CN105256264A - Preparation method for surface nanometer structure of zirconium alloy cladding material - Google Patents
Preparation method for surface nanometer structure of zirconium alloy cladding material Download PDFInfo
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- CN105256264A CN105256264A CN201510744928.5A CN201510744928A CN105256264A CN 105256264 A CN105256264 A CN 105256264A CN 201510744928 A CN201510744928 A CN 201510744928A CN 105256264 A CN105256264 A CN 105256264A
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- zirconium alloy
- cladding material
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- alloy cladding
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Abstract
The invention provides a preparation method for a surface nanometer structure of a zirconium alloy cladding material. The preparation method includes the following steps that after the surface of the zirconium alloy cladding material is cleaned, the zirconium alloy cladding material is put on a clamp and then put on a station of a vacuum chamber, the vacuum degree P of the vacuum chamber is smaller than 6*10-3 Pa, and argon is introduced to serve as the protective gas; pulse electronic beam equipment is started, high voltage is loaded, and the surface of the zirconium alloy is subjected to electronic beam impact strengthening treatment; and finally, the vacuum chamber is opened, and the surface quality of the workpiece is detected. According to the technical scheme, the size of the nanometer structure of a nanometer layer formed on the surface of the zirconium alloy is smaller than 100 nm, and the depth can reach more than 6 microns. As the surface of the zirconium alloy is subjected to the electronic beam surface strengthening treatment, the micro structure of the zirconium alloy is largely refined, the micro hardness and strength are greatly improved, and therefore the comprehensive mechanical performance of the zirconium alloy is improved. The preparation method for the surface nanometer structure of the zirconium alloy cladding material has the advantages of being convenient to operate, simple in equipment, economical, practicable, reliable in technique, high in efficiency, stable in quality and the like.
Description
technical field:
The present invention relates to a kind of preparation method of zirconium alloy cladding material surface nanostructure, belong to material surface process and technical field of modification; The method uses the method for pulsed electron beam to prepare nanostructured layers at zirconium alloy cladding material surface, and then the textura epidermoidea of refinement can material, improves its mechanical property such as microhardness and intensity.
background technology:
Zirconium alloy take zirconium as the non-ferrous alloy that matrix adds other elements and forms, it has good corrosion resisting property, moderate mechanical property and lower thermal neutron absorption cross section in the High Temperature High Pressure water and steam of 300 DEG C ~ 400 DEG C, good consistency is had to nuclear fuel, therefore, zirconium alloy is commonly used for the core structural material of water cooled nuclear reactor, as fuel sheath, penstock, support and duct pipe etc.Along with nuclear reactor technology is towards raising fuel burnup, reactor thermo-efficiency and safe reliability, and reduce fuel cycle cost future development, the performance of zirconium alloy cladding material is had higher requirement, comprises corrosion resistance nature, mechanical property and irradiation dimensional stability etc.And these performances of zirconium alloy and its microtexture (size, distribution, structure etc. as the size of crystal grain, texture and second phase particles) are closely related.Large quantifier elimination shows, obtain crystal grain that evenly tiny, orientation is random then to raising zirconium alloy processing characteristics, weaken irradiation growth etc. there is very crucial effect.Therefore how to improve the surface strength of zirconium alloy, the microstructure on refinement uniform alloy surface, puies forward heavy alloyed performance, and then greatly to extend its refulling cycle be vital.In use, it lost efficacy and often caused whole inefficacy because surface takes the lead in losing efficacy zirconium alloy cladding material, therefore needed to carry out surface Hardening Treatment to zirconium alloy cladding material.
Electron beam (ElectronBeam) process for treating surface is by the beam bombardment of high-energy-density to metallic surface, and adopts the mode of high-speed sweep, makes beam energy be distributed in metallic surface equably.E.B surface treatment technology is well applied in aluminum magnesium alloy and die steel, reaches and improves the performances such as it is heat-resisting, anti-corrosion, wear-resisting.Pulsed electron beam carries out quick refrigeration again after material rapid heating being made the surface of material reach temperature of fusion, improve nucleation rate inhibiting grain growth by kinetic control and can obtain nanostructure at material surface, make its reach ordinary method be difficult to realize surface modification effect.Many investigators positive application electron beam surface intensifying technology is to the research of various alloy and functional materials in recent years.But, the method of current employing electron beam surface strengthening carries out the detailed step of modification and main parameters ranges to zirconium alloy, and also there is not been reported, the present invention prepares method steps and the main parameters ranges of nanostructure by providing a kind of electron beam treatment zirconium alloy cladding material surface, economical and practical, efficiency is high and surface intensified technique of good performance.
summary of the invention:
The invention provides a kind of preparation method of zirconium alloy cladding material surface nanostructure, to realize obtaining uniform nanostructure by adopting electron beam equipment to carry out surface Hardening Treatment to zirconium alloy cladding material, and then the object of the mechanical property such as the microhardness of raising zirconium alloy cladding material surface and intensity.
For achieving the above object, the invention provides following technical scheme: a kind of preparation method of zirconium alloy cladding material surface nanostructure, is characterized in that comprising the following steps:
(1) preparation of workpiece
First polished by zirconium alloy sample bright with sand paper, then in polishing fluid, carry out electropolishing, polish temperature is-20 ~-30 DEG C, and polishing voltage is 20V; After polishing 20-30s, sample is taken out, clean sample surfaces successively with clear water and ethanol, finally dry up its surface;
(2) dress of workpiece is hung
Zirconium alloy sample after surface cleaning processing is contained on fixture, puts on the station of vacuum chamber, vacuumize, until the vacuum tightness P < 6 × 10 of vacuum chamber
-3pa, is then filled with rare gas element as shielding gas in vacuum chamber;
(3) electron beam treatment
Starting impulse electron beam equipment, loads high pressure, carries out electron beam bombardment intensive treatment to the surface of zirconium alloy cladding material.The main parameters ranges of pulsed electron beam surface Hardening Treatment: energy density 1-6J/cm
2, pulse width 1-10 μ s, pulse number 5-100 time;
(4) open vacuum chamber, take out the zirconium alloy cladding material through electron beam bombardment intensive treatment.
Further feature is: described polishing fluid, and the volume ratio of component is: the methyl alcohol of 60%-75%, the ethylene glycol monobutyl ether of 10%-25%, the perchloric acid of 8%-18%.
During polishing zirconium alloy sample, sample is polished bright with 400#, 800#, 1000#, 1500# and 3000# sand paper successively.
The nanostructure size being formed nanostructured layers by the zirconium alloy cladding material surface after pulsed electron beam surface treatment is less than 100nm, and the degree of depth reaches more than 6 μm.
In polishing process, polishing fluid is stirred, sample is constantly rocked.
After electron beam equipment vacuumizes, described inert protective gas is argon gas.
Beneficial effect of the present invention: the preparation method of zirconium alloy cladding material surface nanostructure provided by the present invention, formed on the basis studying the performance variation law in Zr702 surface Hardening Treatment process, test result shows, method for surface hardening provided by the invention meets the performance variation law of Zr702 material, can effectively improve the mechanical properties such as Zr702 microhardness and intensity, make its case depth and organize fine uniform more; Intensive treatment process operation of the present invention is convenient, and equipment is simple, and economical and practical, technically reliable, efficiency is high, steady quality, can realize good economic benefit.
accompanying drawing illustrates:
Fig. 1 provides the electron photomicrograph of the nanostructure of Zr alloy surface for embodiment
embodiment:
Below with reference to the drawings and specific embodiments, the present invention is described in detail.
The invention provides a kind of preparation method of zirconium alloy cladding material surface nanostructure, it is characterized in that comprising the steps:
First zirconium alloy sample is polished bright with sand paper, reach luminance brightness or the degree of cleaning of processing requirement; Specifically can, successively from the 400# that granularity is thicker, until the 3000# that granularity is thinner, namely sample be polished bright with 400#, 800#, 1000#, 1500# and 3000# sand paper successively; Then, in polishing fluid, carry out electropolishing, polish temperature is-20 ~-30 DEG C, and polishing voltage is 20V; Polishing fluid can be suitable liquid of the prior art; The invention provides the polishing fluid of a kind of methyl alcohol, ethylene glycol monobutyl ether and perchloric acid mixed solution, its volume ratio is: the methyl alcohol of 60%-75%, the ethylene glycol monobutyl ether of 10%-25%, the perchloric acid of 8%-18%.In polishing process, preferably polishing fluid is stirred, the present invention adopts magnet rotor slowly to rotate to stir polishing fluid, sample is also preferably constantly rocked, rapidly sample is taken out after polishing 20-30s, clean sample surfaces successively with clear water and ethanol, finally dry up its surface, the surface drying up rear sample does not have water stain vestige.The present invention is in polishing process, and magnet rotor has slowly rotated the effect of stirring and evenly mixing polishing fluid, can also take away sample and be thrown the scrap metal got off, make it be unlikely to concentrate near sample, avoid sample surfaces to adsorb, affect polishing effect.
Sample after surface cleaning processing is contained on fixture, puts on the station of vacuum chamber, vacuumize, until the vacuum tightness P < 6 × 10 of vacuum chamber
-3pa, is then filled with rare gas element as shielding gas, as argon gas, helium etc. in vacuum chamber;
Starting impulse electron beam equipment, loads high pressure, carries out electron beam bombardment intensive treatment to the surface of zirconium alloy cladding material.The main parameters ranges of pulsed electron beam surface Hardening Treatment: energy density 1-6J/cm
2, pulse width 1-10 μ s, pulse number 5-100 time, in this parameter area, all can realize the object of the invention;
Open vacuum chamber, take out the zirconium alloy cladding material through electron beam bombardment intensive treatment; Check workpiece surface quality, the nanostructure size being formed nanostructured layers by the zirconium alloy cladding material surface after pulsed electron beam surface treatment is less than 100nm, and the degree of depth reaches more than 6 μm.
Embodiment:
Choose the Zr702 sample of the 20mm × 30mm of preparation, first 400#, 800#, 1000#, 1500# and 3000# sand paper is selected successively to be polished light, then in the polishing fluid of 70% methyl alcohol+20% ethylene glycol monobutyl ether+10% perchloric acid (volume ratio), carry out electropolishing, polish temperature is-30 DEG C, and polishing voltage is 20V.In polishing process, magnet rotor slowly stirs, and constantly rocks sample simultaneously, is taken out by sample rapidly, clean sample surfaces successively with clear water and ethanol after 30s, and finally dry up its surface, the surface drying up rear sample does not have water stain vestige.Surface cleaning is dried up the sample after process to be contained on special fixture, put on the station of vacuum chamber, vacuumize, until the vacuum tightness 5.0 × 10 of vacuum chamber
-3pa, close vacuum valve, be then filled with in vacuum chamber purity be 99.9% argon gas as shielding gas until 3.0 × 10
4pa.Starting impulse electron beam equipment, loads high pressure, carries out electron beam bombardment intensive treatment to the surface of Zr702 material.The main parameters ranges of pulsed electron beam surface Hardening Treatment: energy density 3-6J/cm
2, pulse width 1.5 μ s, pulse number 20 times.
The nanostructure size utilizing the Zr702 of enhanced processing method process of the present invention surface to form nanostructured layers is after tested less than 100nm, and the degree of depth reaches more than 6 μm, and hardness can reach 260-280HV.
Claims (6)
1. a preparation method for zirconium alloy cladding material surface nanostructure, is characterized in that comprising the following steps:
(1) preparation of workpiece
First polished by zirconium alloy sample bright with sand paper, then in polishing fluid, carry out electropolishing, polish temperature is-20 ~-30 DEG C, and polishing voltage is 20V; After polishing 20-30s, sample is taken out, clean sample surfaces successively with clear water and ethanol, finally dry up its surface;
(2) dress of workpiece is hung
Zirconium alloy sample after surface cleaning processing is contained on fixture, puts on the station of vacuum chamber, vacuumize, until the vacuum tightness P < 6 × 10 of vacuum chamber
-3pa, is then filled with rare gas element as shielding gas in vacuum chamber;
(3) electron beam treatment
Starting impulse electron beam equipment, loads high pressure, carries out electron beam bombardment intensive treatment to the surface of zirconium alloy cladding material;
The main parameters ranges of pulsed electron beam surface Hardening Treatment: energy density 1-6J/cm
2, pulse width 1-10 μ s, pulse number 5-100 time;
(4) open vacuum chamber, take out the zirconium alloy cladding material through electron beam bombardment intensive treatment.
2. the preparation method of zirconium alloy cladding material surface nanostructure according to claim 1, is characterized in that: described polishing fluid, and the volume ratio of component is: the methyl alcohol of 60%-75%, the ethylene glycol monobutyl ether of 10%-25%, the perchloric acid of 8%-18%.
3. the preparation method of zirconium alloy cladding material surface nanostructure according to claim 1 and 2, is characterized in that: polished by sample bright with 400#, 800#, 1000#, 1500# and 3000# sand paper successively.
4. the preparation method of zirconium alloy cladding material surface nanostructure according to claim 1 and 2, it is characterized in that: the nanostructure size being formed nanostructured layers by the zirconium alloy cladding material surface after pulsed electron beam surface treatment is less than 100nm, and the degree of depth reaches more than 6 μm.
5. the preparation method of zirconium alloy cladding material surface nanostructure according to claim 1 and 2, is characterized in that: in polishing process, stirs polishing fluid, constantly rock sample.
6. the preparation method of zirconium alloy cladding material surface nanostructure according to claim 1 and 2, is characterized in that: after electron beam equipment vacuumizes, and described inert protective gas is argon gas.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105714225A (en) * | 2016-04-25 | 2016-06-29 | 重庆理工大学 | Method for obtaining high-density nanometer two crystals in zirconium materials for nuclear power |
| CN105951021A (en) * | 2016-07-06 | 2016-09-21 | 重庆理工大学 | Method for obtaining double-peak batten structure from zirconium alloy |
| CN106282868A (en) * | 2016-09-09 | 2017-01-04 | 重庆理工大学 | The method that high/low temperature mixes non-equilibrium microstructure mutually is obtained in zircaloy |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037784A (en) * | 2007-01-29 | 2007-09-19 | 西安交通大学 | Preparation technique of zirconium radical surface porous nano zirconium oxide biologically active coating |
| CN101886236A (en) * | 2010-06-23 | 2010-11-17 | 重庆理工大学 | Preparation method of surface nano structure of W-Cu alloy contact materials |
| CN101892361A (en) * | 2010-06-23 | 2010-11-24 | 重庆理工大学 | Method for preparing nano structure on copper chromium alloy surface |
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2015
- 2015-11-05 CN CN201510744928.5A patent/CN105256264A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037784A (en) * | 2007-01-29 | 2007-09-19 | 西安交通大学 | Preparation technique of zirconium radical surface porous nano zirconium oxide biologically active coating |
| CN101886236A (en) * | 2010-06-23 | 2010-11-17 | 重庆理工大学 | Preparation method of surface nano structure of W-Cu alloy contact materials |
| CN101892361A (en) * | 2010-06-23 | 2010-11-24 | 重庆理工大学 | Method for preparing nano structure on copper chromium alloy surface |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105714225A (en) * | 2016-04-25 | 2016-06-29 | 重庆理工大学 | Method for obtaining high-density nanometer two crystals in zirconium materials for nuclear power |
| CN105714225B (en) * | 2016-04-25 | 2018-01-16 | 重庆理工大学 | A kind of method in nuclear power with acquisition high density nano twin crystal in zirconium material |
| CN105951021A (en) * | 2016-07-06 | 2016-09-21 | 重庆理工大学 | Method for obtaining double-peak batten structure from zirconium alloy |
| CN106282868A (en) * | 2016-09-09 | 2017-01-04 | 重庆理工大学 | The method that high/low temperature mixes non-equilibrium microstructure mutually is obtained in zircaloy |
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