CN109706414A - A method of improving zircaloy corrosion resistance and surface hardness - Google Patents
A method of improving zircaloy corrosion resistance and surface hardness Download PDFInfo
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- CN109706414A CN109706414A CN201811617585.6A CN201811617585A CN109706414A CN 109706414 A CN109706414 A CN 109706414A CN 201811617585 A CN201811617585 A CN 201811617585A CN 109706414 A CN109706414 A CN 109706414A
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Abstract
The invention discloses a kind of raising zircaloy corrosion resistance and the method for surface hardness, by Zirconium alloy material surface cleaning processing it is good after clamp, and be completely immersed in the sink equipped with pure water, sink has quartzy form simultaneously face laser light-emitting window；Starting impulse laser, on-load voltage carry out shock peening processing to sample surfaces；The design parameter range of Laser Surface Treatment: laser energy 50-600mJ, wavelength 532nm, repetition rate 10Hz, pulse width 8nm, scanning speed 0.1-5mm/s, spot diameter 0.5-4mm；The sample handled through laser reinforcing is taken out after the completion；The method of the present invention generates compact oxidation layer in Zr alloy surface, and obtains ultrafine-grained's modified layer, and after laser treatment, there are biggish residual stress in matrix；The oxidation film of generation can effectively prevent the diffusion of oxonium ion, residual stress can stablize the tetragonal phase zirconium oxide in oxide layer, the corrosion resistance of zircaloy is improved, the surface hardness of zircaloy can be improved in ultrafine-grained's modified layer, so that zircaloy be made to have superior comprehensive performance.
Description
Technical field
The present invention relates to Zirconium alloy material fields.Specifically, being surface-treated the present invention relates to a kind of using pulse laser
The method for improving zircaloy corrosion resistance and surface hardness.
Background technique
Zircaloy is due to its low neutron absorption cross-section, good aqueous corrosion performance resistant to high temperatures, excellent mechanical behavior under high temperature
And the features such as anti-radiation performance, is widely used in nuclear reactor fuel canning material and structural material, referred to as " atom
The metal in epoch ".Extremely harsh, the zirconium as use environment of the zircaloy of fuel canning material and structural material in reactor
Alloy cladding remained under reactor operation operating condition there is a problem that it is many.Firstly, corruption can occur under high temperature water environment
On the one hand erosion, corrosion can generate hydrogen, zirconium alloy substrates, which absorb hydrogen, can occur hydrogen embrittlement, and hydrogen embrittlement and corrosion lead to shell thickness
Reduction will affect the mechanical performance of involucrum；On the other hand, the oxidation film for corroding generation, which is attached to involucrum surface, can reduce involucrum
Thermal conductivity, can also generate heat in corrosion process, will lead to the raising of fuel pellet temperature, influence the security performance of reactor.
Secondly, in reactor, since Flow vibration can cause to generate fretting wear between involucrum and grid spacer, fretting damage by
Gradually become one of the most important reason of fuel rod failure.Also there can be some impurity in the coolant of reactor, these objects
Constantly friction involucrum surface also results in involucrum failure.With nuclear reactor art towards improve burnup, lengthen the cycle of operation, mention
High thermal efficiency and the direction for reducing fuel cycle cost are developed, and propose higher want to the performance of zirconium alloy cladding material
The synthesis service performance asked, therefore how to improve zirconium alloy cladding has become the urgent need of industry.
To solve problems, on the one hand require product design and manufacture constantly using new construction, new material and new process；
On the other hand, surface modification engineering is another effective way for solving the problems, such as such, and surface engineering technology method is improving zirconium conjunction
The service performance of golden product may play a key effect in terms of reducing maintenance cost.It is modified applied to the surface of zircaloy at present
Method mainly has Zr alloy surface pre-oxidation film, differential arc oxidation, ion implanting, ion irradiation, pulsed electron beam processing, laser molten
It covers, is laser alloying, laser impact intensified etc., the main purpose of these methods is to generate one layer of pre-oxidation film in Zr alloy surface
Or change Zr alloy surface microstructure, to obtain excellent corrosion resistance and mechanical performance.
For reiforcing laser impact technology as a kind of important one of surface treatment, principle is the short arteries and veins of high power density
Impulse light action when target sample, protective layer by absorb laser energy quickly form a large amount of highdensity high temperature, high pressures etc. from
Daughter.Continue to act on laser, plasma steep temperature rise expansion, due to the restriction effect for the layer that suffers restraints, so that waiting
Gas ions form high impact wave and to the multi-direction propagation of material internal, when shock wave reaches critical speed, peak value pressure
Dynamic yield strength more than material is made material surface generate the tensile stress for being parallel to material surface and be parallel to shock wave by power
The compression in direction is to occur plastic deformation.After Reciprocity of Laser & Materials, shock wave also fades away, impact zone
The plastic deformation in domain by adjacent material reaction and obtain macroscopical residual compressive stress/strain, while material surface generate it is twin
The crystal defects such as crystalline substance simultaneously form ultrafine dislocation substructure.With shot-peening, rolling, it is interior squeeze etc. traditional surface strengthening technology
Compare, it is laser impact intensified have deeper residual compressive stress and residual stress thermal stability it is more preferable；With accurate repeatability,
The selectivity and past renaturation of strengthening region may be implemented using the feature of small light spot；The roughness of sample is influenced smaller；It can
Crack initiation is prevented, the generation of stress concentration phenomenon is reduced, reduces crack growth rate.
The guarantor of material surface in conventional laser processing method is eliminated with the laser shock peening method of water conservation target sample
Absorber coatings and protective gas environment are protected, treatment process and experimental provision are enormously simplified.Under the high temperature action of laser,
Zircaloy can react with the water as protective layer generates the pre-oxidation film with certain protective role, can be improved zirconium conjunction
The corrosion resistance of gold.In previous studies, zircaloy corrosion resistance is deteriorated mainly by the cubic phase oxidation in oxidation film
Caused by zirconium changes to monocline phase zircite, the opposite monoclinic phase transformation in four directions will lead to column crystal orientation fine and close in oxidation film
Loose equiax crystal transformation, and micro-crack is generated, more channels are provided for the diffusion of oxonium ion, is accelerated and is corroded and cause
Corrosion kinetics is transferred.And compression is to stablize the most important factor of tetragonal phase zirconium oxide, it is therefore, strong by laser-impact
Tetragonal phase zirconium oxide can be stablized in the oxidation reaction process of zircaloy by changing the application residual compressive stress in zirconium alloy substrates, be prevented
Only it changes to monoclinic phase, thus can be improved the corrosion resistance of zircaloy and make corrosion kinetics turnover occur when
Between postpone.The variation of surface microscopic tissue caused by laser impact intensified can effectively improve Zr alloy surface hardness, while laser
Shock peening can also change Zr alloy surface texture.
Summary of the invention
The purpose of the present invention is to provide a kind of raising zircaloy corrosion resistance and the methods of surface hardness, pass through high energy
Pulse laser strengthens Zirconium alloy material surface to obtain the Ultra-fine Grained of pre-oxidation film, surface high residual stress and certain depth
Zr alloy surface texture is organized and changed, and then improves the corrosion resistance and surface hardness of zirconium alloy cladding material, is extended anti-
Heap fuel cycle period is answered, nuclear reactor safety is improved.
In order to achieve the above object, the present invention adopts the following technical scheme:
A method of improving zircaloy corrosion resistance and surface hardness, comprising the following steps:
(1) preparation of sample workpiece
Sample workpiece surface is polished bright, reaches technique requirement；Pickling is carried out in proportioned pickling solution, when pickling
Long 10-20s uses clear water cleaning workpiece sample surfaces immediately after pickling, sample workpiece remained on surface acid solution is removed, then in acetone
It is cleaned by ultrasonic in reagent, cleans duration 5-15min, finally dry up surface, sample workpiece any surface finish after drying, without any
Residue；
(2) clamping of sample workpiece
By sample workpiece clamping of the surface clean after clean on fixture, it is mounted on the sample to match with pulse laser equipment
In sample platform, the height of sample stage is reduced, is completely immersed in sample workpiece in the sink equipped with pure water, and guarantees sample workpiece table
Face bubble-free；
(3) pulse laser processing
Starting impulse laser, on-load voltage carry out intensive treatment, the ginseng of pulsed laser surface hardening to Zr alloy surface
Number range: laser energy 50-600mJ, wavelength 532nm, repetition rate 10Hz, pulse width 8nm, scanning speed 0.1-5mm/
S, spot diameter 0.5-4mm；
(4) disassembly of sample workpiece
Sample stage is increased, the sample handled through laser reinforcing is taken out, sample survey surface quality dries up sample surfaces water
Stain；It analyzes after tested, Zr alloy surface texture changes, and Surface Creation pre-oxidizes film, and hardness and corrosion resistance have
It is improved.
Preferably, in step (1), the pickling solution, the volume ratio of component are as follows: the water of 25-35%, 25-35%'s
Nitric acid, the sulfuric acid of 25-35%, the hydrofluoric acid of 8-15%.
Preferably, sample workpiece is accommodated using four axis sample stages in step (2), sample workpiece is completely immersed in equipped with pure
In the sink of water, the side of sink face pulse laser light-emitting window has quartz glass light admission port, and laser is enable to be irradiated to
The surface of sample workpiece.
It is an advantage of the current invention that removing sample table in conventional method from using the sample of the pre- laser treatment of pure water conservation
The protection absorbed layer and the protective atmosphere environment in experimentation of face spraying, greatly simplifie the processing of Laser Surface Treatment
Process and experimental provision.During laser impact intensified, the water of high temp samples and surrounding reacts, and can eliminate zirconium conjunction
The Surface Texture that golden material generates when rolling, and can generate in Zr alloy surface with protective pre-oxidation film, the pre-oxidation
Film can effectively stop the diffusion of zircaloy oxonium ion in corrosion process, improve the corrosion resistance of zircaloy.It is rushed in laser
It hits after reinforcing, there are biggish residual stress in zirconium alloy substrates, these residual stress can stablize the four directions in oxidation film
Phase effectively prevents the opposite monoclinic phase in zircaloy four directions in oxidation process from changing, prevents fine and close column crystal oxidation film from turning
Become loose isometric crystal structure, the time retardation that the turnover of zircaloy corrosion dynamics occurs effectively improves the anti-of zircaloy
Corrosive nature.Sample surfaces after being strengthened by pulse laser form ultrafine-grained (UFG) microstructure, and the surface for being able to ascend zircaloy is hard
Degree.Finally, after the laser impact intensified processing of water conservation, the corrosion resistance and hardness of zircaloy are obviously improved, tool
There is more excellent comprehensive performance.
Detailed description of the invention
Fig. 1 is laser impact intensified schematic diagram.
1. 4. sample of sink, 5. sample stage that 2. laser beam focussing system 3. of pulse laser has quartz window
Fig. 2 is laser impact intensified rear and the not laser impact intensified zircaloy of comparative example the X ray diffracting spectrum of embodiment.
Fig. 3 is the corrosion of embodiment and comparative example zircaloy in 750 DEG C of water vapours (volume fraction 90%) after corrosion 5h
Increase weight curve.
Specific embodiment
Below with reference to the drawings and specific embodiments, the present invention is described in detail.
Comparative example 1
Choose the plate ZIRLO alloy sample having a size of 10mm × 8mm, first successively select 400#, 800#, 1000#,
The sand paper of 2000# and 3000# sample workpiece surface is polished it is bright, then volume ratio be+30% nitric acid of 10% hydrofluoric acid+
Pickling, pickling duration 15s are carried out in the pickling solution of+30% water of 30% sulfuric acid.Sample workpiece surface is washed with water after pickling immediately
20s washes away residual acid solution, is then cleaned by ultrasonic 10min in acetone, finally dries up sample workpiece surface, workpiece sample after drying
The noresidue of product surface.
Measurement result:
1. as shown in Fig. 2, the object in sample is mutually only zirconium base body, oxide-free by X-ray diffraction analysis.
2. being tested according to standard GB/T/T 4342-1991 the microhardness of sample surfaces, load 100g adds
Time 10s is carried, measuring hardness is 235HV.
3. as shown in figure 3, corroding sample weight gain 623.372mg/ after 5h in 750 DEG C of water vapours (volume fraction 90%)
dm2, corrosion kinetics turnover generation is in 12500s or so.
Embodiment 1
Choose the plate ZIRLO alloy sample having a size of 10mm × 8mm, first successively select 400#, 800#, 1000#,
The sand paper of 2000# and 3000# sample workpiece surface is polished it is bright, then volume ratio be+30% nitric acid of 10% hydrofluoric acid+
Pickling, pickling duration 15s are carried out in the pickling solution of+30% water of 30% sulfuric acid.Sample workpiece surface is washed with water after pickling immediately
20s washes away residual acid solution, is then cleaned by ultrasonic 10min in acetone, finally dries up sample workpiece surface, workpiece sample after drying
The noresidue of product surface.As shown in Figure 1, the sample workpiece after surface cleaning processing on fixture and is mounted on sample stage
On 5,5 height of sample stage is reduced, is completely immersed in sample workpiece in the sink 4 with quartz window equipped with pure water, and protect
Demonstrate,prove sample surfaces bubble-free.Starting impulse laser 1, so that laser passes through laser beam focussing system 2, and by having quartz window
The quartz window of the sink 4 of mouth is irradiated to the surface of sample workpiece, and on-load voltage carries out pulse to the surface of ZIRLO material and swashs
Optical surface intensive treatment.The major parameter of pulsed laser surface hardening: energy 250mJ, wavelength 532nm, pulse width 8nm, weight
Complex frequency 10Hz, spot diameter 1mm, scanning speed 0.286mm/s.
Measurement result:
1. as shown in Fig. 2, by X-ray diffraction analysis, tetragonal phase zirconium oxide in the oxidation film of laser impact intensified generation
Content be higher than monoclinic phase zirconium oxide.
2. according to standard GB/T/T 4342-1991 to the microhardness of the sample surfaces after laser surface strengthening treatment
It is tested, load 100g, load time 10s, measuring hardness is 254HV, and compared with comparative example 1, surface hardness is promoted
8.1%.
3. as shown in figure 3, corroding sample weight gain 528.322mg/ after 5h in 750 DEG C of water vapours (volume fraction 90%)
dm2, compared with comparative example 1, corrosion resistance improves about 15.25%；Corrosion kinetics turnover occurs in 15000s or so, with than
It is compared compared with example 1, about 2500s is delayed in corrosion kinetics turnover.
Embodiment 2
Choose the plate ZIRLO alloy sample having a size of 10mm × 8mm, first successively select 400#, 800#, 1000#,
The sand paper of 2000# and 3000# sample workpiece surface is polished it is bright, then volume ratio be+33% nitric acid of 8% hydrofluoric acid+
Pickling, pickling duration 18s are carried out in the pickling solution of+33% water of 26% sulfuric acid.Sample workpiece surface is washed with water after pickling immediately
20s washes away residual acid solution, is then cleaned by ultrasonic 12min in acetone, finally dries up sample workpiece surface, workpiece sample after drying
The noresidue of product surface.As shown in Figure 1, the sample workpiece after surface cleaning processing on fixture and is mounted on sample stage
On 5,5 height of sample stage is reduced, is completely immersed in sample workpiece in the sink 4 with quartz window equipped with pure water, and protect
Demonstrate,prove sample surfaces bubble-free.Starting impulse laser 1, so that laser passes through laser beam focussing system 2, and by having quartz window
The quartz window of the sink 4 of mouth is irradiated to the surface of sample workpiece, and on-load voltage carries out pulse to the surface of ZIRLO material and swashs
Optical surface intensive treatment.The major parameter of pulsed laser surface hardening: energy 350mJ, wavelength 532nm, pulse width 8nm, weight
Complex frequency 10Hz, spot diameter 1.5mm, scanning speed 0.143mm/s.
Measurement result:
1. as shown in Fig. 2, by X-ray diffraction analysis, tetragonal phase zirconium oxide in the oxidation film of laser impact intensified generation
Content be higher than monoclinic phase zirconium oxide.
2. according to standard GB/T/T 4342-1991 to the microhardness of the sample surfaces after laser surface strengthening treatment
It is tested, load 100g, load time 10s, measuring hardness is 294HV, and compared with comparative example 1, surface hardness is promoted about
25.1%.
3. as shown in figure 3, corroding sample weight gain 468.908mg/ after 5h in 750 DEG C of water vapours (volume fraction 90%)
dm2, compared with comparative example 1, corrosion resistance improves about 24.78%；Corrosion kinetics turnover occurs in 18000s or so, with than
It is compared compared with example 1, about 5500s is delayed in corrosion kinetics turnover.
Embodiment 3
Choose the plate ZIRLO alloy sample having a size of 10mm × 8mm, first successively select 400#, 800#, 1000#,
The sand paper of 2000# and 3000# sample workpiece surface is polished it is bright, then volume ratio be+28% nitric acid of 12% hydrofluoric acid+
Pickling, pickling duration 14s are carried out in the pickling solution of+28% water of 32% sulfuric acid.Sample workpiece surface is washed with water after pickling immediately
20s washes away residual acid solution, is then cleaned by ultrasonic 8min in acetone, finally dries up sample workpiece surface, sample workpiece after drying
Surface noresidue.As shown in Figure 1, the sample workpiece after surface cleaning processing on fixture and is mounted on sample stage 5
On, 5 height of sample stage is reduced, is completely immersed in sample workpiece in the sink 4 with quartz window equipped with pure water, and guarantee
Sample surfaces bubble-free.Starting impulse laser 1, so that laser passes through laser beam focussing system 2, and by having quartz window
The quartz window of sink 4 be irradiated to the surface of sample workpiece, on-load voltage carries out pulse laser to the surface of ZIRLO material
Surface Hardening Treatment.The major parameter of pulsed laser surface hardening: energy 450mJ, wavelength 532nm, pulse width 8nm are repeated
Frequency 10Hz, spot diameter 2.0mm, scanning speed 1.144mm/s.
Measurement result:
1. as shown in Fig. 2, by X-ray diffraction analysis, tetragonal phase zirconium oxide in the oxidation film of laser impact intensified generation
Content be higher than monoclinic phase zirconium oxide.
2. according to standard GB/T/T 4342-1991 to the microhardness of the sample surfaces after laser surface strengthening treatment
It is tested, load 100g, load time 10s, measuring hardness is 334HV, and compared with comparative example 1, surface hardness is promoted about
42.13%.
3. as shown in figure 3, corroding sample weight gain 405.944mg/ after 5h in 750 DEG C of water vapours (volume fraction 90%)
dm2, compared with comparative example 1, corrosion resistance improves about 34.88%；Corrosion kinetics turnover occur after 18000s, with than
It is compared compared with example 1, corrosion kinetics turnover is significantly delayed.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art are not departing from the principle of the present invention and objective
In the case where can make changes, modifications, alterations, and variations to the above described embodiments within the scope of the invention.
Claims (3)
1. a kind of method for improving zircaloy corrosion resistance and surface hardness, it is characterised in that: the following steps are included:
(1) preparation of sample workpiece
Sample workpiece surface is polished bright, reaches technique requirement；Pickling, pickling duration are carried out in proportioned pickling solution
10-20s uses clear water cleaning workpiece sample surfaces immediately after pickling, remove sample workpiece remained on surface acid solution, then tries in acetone
It is cleaned by ultrasonic in agent, cleans duration 5-15min, finally dry up surface, sample workpiece any surface finish after drying, without any residual
Stay object；
(2) clamping of sample workpiece
By sample workpiece clamping of the surface clean after clean on fixture, it is mounted on the sample stage to match with pulse laser equipment
On, reduce the height of sample stage, be completely immersed in sample workpiece in the sink equipped with pure water, and guarantee sample workpiece surface without
Bubble；
(3) pulse laser processing
Starting impulse laser, on-load voltage carry out intensive treatment, the parameter model of pulsed laser surface hardening to Zr alloy surface
It encloses: laser energy 50-600mJ, wavelength 532nm, repetition rate 10Hz, pulse width 8nm, scanning speed 0.1-5mm/s, light
Spot diameter 0.5-4mm；
(4) disassembly of sample workpiece
Sample stage is increased, the sample handled through laser reinforcing is taken out, it is water stain to dry up sample surfaces for sample survey surface quality；Through
Test analysis, Zr alloy surface texture change, and Surface Creation pre-oxidizes film, and hardness and corrosion resistance are mentioned
It is high.
2. a kind of method for improving zircaloy corrosion resistance and surface hardness according to claim 1, it is characterised in that:
In step (1), the pickling solution, the volume ratio of component are as follows: the water of 25-35%, the nitric acid of 25-35%, the sulphur of 25-35%
Acid, the hydrofluoric acid of 8-15%.
3. a kind of method for improving zircaloy corrosion resistance and surface hardness according to claim 1, it is characterised in that:
Sample workpiece is accommodated using sample stage in step (2), sample workpiece is completely immersed in the sink equipped with pure water, sink face
The side of pulse laser light-emitting window has quartz glass light admission port, and laser is enable to be irradiated to the surface of sample workpiece.
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| CN201811617585.6A CN109706414B (en) | 2018-12-28 | 2018-12-28 | Method for improving corrosion resistance and surface hardness of zirconium alloy |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112858150A (en) * | 2021-01-11 | 2021-05-28 | 南京理工大学 | Method for screening nuclear power reactor pressure vessel alloy irradiation-resistant material |
| 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 |
| CN115679234A (en) * | 2022-11-30 | 2023-02-03 | 昆明理工大学 | Method for improving wear resistance and corrosion resistance of zirconium-based amorphous alloy |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2018
- 2018-12-28 CN CN201811617585.6A patent/CN109706414B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112858150A (en) * | 2021-01-11 | 2021-05-28 | 南京理工大学 | Method for screening nuclear power reactor pressure vessel alloy irradiation-resistant material |
| 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 |
| CN115679234A (en) * | 2022-11-30 | 2023-02-03 | 昆明理工大学 | Method for improving wear resistance and corrosion resistance of zirconium-based amorphous alloy |
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