perchloric acid solution with the mass concentration of 71% and a glacial acetic acid solution with the mass concentration of 99.5% according to the volume ratio of 1: 15, the voltage used during electrolytic polishing is 50-58V, the electrolytic polishing current is 0.8-1.2 mA, the polishing time is 10-15 s, and the temperature is-15 ℃.
5. The method of modifying a superarrosive surface of a titanium alloy according to any one of claims 1 to 4, wherein: the temperature of ultrasonic cleaning is 20 ℃, and the time of ultrasonic cleaning is 20min.
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