CN102586709A - Method for performing thermal treatment on zirconium alloy - Google Patents

Method for performing thermal treatment on zirconium alloy Download PDF

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CN102586709A
CN102586709A CN2012100998269A CN201210099826A CN102586709A CN 102586709 A CN102586709 A CN 102586709A CN 2012100998269 A CN2012100998269 A CN 2012100998269A CN 201210099826 A CN201210099826 A CN 201210099826A CN 102586709 A CN102586709 A CN 102586709A
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zirconium alloy
blank
sheet material
annealing
predeformation
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CN102586709B (en
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栾佰峰
柴林江
刘庆
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Chongqing University
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Chongqing University
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Abstract

The invention discloses a method for performing thermal treatment on zirconium alloy. The method comprises the following steps of: firstly, quenching a zirconium alloy blank to obtain a quenched blank; secondly, cooling the quenched blank to room temperature, and deforming the quenched blank until the deformation degree is 5 to 30 percent, namely pre-deforming the quenched blank at room temperature to obtain a pre-deformed blank; heating the pre-deformed blank to 350 to 700 DEG C, and annealing for 0.2 to 30 hours for the first time; thirdly, performing hot-rolling on the pre-deformed blank; fourthly, annealing repeatedly, and performing cold machining to obtain a plate; and finally, re-crystallizing and annealing the plate to obtain the finished product plate. Compared with the traditional method for performing thermal treatment on the zirconium alloy, the method for performing thermal zirconium alloy fulfils the aim of distributing second phase particles of the zirconium alloy in a dispersing way and improving the size uniformity of crystal particles of the zirconium alloy.

Description

A kind of heat treating method of zirconium alloy
Technical field
The present invention relates to the metal heat treatmet technical field, more particularly, relate to a kind of heat treating method of zirconium alloy.
Background technology
Zirconium alloy has that thermal neutron absorption cross section is little, thermal conductivity is high, good processability, and high temperature high voltage resistant water, water vapour corrosive characteristics, is widely used as the can material and the core structural material of water-cooled power reactor in the Nuclear power plants.Along with nuclear reactor technology towards improving fuel burnup, reactor thermo-efficiency and safe reliability; And reduction fuel cycle cost direction develops; To the demands for higher performance of zirconium alloy cladding material, comprise corrosion resistance nature, mechanical property and irradiation dimensional stability etc.And these performances of zirconium alloy and its microtexture (like the size of crystal grain, texture and second size, distribution, structure etc. of particle mutually) are closely related.A large amount of researchs show, when the second phase particle dispersion distributes, are beneficial to the raising of zirconium alloy corrosion resistance nature most, obtain evenly tiny, orientation crystal grain at random then to improving the zirconium alloy processing characteristics, weakening irradiation growth etc. and have the very effect of key.
Zirconium alloy can not directly use after casting blank, also need carry out a series of thermal treatment, so that zirconium alloy can have better properties.Existing zirconium alloy heat treating method is: the cold working → recrystallization annealing after blank → quenching → hot rolling → several times process annealing and the process annealing → finished product sheet material.And in fact, please refer to Fig. 3-1, and the metallograph that Fig. 3-1 distributes for the zirconium alloy sheet material second that adopts current technology to produce mutually, as can be seen from the figure, zirconium alloy is after handling through hot rolling, and the zonal arrangement situation has just appearred in the second phase particle; Simultaneously, please refer to Fig. 3-2, Fig. 3-2 produces the metallograph of the grain-size of zirconium alloy sheet material for adopting current technology, and we can see from figure, have occurred uneven grain structure in the zirconium alloy matrix, and have formed the bimodal texture of stable basal plane.The zonal arrangement of the second phase particle and uneven grain structure all can have a negative impact to the correlated performance of zirconium alloy.
Therefore, how a kind of heat treating method of zirconium alloy is provided,, becomes the technical problem that those skilled in the art need solution badly with disperse distribution that realizes the zirconium alloy second phase particle and the purpose that improves zirconium alloy even grain size property.
Summary of the invention
In view of this, the present invention provides a kind of heat treating method of zirconium alloy, with disperse distribution that realizes the zirconium alloy second phase particle and the purpose that improves zirconium alloy even grain size property.
For realizing above-mentioned purpose, the present invention provides following technical scheme:
A kind of heat treating method of zirconium alloy may further comprise the steps:
Step 01) blank with zirconium alloy carries out quench treatment, obtains the blank that quenches;
Step 02) with quenching blank cool to room temperature, carry out the deformation process that deflection is 5%-30%, obtain the predeformation blank;
Step 03) the predeformation blank is heated to 350 ℃-700 ℃ and carries out the anneal first time, annealing time is 0.2 hour-30 hours;
Step 04) the predeformation blank is carried out hot rolling and handle, obtain the sheet material blank;
Step 05) the sheet material blank is carried out the cold working after process annealing processing and the process annealing;
Step 06) repeated several times step 05),, obtains sheet material to the requirement of sheet material blank shape size Compound Machining;
Step 07) sheet material is carried out recrystallization annealing and handle, obtain finished product sheet material.
Preferably, above-mentioned zirconium alloy is specially the Zr-Sn-Nb alloy, and wherein, the weight percent of Sn element is between 0.3%-1.5%, and the weight percent of Nb element comprises alloying elements such as micro-Fe, Cr, Cu between 0.15%-1.25%, and surplus is Zr.
The invention provides a kind of heat treating method of zirconium alloy, the steps include: at first, blank is carried out quench treatment, obtain the blank that quenches; Afterwards, with quenching blank cool to room temperature, it is carried out the deformation process that deflection is 5%-30%, promptly room temperature predeformation is handled, and obtains the predeformation blank; Again the predeformation blank is heated to 350 ℃-650 ℃ and carries out the anneal first time, annealing time is 0.2 hour-30 hours; Then, the predeformation blank being carried out hot rolling handles; Repeat cold working after process annealing and the process annealing again, obtain sheet material; At last, sheet material is carried out recrystallization annealing handle, obtain finished product sheet material.
Compare with existing zirconium alloy heat treating method, zirconium alloy heat treating method provided by the invention has increased room temperature predeformation and the anneal two procedures first time between quench treatment and hot rolling processing.Room temperature predeformation has been introduced defectives such as a large amount of rooms and dislocation for the zirconium alloy matrix; Thereby make of according to qualifications the separate out effect reduction of the second phase particle at former β-Zr crystal boundary place; And tend to the high-energy fault location in matrix of separating out of more disperse, make the second phase particle of zirconium alloy be disperse and distribute.In addition; A large amount of defectives in the introducing matrix have also improved the nucleation rate and the coarsening rate of recrystallize nucleus greatly; Make the motivating force of recrystallize increase, and the Zener resistance of precipitated phase is constant basically, the average recrystallization crystal particle dimension that finally makes predeformation handle sample is merely several microns; Be far smaller than not predeformation processing sample, and the irregularity of grain shape is greatly improved also.Therefore, the room temperature predeformation of increase handle with anneal for the first time promoted zirconium alloy second mutually even, the disperse of particle separate out, refinement crystal grain, adjusted and eliminated the tissue defects of zirconium alloy crystal grain, improved the homogeneity of zirconium alloy grain-size.
By the above, after the heat treating method that the application of the invention provided is heat-treated zirconium alloy, realized the purpose that the zirconium alloy second phase particle dispersion is distributed and improve zirconium alloy even grain size property.
Description of drawings
In order to be illustrated more clearly in the embodiment of the invention or technical scheme of the prior art; To do to introduce simply to the accompanying drawing of required use in embodiment or the description of the Prior Art below; Obviously, the accompanying drawing in describing below only is some embodiments of the present invention, for those of ordinary skills; Under the prerequisite of not paying creative work, can also obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is the schema of zirconium alloy production technique in the prior art;
The schema of the zirconium alloy heat treating method that Fig. 2 provides for the embodiment of the invention;
Fig. 3-1 is the second phase particle distribution metallograph through the zirconium alloy of prior art production;
Fig. 3-2 is the grain-size metallograph through the zirconium alloy of prior art production;
Fig. 4-1 is for providing the second phase particle distribution metallograph of the zirconium alloy after heat treating method is handled through one of the embodiment of the invention;
Fig. 4-2 is for providing the grain-size metallograph of the zirconium alloy after heat treating method is handled through one of the embodiment of the invention;
Fig. 5-1 is for providing the second phase particle distribution metallograph of the zirconium alloy after heat treating method is handled through two of the embodiment of the invention;
Fig. 5-2 is for providing the grain-size metallograph of the zirconium alloy after heat treating method is handled through two of the embodiment of the invention.
Embodiment
To combine the accompanying drawing in the embodiment of the invention below, the technical scheme in the embodiment of the invention is carried out clear, intactly description, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills are not making the every other embodiment that is obtained under the creative work prerequisite, all belong to the scope of the present invention's protection.
The embodiment of the invention discloses a kind of heat treating method of zirconium alloy, with the purpose that realizes the zirconium alloy second phase particle dispersion being distributed and improving zirconium alloy even grain size property.
Through specific embodiment the present invention is done further detailed description below.
Embodiment one
Please refer to Fig. 2, the zirconium alloy heat treating method that the embodiment of the invention provided may further comprise the steps:
S10) the zirconium alloy blank is carried out quench treatment, obtain the blank that quenches;
S20) the quenching blank is cooled to room temperature, then it being carried out deflection is 20% deformation process, and promptly room temperature predeformation is handled, and obtains the predeformation blank;
S30) the predeformation blank is heated to 650 ℃ and carries out the anneal first time, annealing time is 30 hours;
S40) the predeformation blank to the process anneal first time carries out the hot rolling processing, obtains the sheet material blank;
S50) the sheet material blank is carried out process annealing, after the process annealing, carry out cold working;
S60) repeated several times step S50) physical dimension to the sheet material blank meets processing request, obtains sheet material;
S70) sheet material is carried out recrystallization annealing and handle, obtain finished product sheet material.
Compare with existing zirconium alloy complete processing, the zirconium alloy heat treating method that the embodiment of the invention provided has increased room temperature predeformation and the anneal two procedures first time between quench treatment and hot rolling processing.
After adopting heat treating method that the embodiment of the invention provided that zirconium alloy is handled,, obtain distribute the mutually grain-size metallograph (Fig. 4-2) of metallograph (Fig. 4-1) and zirconium alloy of second of zirconium alloy respectively again through the method for metallurgical analysis.Comparison diagram 3-1 and Fig. 4-1 can find that the second phase particle of zirconium alloy is tangible disperse distribution among Fig. 4-1, and this explanation heat treating method that the embodiment of the invention provided can make the second phase particle of zirconium alloy form the disperse distribution; Simultaneously; Comparison diagram 3-2 and Fig. 4-2 can find that the zirconium alloy crystal grain among Fig. 4-2 is tiny evenly, texture at random; This explanation heat treating method that the embodiment of the invention provided can refinement zirconium alloy crystal grain; The tissue defects of adjustment and elimination zirconium alloy crystal grain, the homogeneity of raising zirconium alloy grain-size.Can know that by above contrast the heat treating method of the zirconium alloy that the application of the invention embodiment is provided has been realized the purpose that the zirconium alloy second phase particle dispersion is distributed and improve zirconium alloy even grain size property.
Preferably; In the zirconium alloy heat treating method that the foregoing description provided, described zirconium alloy is specially the Zr-Sn-Nb alloy, wherein; The weight percent of Sn element is between 0.3%-1.5%; The weight percent of Nb element comprises alloying elements such as micro-Fe, Cr, Cu between 0.15%-1.25%, surplus is Zr.
Embodiment two
The zirconium alloy blank is through after the quench treatment, carries out deflection and is 20% room temperature predeformation and handle, and carries out the anneal first time afterwards, and annealing temperature is set at 650 ℃, and annealing time is 1.5 hours.Through after the above-mentioned processing, again zirconium alloy is carried out the cold working after hot rolling, 2 process annealing and the each process annealing, last recrystallization annealing is handled, and obtains finished product sheet material.Same, obtain Fig. 5-1 respectively through carrying out metallurgical analysis, second of the zirconium alloy metallograph that distributes mutually, and Fig. 5-2, the grain-size metallograph of zirconium alloy.It is contrasted with Fig. 3-1, Fig. 3-2 respectively, and significantly, after the method that adopts the embodiment of the invention two to be provided was handled zirconium alloy, the second phase particle dispersion of zirconium alloy ability distributed, and simultaneously, the grain-size of zirconium alloy is tiny, even.
Embodiment three
The zirconium alloy blank is through after the quench treatment, carries out deflection and is 10% room temperature predeformation and handle, and carries out the anneal first time afterwards, and annealing temperature is set at 450 ℃, and annealing time is 10 hours.Through after the above-mentioned processing, again zirconium alloy is carried out the cold working after hot rolling, 3 process annealing and the each process annealing, last recrystallization annealing is handled, and obtains finished product sheet material.Same, find that through carrying out metallurgical analysis after the employing method that the embodiment of the invention provided was handled zirconium alloy, the second phase particle dispersion of zirconium alloy ability distributed, simultaneously, the grain-size of zirconium alloy is tiny, even.
Embodiment four
The zirconium alloy blank is through after the quench treatment, carries out deflection and is 20% room temperature predeformation and handle, and carries out the anneal first time afterwards, and annealing temperature is set at 550 ℃, and annealing time is 5 hours.Through after the above-mentioned processing, again zirconium alloy is carried out the cold working after hot rolling, 3 process annealing and the each process annealing, last recrystallization annealing is handled, and obtains finished product sheet material.Same, find that through carrying out metallurgical analysis after the employing method that the embodiment of the invention provided was handled zirconium alloy, the second phase particle dispersion of zirconium alloy ability distributed, simultaneously, the grain-size of zirconium alloy is tiny, even.
Embodiment five
The zirconium alloy blank is through after the quench treatment, carries out deflection and is 5% room temperature predeformation and handle, and carries out the anneal first time afterwards, and annealing temperature is set at 350 ℃, and annealing time is 30 hours.Through after the above-mentioned processing, again zirconium alloy is carried out the cold working after hot rolling, 3 process annealing and the each process annealing, last recrystallization annealing is handled, and obtains finished product sheet material.Same, find that through carrying out metallurgical analysis after the employing method that the embodiment of the invention provided was handled zirconium alloy, the second phase particle dispersion of zirconium alloy ability distributed, simultaneously, the grain-size of zirconium alloy is tiny, even.
Embodiment six
The zirconium alloy blank is through after the quench treatment, carries out deflection and is 30% room temperature predeformation and handle, and carries out the anneal first time afterwards, and annealing temperature is set at 700 ℃, and annealing time is 0.2 hour.Through after the above-mentioned processing, again zirconium alloy is carried out the cold working after hot rolling, 3 process annealing and the each process annealing, last recrystallization annealing is handled, and obtains finished product sheet material.Same, find that through carrying out metallurgical analysis after the employing method that the embodiment of the invention provided was handled zirconium alloy, the second phase particle dispersion of zirconium alloy ability distributed, simultaneously, the grain-size of zirconium alloy is tiny, even.
Each embodiment adopts the mode of going forward one by one to describe in this specification sheets, and what each embodiment stressed all is and the difference of other embodiment that identical similar part is mutually referring to getting final product between each embodiment.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be conspicuous concerning those skilled in the art, and defined General Principle can realize under the situation that does not break away from the spirit or scope of the present invention in other embodiments among this paper.Therefore, the present invention will can not be restricted to these embodiment shown in this paper, but will meet and principle disclosed herein and features of novelty the wideest corresponding to scope.

Claims (2)

1. the heat treating method of a zirconium alloy is characterized in that, may further comprise the steps:
Step 01) blank with said zirconium alloy carries out quench treatment, obtains the blank that quenches;
Step 02) with said quenching blank cool to room temperature, carries out the deformation process that deflection is 5%-30%, obtain the predeformation blank;
Step 03) said predeformation blank is heated to 350 ℃-700 ℃ and carries out the anneal first time, annealing time is 0.2 hour-30 hours;
Step 04) said predeformation blank is carried out hot rolling and handle, obtain the sheet material blank;
Step 05) said sheet material blank is carried out the cold working after process annealing processing and the process annealing;
Step 06) repeated several times step 05),, obtains sheet material to the requirement of said sheet material blank shape size Compound Machining;
Step 07) said sheet material is carried out recrystallization annealing and handle, obtain finished product sheet material.
2. heat treating method according to claim 1; It is characterized in that said zirconium alloy is specially the Zr-Sn-Nb alloy, wherein; The weight percent of Sn element is between 0.3%-1.5%; The weight percent of Nb element comprises alloying elements such as micro-Fe, Cr, Cu between 0.15%-1.25%, surplus is Zr.
CN 201210099826 2012-04-05 2012-04-05 Method for performing thermal treatment on zirconium alloy Expired - Fee Related CN102586709B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105925846A (en) * 2016-06-24 2016-09-07 西部新锆核材料科技有限公司 Zr-Sn-Nb-Hf alloy bar and manufacture method thereof
CN113667914A (en) * 2021-08-09 2021-11-19 燕山大学 Method for preparing high-strength pure zirconium through cold deformation
CN113981347A (en) * 2021-09-29 2022-01-28 西安交通大学 High-strength-plasticity heterostructure zirconium alloy and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002105609A (en) * 2000-09-26 2002-04-10 Japan Science & Technology Corp High hydrogen storage alloy and its manufacturing method
CN1366089A (en) * 2001-01-19 2002-08-28 韩国原子力研究所 Method of manufacturing alloy pipe and sheet containing niobium and zirconium used for high burnup nuclear fuel
CN102172621A (en) * 2011-03-22 2011-09-07 重庆大学 Variable-orientation rolling method of zirconium alloy plate

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002105609A (en) * 2000-09-26 2002-04-10 Japan Science & Technology Corp High hydrogen storage alloy and its manufacturing method
CN1366089A (en) * 2001-01-19 2002-08-28 韩国原子力研究所 Method of manufacturing alloy pipe and sheet containing niobium and zirconium used for high burnup nuclear fuel
CN102172621A (en) * 2011-03-22 2011-09-07 重庆大学 Variable-orientation rolling method of zirconium alloy plate

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105925846A (en) * 2016-06-24 2016-09-07 西部新锆核材料科技有限公司 Zr-Sn-Nb-Hf alloy bar and manufacture method thereof
CN105925846B (en) * 2016-06-24 2018-02-23 西部新锆核材料科技有限公司 A kind of Zr Sn Nb Hf alloy bar materials and preparation method thereof
CN113667914A (en) * 2021-08-09 2021-11-19 燕山大学 Method for preparing high-strength pure zirconium through cold deformation
CN113667914B (en) * 2021-08-09 2022-04-19 燕山大学 Method for preparing high-strength pure zirconium through cold deformation
CN113981347A (en) * 2021-09-29 2022-01-28 西安交通大学 High-strength-plasticity heterostructure zirconium alloy and preparation method thereof

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