CN106282868A - The method that high/low temperature mixes non-equilibrium microstructure mutually is obtained in zircaloy - Google Patents
The method that high/low temperature mixes non-equilibrium microstructure mutually is obtained in zircaloy Download PDFInfo
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- CN106282868A CN106282868A CN201610819475.2A CN201610819475A CN106282868A CN 106282868 A CN106282868 A CN 106282868A CN 201610819475 A CN201610819475 A CN 201610819475A CN 106282868 A CN106282868 A CN 106282868A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F3/00—Changing the physical structure of non-ferrous metals or alloys by special physical methods, e.g. treatment with neutrons
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/16—Polishing
- C25F3/22—Polishing of heavy metals
- C25F3/26—Polishing of heavy metals of refractory metals
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Abstract
The invention provides the method that high/low temperature mixes non-equilibrium microstructure mutually that obtains in zircaloy: be processed by shot blasting to be placed on the station of pulse laser by two-phase Zr alloy surface, use argon as protective gas, with pulse laser beam, sample surfaces is processed.The main parameters ranges of this Laser Surface Treatment method: laser power 20 ~ 600W, energy density 3 ~ 50J/mm2, pulse width 2 ~ 6ms, defocusing amount 2 ~ 4mm, scanning speed 5 ~ 25mm/s, beam diameter 1mm.The present invention is after processing two-phase zircaloy, it is thus achieved that a kind of containing high-temperature-phase with the non-equilibrium line and staff control of low-temperature phase, may be conveniently used α → β phase change characteristics of Study For Zirconium alloy;This mixing microstructure includes original α phase, original β phase and α lath (being formed by newly-generated β phase in version);Microscopic structure under high temperature can be retained to room temperature by the present invention, it is easier to ground carries out α → β phase transformation of routine and characterizes zircaloy;Easy to operate, equipment is simple, economical and practical, technically reliable, steady quality.
Description
Technical field
The present invention provides the method that high/low temperature mixes non-equilibrium microstructure mutually that obtains in zircaloy, and the method is to utilize pulse
Two-phase Zirconium alloy material surface is processed by laser beam, forms the modified layer group with certain depth on Zirconium alloy material surface
Knit, belong to metal material process field.
Background technology
Zircaloy is with its relatively low thermal neutron absorption cross section, excellent decay resistance and good comprehensive mechanical property
Can, it is commonly used for the core structural material of water cooled nuclear reactor, such as fuel can, manometer tube, support etc..Along with nuclear reactor skill
The development of art, has higher requirement to the performance of zirconium alloy cladding material.
At present, zircaloy is carried out β phase quenching is an important step in its process of manufacture, and main purpose is to make conjunction
Gold element super saturated solid solution is in α phase, and this is for realizing the size to second phase particles, distribution etc. during following process
The control of feature, thus it is the most crucial to optimize performance.It is true that in carrying out a α → β → α transition process, zircaloy micro-
See tissue and the change of highly significant also can occur.β → α phase transformation has been done numerous studies by many researcheres, including cooldown rate, closes
The impact on β → α phase-change organization of gold composition and impurity element and the variant housing choice behavior etc. of β → α phase transition process;Such as Slattery
?J Less-Common MetOn deliver“The effect of cooling rate on the β/α transformation in the zirconium/2 at.% chromium/0.16 at.% iron alloy ”(1968,
16:91-101), as a example by Zr-2Cr-0.16Fe alloy, elaborate the impact that β → α is changed by rate of cooling.And Gey etc. existsJ NuclMater delivers“Study of the β→α variant selection for a zircaloy-4 rod heated to the β transus in presence or not of an axial tensile stress”(2004,
328:137-145), the variant to single-phase Zr-4 alloy β → α transition process selects shape for making correlational study.But, due to height
The restriction that temperature characterizes mutually, the research for α → β transition process is the most immature at present, still suffers from bigger dispute in some aspects,
Such as the growth pattern about β phase newly-generated in two-phase zircaloy.Daymond is published inActa Mater's“Texture inheritance and variant selection through an hcp–bcc–hcp phase transformation”(2010,58:4053-4066) show that the high temperature β phase of Zr-2.5Nb alloy is mainly at original grain
Internal forming core with grow up, and Sattari etc. existJ Nucl MaterOn deliver“Variant selection and transformation texture in zirconium alloy Excel”(2014,453:120-123) are with Zr-3.5Sn-
As a example by 0.8Mo-0.8Nb, elaborate high temperature β phase main in epitaxially grown mode at original β phase surrounding growth.Above dispute
The main cause existed is a lack of the accurate research of the microstructure to zircaloy α → β transition process.
Laser surface treating technology is to metal material surface by the laser beam projects of high-energy-density, and uses high speed to sweep
The mode retouched, makes material surface be brought rapidly up undergoing phase transition and even melt, and produces the thermograde of superelevation at material surface, thus
Rely on self cooling to matrix heat radiation, cause high rate of cooling, cause being heated of material inconsistent, diffusion of alloy elements
Uneven and then cause nonequilibrium phase transition, produce nonequilibrium mixing microstructure.Offer one is swashed by the present invention by pulse
Optical processing Zirconium alloy material, finally gives containing original α phase, original β phase and α lath (by newly-generated β phase in version
Become) high-temperature-phase that forms and the non-equilibrium line and staff control of low-temperature phase, in order to the sign of the microstructure of α → β transition process.
Summary of the invention
The invention provides the method that high/low temperature mixes non-equilibrium microstructure mutually that obtains in zircaloy, to realize by using
Zirconium alloy material surface is processed by pulse laser equipment, it is thus achieved that a kind of containing (do not change/ change) high-temperature-phase with low
The non-equilibrium line and staff control of temperature phase, may be conveniently used α → β phase change characteristics of Study For Zirconium alloy.This mixes microstructure bag
Include original α phase, original β phase and α lath (being formed by newly-generated β phase in version).By method provided by the present invention, can
So that the microscopic structure under high temperature is retained to room temperature, in order to more easily zircaloy to be carried out routine α → β phase transformation is carried out
Characterize.
For achieving the above object, the present invention provides following technical scheme:
First with linear cutting equipment by the sample of zircaloy along roll to, laterally, normal direction cut workpiece by certain size respectively.And
Select the silicon carbide paper of 400#, 800#, 1000#, 1500#, 2000# and 3000# model by sample polishing light successively, then exist
Carrying out electrobrightening in polishing fluid, polishing voltage is 20V, and polish temperature is-30~-20 DEG C, and polishing time is 40~60s.Electricity
Solve after polishing completes and workpiece is taken out rapidly, and respectively with clear water and washes of absolute alcohol surface of the work.Finally by surface of the work
Dry up, do not stay water stain vestige.Polishing fluid can be suitable liquid of the prior art;The present invention provides a kind of perchloric acid, methanol
With the polishing fluid of ethylene glycol monobutyl ether mixed liquor, its volume fraction is: the perchloric acid of 5% ~ 15%, the methanol of 65% ~ 85%, 10% ~
The ethylene glycol monobutyl ether of 25%.
By the sample clamping after surface cleaning processing on the fixture of adapted, put into the operating room of pulse laser equipment,
And in operating room, it is passed through protective gas;Such as argon, helium etc.;Starting impulse laser equipment, on-load voltage, to Zirconium alloy material
Surface carry out laser surface strengthening treatment.The main parameters ranges that pulsed laser surface hardening processes: laser power 20 ~
600W, energy density 3 ~ 50J/mm2, pulse width 2 ~ 6ms, defocusing amount 2 ~ 4mm, scanning speed 5 ~ 25mm/s, beam diameter is
1mm,;Take out the sample processed through laser reinforcing, check workpiece surface quality, suitably the surface machine of sample is added smooth.
Beneficial effects of the present invention: the high/low temperature that obtains in zircaloy provided by the present invention mixes non-equilibrium microstructure mutually
Method, the Zirconium alloy material surface after being processed by pulse laser surface is formed the modified layer tissue with certain depth, is changing
Property layer partial below (degree of depth is between 200um 900um) find containing original α phase, original β phase and α lath (by newly-generated β
Phase in version forms) high-temperature-phase that forms and the non-equilibrium line and staff control of low-temperature phase.Under room temperature, the existence of this line and staff control makes double
α → β phase transformation of phase zircaloy characterize become convenient effectively.Study For Zirconium alloy phase change feature provided by the present invention effective
Method, be research different parameters under to the performance variation law in Zr-2.5Nb surface laser processing procedure on the basis of formed
, test result shows, by method provided by the present invention, can obtain containing original α phase, original β phase and α lath (by newly
The β phase in version generated forms) high-temperature-phase that forms and the non-equilibrium line and staff control of low-temperature phase, two-phase zirconium is easy in the existence of this tissue
α → β phase transformation of alloy characterizes.The method also have easy to operate, equipment is simple, economical and practical, technically reliable, efficiency high, matter
The advantages such as amount is stable.
Accompanying drawing explanation
Fig. 1 be embodiment provide Zr alloy surface modified layer non-equilibrium line and staff control region ECC figure and not homophase it
Between orientation relationship figure.
Detailed description of the invention:
Below with reference to the drawings and specific embodiments, the present invention is described in detail.
The invention provides the method that high/low temperature mixes non-equilibrium microstructure mutually that obtains in zircaloy, it is characterised in that include
Following steps:
First with linear cutting equipment by the sample of Zirconium alloy material along roll to, laterally, normal direction cuts by technological requirement, it is thus achieved that one
The workpiece of sizing three-dimensional shape.And with silicon carbide paper by sample polishing light, select the most successively 400#, 800#, 1000#,
Sample is polished light by the silicon carbide paper of 1500# and 3000# model step by step, afterwards workpiece is carried out electrobrightening.Electrobrightening
After completing, workpiece is taken out rapidly, and respectively with clear water and washes of absolute alcohol surface of the work.Finally surface of the work is dried up, no
Stay water stain vestige.It is 20V that surface of the work processes the polishing voltage of electrobrightening used, and polish temperature be-30~-20 DEG C, polishes
Time is 40~60s.The present invention provides a kind of concrete electrolytic polishing liquid, perchloric acid, methanol and ethylene glycol monobutyl ether mix
Obtaining, its proportioning volume fraction is: the perchloric acid of 5% ~ 15%, the methanol of 65% ~ 85%, the ethylene glycol monobutyl ether of 10% ~ 25%.
By the sample workpiece clamping after surface cleaning processing on the fixture of adapted, put into the operating room of pulse laser equipment
In, and in operating room, it is passed through argon as protective gas;
Starting impulse laser equipment, on-load voltage, the surface of Zirconium alloy material workpiece is processed.Pulsed laser surface hardening
The main parameters ranges processed: laser power 20 ~ 600W, energy density 3 ~ 50J/mm2, pulse width 2 ~ 6ms, defocusing amount 2 ~
4mm, scanning speed 5 ~ 25mm/s, beam diameter is 1mm, in this parameter area, all can realize the object of the invention;
Finally take out sample, check workpiece surface quality, suitably the surface machine of sample is added smooth.By pulse laser surface
Nuclear power Zirconium alloy material surface of the work after reason forms the modified layer tissue with certain depth, modified layer partial below (away from
Surface of the work about 300um or deeper region, i.e. between the distance surface of the work 200um 900um degree of depth) find containing original
High-temperature-phase that α phase, original β phase and α lath (being formed by newly-generated β phase in version) form and the non-equilibrium mixing group of low-temperature phase
Knit.Further test discovery, at distance surface of the work 250um 550um depth bounds, the high-temperature-phase of formation and low-temperature phase
Non-equilibrium line and staff control is the most obvious.
The Zirconium alloy material workpiece of the present invention, when on-load voltage, start pulse laser equipment intensive treatment, workpiece surface
It is brought rapidly up undergoing phase transition and even melts, produce the thermograde of superelevation at material surface, thus rely on to matrix heat radiation certainly
Coldness of the body but, causes high rate of cooling, causes being heated of material inconsistent, and diffusion of alloy elements is uneven and then causes non-flat
Weighing apparatus phase transformation, produces nonequilibrium mixing microstructure, obtains high-temperature-phase of the present invention and the non-equilibrium line and staff control of low-temperature phase mixing.
Embodiment:
Choose the Zr-2.5Nb sample of a size of 15mm × 8mm × 3mm after line cutting, and select successively 400#, 800#, 1000#,
The silicon carbide paper of 1500# and 3000# model, by sample polishing light, carries out electrobrightening in polishing fluid, and polishing voltage is
20V, polish temperature is-30 DEG C, and polishing time is 30s.Workpiece is taken out rapidly after completing by electrobrightening, and respectively with clear water with
Washes of absolute alcohol surface of the work.Finally surface of the work is dried up, do not stay water stain vestige.Polishing fluid is 70% methanol+20% second two
Alcohol monobutyl ether+10% perchloric acid (volume ratio).
By the sample clamping after surface cleaning processing on special fixture, put into the work of the operating room of pulse laser equipment
On position, and in operating room, it is filled with argon that purity is 99.9% as protective gas.Starting impulse laser equipment, on-load voltage,
The surface of Zr-2.5Nb material is carried out pulsed laser surface hardening process.The major parameter model that pulsed laser surface hardening processes
Enclose: laser power 20 ~ 600W, energy density 3 ~ 50J/mm2, pulse width 5ms, defocusing amount 2mm, scanning speed 8mm/s, light beam
A diameter of 1mm, in this parameter area, all can realize the object of the invention;
Two-phase Zr-2.5Nb surface after utilizing method for surface hardening of the present invention to process after tested is formed has certain depth
Modified layer tissue, in modified layer partial below (away from surface of the work about 300um or deeper region), the present embodiment degree of depth is at 350um
Find high-temperature-phase and the low-temperature phase formed containing original α phase, original β phase and α lath (being formed by newly-generated β phase in version)
Non-equilibrium line and staff control.Under room temperature, the existence of this line and staff control makes α → β phase transformation sign of two-phase zircaloy become more
Easily and effectively.
Claims (7)
1. in zircaloy, obtain the method that high/low temperature mixes non-equilibrium microstructure mutually, it is characterised in that comprise the following steps:
(1) preparation of workpiece
First with linear cutting equipment by the sample of zircaloy along roll to, laterally, normal direction cut workpiece by the size of technological requirement,
Obtain the workpiece of three-dimensional shape;
(2) polishing of workpiece
By the workpiece smooth light of metallographic silicon carbide paper polishing, afterwards workpiece is carried out electrobrightening;Electrobrightening will after completing
Workpiece takes out, and respectively with clear water and washes of absolute alcohol surface of the work;Finally surface of the work is dried up, do not stay water stain vestige;
(3) clamping of workpiece
Clamping workpiece after abovementioned steps being processed is good, puts into the operating room of pulse laser equipment, and is filled with in operating room
Noble gas is as protective gas;
(4) pulse laser processing of workpiece
Starting impulse laser equipment, on-load voltage, the surface of Zirconium alloy material workpiece is carried out laser surface strengthening treatment;
(5) take out the workpiece that laser reinforcing processes, check workpiece surface quality;Formed at Zirconium alloy material surface of the work and have
The modified layer tissue of certain depth, below modified layer, is formed containing original α phase, original β phase and by newly-generated β
The high-temperature-phase of the α lath composition of phase in version and the non-equilibrium line and staff control of low-temperature phase mixing.
The method that acquisition high/low temperature mixes non-equilibrium microstructure mutually in zircaloy the most according to claim 1, its feature exists
In: in step (2), surface of the work processes electrolytic polishing liquid volume fraction used and is: the perchloric acid of 5% ~ 15%, 65% ~ 85%
Methanol, the ethylene glycol monobutyl ether of 10% ~ 25%.
The method that acquisition high/low temperature mixes non-equilibrium microstructure mutually in zircaloy the most according to claim 1 and 2, its feature
Being: in step (2), it is 20V that surface of the work processes the polishing voltage of electrobrightening used, and polish temperature is-30~-20
DEG C, polishing time is 40~60s.
The method that acquisition high/low temperature mixes non-equilibrium microstructure mutually in zircaloy the most according to claim 1, its feature exists
In: in step (3), behind the operating room that pulse laser equipment put into by workpiece, the inert protective gas being filled with is argon.
5. according to the arbitrary described method that acquisition high/low temperature mixes non-equilibrium microstructure mutually in zircaloy of claim 1,2,4,
It is characterized in that: in step (4), the main parameters ranges that pulsed laser surface hardening processes: laser power 20 ~ 600W, energy
Metric density 3 ~ 50J/mm2, pulse width 2 ~ 6ms, defocusing amount 2 ~ 4mm, scanning speed 5 ~ 25mm/s, beam diameter is 1mm.
6. according to the arbitrary described method that acquisition high/low temperature mixes non-equilibrium microstructure mutually in zircaloy of claim 1,2,4,
It is characterized in that: described workpiece is beaten step by step through the metallographic silicon carbide paper of 400#, 800#, 1000#, 1500#, 2000# and 3000#
Mill.
7. according to the arbitrary described method that acquisition high/low temperature mixes non-equilibrium microstructure mutually in zircaloy of claim 1,2,4,
It is characterized in that: described mixing non-equilibrium microstructure, formed between distance surface of the work 200um 900um.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108950618A (en) * | 2018-08-13 | 2018-12-07 | 重庆理工大学 | A method of obtaining high purity titanium superhard surfaces modified layer |
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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 |
CN105256264A (en) * | 2015-11-05 | 2016-01-20 | 重庆理工大学 | Preparation method for surface nanometer structure of zirconium alloy cladding material |
CN105442034A (en) * | 2016-01-14 | 2016-03-30 | 重庆理工大学 | Method for changing zirconium alloy surface texture |
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 |
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 |
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2016
- 2016-09-09 CN CN201610819475.2A patent/CN106282868B/en not_active Expired - Fee Related
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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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 |
CN105256264A (en) * | 2015-11-05 | 2016-01-20 | 重庆理工大学 | Preparation method for surface nanometer structure of zirconium alloy cladding material |
CN105442034A (en) * | 2016-01-14 | 2016-03-30 | 重庆理工大学 | Method for changing zirconium alloy surface texture |
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 |
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 |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108950618A (en) * | 2018-08-13 | 2018-12-07 | 重庆理工大学 | A method of obtaining high purity titanium superhard surfaces modified layer |
CN108950618B (en) * | 2018-08-13 | 2020-01-14 | 重庆理工大学 | Method for obtaining high-purity titanium superhard surface modified layer |
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