CN109706414B - Method for improving corrosion resistance and surface hardness of zirconium alloy - Google Patents
Method for improving corrosion resistance and surface hardness of zirconium alloy Download PDFInfo
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- CN109706414B CN109706414B CN201811617585.6A CN201811617585A CN109706414B CN 109706414 B CN109706414 B CN 109706414B CN 201811617585 A CN201811617585 A CN 201811617585A CN 109706414 B CN109706414 B CN 109706414B
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Abstract
The invention discloses a method for improving the corrosion resistance and surface hardness of zirconium alloy, which is characterized in that a zirconium alloy material is clamped after being cleaned and processed on the surface and is completely immersed in a water tank filled with purified water, and the water tank is provided with a quartz window and is opposite to a light outlet of a laser; starting a pulse laser, loading voltage, and performing impact strengthening treatment on the surface of the sample; specific parameter ranges for laser surface treatment: laser energy is 50-600mJ, wavelength is 532nm, repetition frequency is 10Hz, pulse width is 8nm, scanning speed is 0.1-5mm/s, and spot diameter is 0.5-4 mm; taking out the sample subjected to laser strengthening treatment after the completion; the method generates a compact oxide layer on the surface of the zirconium alloy, obtains an ultrafine crystal structure modified layer, and has larger residual stress in a matrix after laser treatment; the generated oxide film can effectively prevent oxygen ions from diffusing, the residual stress can stabilize tetragonal zirconia in the oxide layer, the corrosion resistance of the zirconium alloy is improved, and the superfine crystal structure modification layer can improve the surface hardness of the zirconium alloy, so that the zirconium alloy has more excellent comprehensive performance.
Description
Technical Field
The invention relates to the field of zirconium alloy materials. Specifically, the invention relates to a method for improving corrosion resistance and surface hardness of a zirconium alloy by using pulsed laser surface treatment.
Background
The zirconium alloy is widely applied to fuel cladding materials and structural materials of a nuclear reactor core due to the characteristics of low neutron absorption cross section, good high-temperature water corrosion resistance, excellent high-temperature mechanical property, excellent radiation resistance and the like, and is called as metal in the atomic era. The zirconium alloy used as the fuel cladding material and the structural material has extremely harsh use environment in the reactor, and the zirconium alloy cladding still has a plurality of problems under the operating condition of the reactor. Firstly, corrosion can occur in a high-temperature water environment, on one hand, hydrogen can be generated due to the corrosion, hydrogen embrittlement can occur due to the hydrogen absorbed by a zirconium alloy substrate, and the mechanical property of the cladding can be influenced due to the reduction of the thickness of the cladding caused by the hydrogen embrittlement and the corrosion; on the other hand, the oxide film generated by corrosion is attached to the surface of the cladding, so that the thermal conductivity of the cladding is reduced, heat is generated in the corrosion process, the temperature of the fuel pellets is increased, and the safety performance of the reactor is affected. Secondly, fretting damage has become one of the most important causes of fuel rod failure in reactors due to fretting between the cladding and spacer grids caused by flow-induced vibration. Impurities may also be present in the coolant of the reactor and these objects continually rub against the cladding surface, also leading to cladding failure. With the development of reactor technology towards improving fuel consumption, lengthening operation period, improving thermal efficiency and reducing fuel circulation cost, higher requirements are put forward on the performance of zirconium alloy cladding materials, so how to improve the comprehensive use performance of zirconium alloy cladding becomes an urgent need of the industry.
In order to solve such problems, on one hand, the product design and manufacture are required to continuously adopt new structures, new materials and new processes; on the other hand, surface modification engineering is another effective way to solve the problems, and a surface engineering technical method may play a key role in improving the service performance of zirconium alloy products and reducing the maintenance cost. The surface modification method mainly comprises the steps of preoxidation film on the surface of the zirconium alloy, micro-arc oxidation, ion injection, ion irradiation, pulsed electron beam treatment, laser cladding, laser alloying, laser shock strengthening and the like.
As one of important surface processes, the laser shock peening technology is based on the principle that when a short pulse laser with high power density is applied to a target sample, a protective layer rapidly forms a large amount of high-density high-temperature and high-pressure plasma by absorbing laser energy. The plasma rapidly rises and expands with the continuous action of the laser, and is limited by the restraint layer, so that the plasma forms high-strength shock waves and propagates in multiple directions to the interior of the material, and when the shock waves reach a critical speed, the peak pressure of the shock waves exceeds the dynamic yield strength of the material, so that the surface layer of the material generates tensile stress parallel to the surface of the material and compressive stress parallel to the direction of the shock waves, and plastic deformation is generated. After the interaction between the laser and the material is finished, the shock wave also disappears gradually, the plastic deformation of the impact area is reacted by the surrounding material to obtain macroscopic residual compressive stress/strain, and simultaneously, the surface of the material generates crystal defects such as twin crystals and the like and forms an extremely fine dislocation substructure. Compared with the traditional surface strengthening technologies such as shot blasting, rolling, internal extrusion and the like, the laser shock strengthening has deeper residual compressive stress and better thermal stability of the residual stress; the method has accurate repeatability, and can realize the selectivity and the repeatability of the reinforced area by utilizing the characteristics of the small light spot; the influence on the roughness of the sample is small; can prevent cracks from generating, reduce the occurrence of stress concentration phenomenon and reduce the crack propagation rate.
The laser shock peening method for protecting the target sample by water avoids a protective absorption coating on the surface of the material and a protective gas environment in the traditional laser processing method, and greatly simplifies the processing process and the experimental device. Under the high-temperature action of laser, the zirconium alloy can react with water serving as a protective layer to generate a pre-oxidation film with a certain protective effect, and the corrosion resistance of the zirconium alloy can be improved. In previous researches, the deterioration of the corrosion resistance of the zirconium alloy is mainly caused by the transformation from tetragonal phase zirconia in an oxide film to monoclinic phase zirconia, the transformation from the tetragonal phase to the monoclinic phase can cause the transformation from dense columnar crystal orientation to loose isometric crystal in the oxide film and generate microcracks, more channels are provided for the diffusion of oxygen ions, the corrosion is accelerated and the corrosion kinetics are turned. The compressive stress is the most important factor for stabilizing the tetragonal zirconia, so that the tetragonal zirconia can be stabilized in the oxidation reaction process of the zirconium alloy by applying residual compressive stress in the zirconium alloy matrix through laser shock strengthening to prevent the tetragonal zirconia from being transformed to a monoclinic phase, thereby improving the corrosion resistance of the zirconium alloy and delaying the time for generating corrosion kinetic transformation. The change of the surface microstructure caused by laser shock strengthening can effectively improve the surface hardness of the zirconium alloy, and simultaneously, the laser shock strengthening can also change the surface texture of the zirconium alloy.
Disclosure of Invention
The invention aims to provide a method for improving corrosion resistance and surface hardness of a zirconium alloy, which is characterized in that a pre-oxidation film, high surface residual stress and ultrafine grain structure with a certain depth are obtained by strengthening the surface of a zirconium alloy material through high-energy pulse laser, the surface texture of the zirconium alloy is changed, the corrosion resistance and the surface hardness of a zirconium alloy cladding material are further improved, the fuel circulation period of a reactor is prolonged, and the safety of the reactor is improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for improving corrosion resistance and surface hardness of zirconium alloy comprises the following steps:
(1) preparation of workpiece samples
Polishing the surface of a workpiece sample to be bright so as to meet the process requirement; pickling in a proportioned pickling solution for 10-20s, immediately cleaning the surface of a workpiece sample with clear water after pickling to remove residual acid liquor on the surface of the workpiece sample, then carrying out ultrasonic cleaning in an acetone reagent for 5-15min, finally drying the surface, and drying the surface of the workpiece sample to be smooth and clean without any residue;
(2) clamping of workpiece sample
Clamping a workpiece sample with a clean surface on a clamp, mounting the workpiece sample on a sample table matched with pulse laser equipment, and reducing the height of the sample table to ensure that the workpiece sample is completely immersed in a water tank filled with purified water and ensure that no bubbles exist on the surface of the workpiece sample;
(3) pulsed laser processing
Starting a pulse laser, loading voltage, and carrying out strengthening treatment on the surface of the zirconium alloy, wherein the parameter range of the surface strengthening of the pulse laser is as follows: laser energy is 50-600mJ, wavelength is 532nm, repetition frequency is 10Hz, pulse width is 8nm, scanning speed is 0.1-5mm/s, and spot diameter is 0.5-4 mm;
(4) disassembly of workpiece samples
Raising the sample table, taking out the sample subjected to laser strengthening treatment, inspecting the surface quality of the sample, and drying water stains on the surface of the sample; through test and analysis, the surface texture of the zirconium alloy is changed, a pre-oxidation film is generated on the surface, and the hardness and the corrosion resistance are improved.
Preferably, in the step (1), the pickling solution comprises the following components in volume ratio: 25-35% of water, 25-35% of nitric acid, 25-35% of sulfuric acid and 8-15% of hydrofluoric acid.
Preferably, in the step (2), the workpiece sample is held by using a four-axis sample stage, the workpiece sample is completely immersed in a water tank filled with purified water, and a quartz glass light through port is arranged on the side of the water tank, which is opposite to the light outlet port of the pulse laser, so that the laser can irradiate the surface of the workpiece sample.
The method has the advantages that the purified water is used for protecting the sample subjected to the pre-laser treatment, a protective absorption layer sprayed on the surface of the sample in the traditional method and a protective atmosphere environment in the experimental process are omitted, and the processing process and the experimental device of the laser surface treatment are greatly simplified. In the laser shock strengthening process, the high-temperature sample reacts with surrounding water, so that the surface texture generated in the rolling of the zirconium alloy material can be eliminated, a protective pre-oxidation film can be generated on the surface of the zirconium alloy, the pre-oxidation film can effectively prevent oxygen ions from diffusing in the corrosion process of the zirconium alloy, and the corrosion resistance of the zirconium alloy is improved. After laser shock strengthening, large residual stress exists in the zirconium alloy matrix, the residual stress can stabilize the tetragonal phase in the oxidation film, effectively prevent the tetragonal phase from being transformed to the monoclinic phase in the oxidation process of the zirconium alloy, prevent the compact columnar crystal oxidation film from being transformed into a loose isometric crystal structure, delay the time of the occurrence of corrosion kinetic transition of the zirconium alloy, and effectively improve the corrosion resistance of the zirconium alloy. The sample surface strengthened by the pulse laser forms an ultra-fine grain structure, and the surface hardness of the zirconium alloy can be improved. Finally, after the laser shock strengthening treatment of water protection, the corrosion resistance and hardness of the zirconium alloy are obviously improved, and the zirconium alloy has more excellent comprehensive performance.
Drawings
FIG. 1 is a schematic illustration of laser shock peening.
1. Pulse laser 2, laser beam focusing system 3, water tank 4 with quartz window, sample 5, sample stage
FIG. 2 is an X-ray diffraction pattern of a non-laser-shock-strengthened zirconium alloy of examples and comparative examples after laser shock strengthening.
FIG. 3 is a graph of the corrosion weight gain of the zirconium alloys of the examples and comparative examples after 5h of corrosion in water vapor (volume fraction 90%) at 750 ℃.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Comparative example 1
Selecting a plate-shaped ZIRLO alloy sample with the size of 10mm multiplied by 8mm, firstly sequentially selecting 400#, 800#, 1000#, 2000# and 3000# sandpaper to polish the surface of a workpiece sample to be bright, and then pickling in a pickling solution with the volume ratio of 10% hydrofluoric acid, 30% nitric acid, 30% sulfuric acid and 30% water for 15 s. And immediately washing the surface of the workpiece sample with water for 20s after acid washing, washing away residual acid liquor, then ultrasonically washing in acetone for 10min, finally drying the surface of the workpiece sample, wherein no residue is left on the surface of the workpiece sample after drying.
And (3) measuring results:
1. as shown in fig. 2, the phase in the sample was only a zirconium matrix and no oxide through X-ray diffraction analysis.
2. The microhardness of the surface of the sample is tested according to the national standard GB/T4342-1991, the load is 100g, the loading time is 10s, and the measured hardness is 235 HV.
3. As shown in FIG. 3, the weight gain of the sample was 623.372mg/dm after 5h of corrosion in water vapor (volume fraction 90%) at 750 ℃2The corrosion kinetics turn occurs around 12500 s.
Example 1
Selecting a plate-shaped ZIRLO alloy sample with the size of 10mm multiplied by 8mm, firstly sequentially selecting 400#, 800#, 1000#, 2000# and 3000# sandpaper to polish the surface of a workpiece sample to be bright, and then pickling in a pickling solution with the volume ratio of 10% hydrofluoric acid, 30% nitric acid, 30% sulfuric acid and 30% water for 15 s. And immediately washing the surface of the workpiece sample with water for 20s after acid washing, washing away residual acid liquor, then ultrasonically washing in acetone for 10min, finally drying the surface of the workpiece sample, wherein no residue is left on the surface of the workpiece sample after drying. As shown in FIG. 1, the workpiece sample after surface cleaning treatment is mounted on a fixture and mounted on a sample stage 5, and the height of the sample stage 5 is lowered to completely immerse the workpiece sample in a water tank 4 with a quartz window filled with purified water and ensure that the surface of the sample is free of bubbles. And starting the pulse laser 1, so that laser passes through the laser beam focusing system 2 and irradiates the surface of the workpiece sample through a quartz window of a water tank 4 with a quartz window, and loading voltage to perform pulse laser surface strengthening treatment on the surface of the ZIRLO material. Main parameters of pulsed laser surface strengthening: 250mJ of energy, 532nm of wavelength, 8nm of pulse width, 10Hz of repetition frequency, 1mm of spot diameter and 0.286mm/s of scanning speed.
And (3) measuring results:
1. as shown in fig. 2, the content of tetragonal zirconia in the oxide film produced by laser shock peening was higher than that of monoclinic zirconia by X-ray diffraction analysis.
2. The microhardness of the sample surface after the laser surface strengthening treatment is tested according to the national standard GB/T4342-1991, the load is 100g, the loading time is 10s, the measured hardness is 254HV, and compared with the comparative example 1, the surface hardness is improved by 8.1%.
3. As shown in FIG. 3, the weight gain of the sample was 528.322mg/dm after 5h of corrosion in water vapor (volume fraction 90%) at 750 ℃2The corrosion resistance is improved by about 15.25% compared with comparative example 1; the etch kinetics transition occurred at about 15000s, which was delayed by about 2500s compared to comparative example 1.
Example 2
Selecting a plate-shaped ZIRLO alloy sample with the size of 10mm multiplied by 8mm, firstly sequentially selecting 400#, 800#, 1000#, 2000# and 3000# sandpaper to polish the surface of a workpiece sample to be bright, and then carrying out acid pickling in acid pickling solution with the volume ratio of 8% hydrofluoric acid, 33% nitric acid, 26% sulfuric acid and 33% water, wherein the acid pickling time is 18 s. And immediately washing the surface of the workpiece sample with water for 20s after acid washing, washing away residual acid liquor, then ultrasonically washing in acetone for 12min, finally drying the surface of the workpiece sample, wherein no residue is left on the surface of the workpiece sample after drying. As shown in FIG. 1, the workpiece sample after surface cleaning treatment is mounted on a fixture and mounted on a sample stage 5, and the height of the sample stage 5 is lowered to completely immerse the workpiece sample in a water tank 4 with a quartz window filled with purified water and ensure that the surface of the sample is free of bubbles. And starting the pulse laser 1, so that laser passes through the laser beam focusing system 2 and irradiates the surface of the workpiece sample through a quartz window of a water tank 4 with a quartz window, and loading voltage to perform pulse laser surface strengthening treatment on the surface of the ZIRLO material. Main parameters of pulsed laser surface strengthening: 350mJ of energy, 532nm of wavelength, 8nm of pulse width, 10Hz of repetition frequency, 1.5mm of spot diameter and 0.143mm/s of scanning speed.
And (3) measuring results:
1. as shown in fig. 2, the content of tetragonal zirconia in the oxide film produced by laser shock peening was higher than that of monoclinic zirconia by X-ray diffraction analysis.
2. The microhardness of the sample surface after the laser surface strengthening treatment is tested according to the national standard GB/T4342-1991, the load is 100g, the loading time is 10s, the measured hardness is 294HV, and compared with the comparative example 1, the surface hardness is improved by about 25.1%.
3. As shown in FIG. 3, the weight gain of the sample was 468.908mg/dm after 5h of corrosion in water vapor (volume fraction 90%) at 750 ℃2The corrosion resistance is improved by about 24.78% compared with comparative example 1; the corrosion kinetics transition occurred around 18000s, which was delayed by about 5500s compared to comparative example 1.
Example 3
Selecting a plate-shaped ZIRLO alloy sample with the size of 10mm multiplied by 8mm, firstly sequentially selecting 400#, 800#, 1000#, 2000# and 3000# sandpaper to polish the surface of a workpiece sample to be bright, and then carrying out acid pickling in an acid pickling solution with the volume ratio of 12% hydrofluoric acid, 28% nitric acid, 32% sulfuric acid and 28% water, wherein the acid pickling time is 14 s. And immediately washing the surface of the workpiece sample with water for 20s after acid washing, washing away residual acid liquor, then ultrasonically washing in acetone for 8min, finally drying the surface of the workpiece sample, wherein no residue is left on the surface of the workpiece sample after drying. As shown in FIG. 1, the workpiece sample after surface cleaning treatment is mounted on a fixture and mounted on a sample stage 5, and the height of the sample stage 5 is lowered to completely immerse the workpiece sample in a water tank 4 with a quartz window filled with purified water and ensure that the surface of the sample is free of bubbles. And starting the pulse laser 1, so that laser passes through the laser beam focusing system 2 and irradiates the surface of the workpiece sample through a quartz window of a water tank 4 with a quartz window, and loading voltage to perform pulse laser surface strengthening treatment on the surface of the ZIRLO material. Main parameters of pulsed laser surface strengthening: energy of 450mJ, wavelength of 532nm, pulse width of 8nm, repetition frequency of 10Hz, spot diameter of 2.0mm, and scanning speed of 1.144 mm/s.
And (3) measuring results:
1. as shown in fig. 2, the content of tetragonal zirconia in the oxide film produced by laser shock peening was higher than that of monoclinic zirconia by X-ray diffraction analysis.
2. The microhardness of the sample surface after the laser surface strengthening treatment is tested according to the national standard GB/T4342-1991, the load is 100g, the loading time is 10s, the measured hardness is 334HV, and compared with the comparative example 1, the surface hardness is improved by about 42.13%.
3. As shown in FIG. 3, the weight gain of the sample was 405.944mg/dm after 5h of corrosion in water vapor (volume fraction 90%) at 750 ℃2The corrosion resistance is improved by about 34.88% compared with that of comparative example 1; the corrosion kinetics transition occurred after 18000s, which was greatly delayed compared to comparative example 1.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made in the above embodiments by those of ordinary skill in the art without departing from the principle and spirit of the present invention.
Claims (2)
1. A method for improving corrosion resistance and surface hardness of zirconium alloy is characterized in that: the method comprises the following steps:
(1) preparation of workpiece samples
Polishing the surface of a workpiece sample to be bright so as to meet the process requirement; pickling in a proportioned pickling solution for 10-20s, immediately cleaning the surface of a workpiece sample with clear water after pickling to remove residual acid liquor on the surface of the workpiece sample, then carrying out ultrasonic cleaning in an acetone reagent for 5-15min, finally drying the surface, and drying the surface of the workpiece sample to be smooth and clean without any residue;
(2) clamping of workpiece sample
Clamping a workpiece sample with a clean surface on a clamp, mounting the workpiece sample on a sample table matched with pulse laser equipment, and reducing the height of the sample table to ensure that the workpiece sample is completely immersed in a water tank filled with purified water and ensure that no bubbles exist on the surface of the workpiece sample;
(3) pulsed laser processing
Starting a pulse laser, loading voltage, and carrying out strengthening treatment on the surface of the zirconium alloy, wherein the parameter range of the surface strengthening of the pulse laser is as follows: laser energy is 50-600mJ, wavelength is 532nm, repetition frequency is 10Hz, pulse width is 8nm, scanning speed is 0.1-5mm/s, and spot diameter is 0.5-4 mm;
(4) disassembly of workpiece samples
Raising the sample table, taking out the sample subjected to laser strengthening treatment, inspecting the surface quality of the sample, and drying water stains on the surface of the sample; through test analysis, the surface texture of the zirconium alloy is changed, a pre-oxidation film is generated on the surface, and the hardness and the corrosion resistance are improved;
and (3) in the step (2), a sample table is used for holding a workpiece sample, the workpiece sample is completely immersed into a water tank filled with purified water, and a quartz glass light through opening is formed in one side of the water tank, which is opposite to a light outlet of the pulse laser, so that laser can irradiate the surface of the workpiece sample.
2. The method for improving the corrosion resistance and the surface hardness of the zirconium alloy according to claim 1, wherein the method comprises the following steps: in the step (1), the pickling solution comprises the following components in percentage by volume: 25-35% of water, 25-35% of nitric acid, 25-35% of sulfuric acid and 8-15% of hydrofluoric acid.
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| CN114509460A (en) * | 2022-02-18 | 2022-05-17 | 中国核动力研究设计院 | Pretreatment method for zirconium alloy scanning electron microscope sample before neutron irradiation |
| CN115679234B (en) * | 2022-11-30 | 2023-06-02 | 昆明理工大学 | Method for improving wear-resistant and corrosion-resistant properties of zirconium-based amorphous alloy |
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| US4279667A (en) * | 1978-12-22 | 1981-07-21 | General Electric Company | Zirconium alloys having an integral β-quenched corrosion-resistant surface region |
| CN105648516A (en) * | 2016-01-18 | 2016-06-08 | 重庆理工大学 | Method for obtaining ultra-hard surface modification layers of zirconium alloy |
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| US4279667A (en) * | 1978-12-22 | 1981-07-21 | General Electric Company | Zirconium alloys having an integral β-quenched corrosion-resistant surface region |
| CN105648516A (en) * | 2016-01-18 | 2016-06-08 | 重庆理工大学 | Method for obtaining ultra-hard surface modification layers of zirconium alloy |
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