CN102586709B - Method for performing thermal treatment on zirconium alloy - Google Patents
Method for performing thermal treatment on zirconium alloy Download PDFInfo
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- CN102586709B CN102586709B CN 201210099826 CN201210099826A CN102586709B CN 102586709 B CN102586709 B CN 102586709B CN 201210099826 CN201210099826 CN 201210099826 CN 201210099826 A CN201210099826 A CN 201210099826A CN 102586709 B CN102586709 B CN 102586709B
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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
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 the characteristics of high temperature high voltage resistant water, water vapour corrosion, is widely used as 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 (as the size of size, texture and the second phase particle of crystal grain, distribution, structure etc.) are closely related.A large amount of studies show that, when the second phase particle dispersion distributes, is beneficial to the raising of zirconium alloy corrosion resistance nature most, obtains evenly tiny, orientation crystal grain at random then to improving the zirconium alloy processing characteristics, weakening irradiation growth etc. and have very crucial effect.
Zirconium alloy can not directly use after casting blank, also needs to 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 mutually for the zirconium alloy sheet material second that adopts current technology to produce, 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 inhomogeneous 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 inhomogeneous grain structure all can have a negative impact to the correlated performance of zirconium alloy.
Therefore, how to provide a kind of heat treating method of zirconium alloy, with the disperse distribution that realizes the zirconium alloy second phase particle and the purpose that improves the zirconium alloy even grain size, become the technical problem that those skilled in the art need solution badly.
Summary of the invention
In view of this, the invention provides a kind of heat treating method of zirconium alloy, with the disperse distribution that realizes the zirconium alloy second phase particle and the purpose that improves the zirconium alloy even grain size.
For achieving the above object, the 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 cold working after process annealing processing and the process annealing;
Step 06) repeated several times step 05), to the requirement of sheet material blank shape size Compound Machining, obtains sheet material;
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%, namely room temperature predeformation is handled, and obtains the predeformation blank; The predeformation blank is heated to 350 ℃-650 ℃ again 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 the second phase particle in the effect of separating out the according to qualifications reduction 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 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 substantially, finally make predeformation handle the average recrystallization crystal particle dimension of sample only for 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 and for the first time anneal 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 provides is heat-treated zirconium alloy, realized the purpose that the zirconium alloy second phase particle dispersion is distributed and improve the zirconium alloy even grain size.
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, apparently, 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;
The second phase particle distribution metallograph of the zirconium alloy after handling through the embodiment of the invention one heat treating method that provides is provided Fig. 4-1;
The grain-size metallograph of the zirconium alloy after handling through the embodiment of the invention one heat treating method that provides is provided Fig. 4-2;
The second phase particle distribution metallograph of the zirconium alloy after handling through the embodiment of the invention two heat treating method that provides is provided Fig. 5-1;
The grain-size metallograph of the zirconium alloy after handling through the embodiment of the invention two heat treating method that provides is provided Fig. 5-2.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the invention, the technical scheme in the embodiment of the invention is clearly and completely described, 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 belong to the scope of protection of the invention not making the every other embodiment that obtains under the creative work prerequisite.
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 the zirconium alloy even grain size.
Below by specific embodiment the present invention is described in further detail.
Embodiment one
Please refer to Fig. 2, the zirconium alloy heat treating method that the embodiment of the invention provides 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 namely 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 provides has increased room temperature predeformation and the anneal two procedures first time between quench treatment and hot rolling processing.
After the heat treating method that adopts the embodiment of the invention to provide is handled zirconium alloy, again by the method for metallurgical analysis, obtain distribute the mutually grain-size metallograph (Fig. 4-2) of metallograph (Fig. 4-1) and zirconium alloy of second of zirconium alloy respectively.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 heat treating method that this explanation embodiment of the invention provides 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 heat treating method of providing of explanation embodiment of the invention can refinement zirconium alloy crystal grain, adjust and eliminate the tissue defects of zirconium alloy crystal grain, improve the homogeneity of zirconium alloy grain-size.By above contrast as can be known, the heat treating method of the zirconium alloy that the application of the invention embodiment provides has been realized the purpose that the zirconium alloy second phase particle dispersion is distributed and improve the zirconium alloy even grain size.
Preferably, in the zirconium alloy heat treating method that above-described embodiment provides, 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 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 by 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 provide was handled zirconium alloy, the second phase particle dispersion of zirconium alloy energy 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 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 by carrying out metallurgical analysis after the method that adopts the embodiment of the invention to provide was handled zirconium alloy, the second phase particle dispersion of zirconium alloy energy 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 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 by carrying out metallurgical analysis after the method that adopts the embodiment of the invention to provide was handled zirconium alloy, the second phase particle dispersion of zirconium alloy energy 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 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 by carrying out metallurgical analysis after the method that adopts the embodiment of the invention to provide was handled zirconium alloy, the second phase particle dispersion of zirconium alloy energy 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 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 by carrying out metallurgical analysis after the method that adopts the embodiment of the invention to provide was handled zirconium alloy, the second phase particle dispersion of zirconium alloy energy 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 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 apparent 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 herein.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the wideest scope consistent with principle disclosed herein and features of novelty.
Claims (2)
1. the heat treating method of a zirconium alloy is characterized in that, may further comprise the steps:
Step 01) blank with described zirconium alloy carries out quench treatment, obtains the blank that quenches;
Step 02) with described quenching blank cool to room temperature, carries out the deformation process that deflection is 5%-30%, obtain the predeformation blank;
Step 03) described predeformation blank is heated to 350 ℃-700 ℃ and carries out the anneal first time, annealing time is 0.2 hour-30 hours;
Step 04) described predeformation blank is carried out hot rolling and handle, obtain the sheet material blank;
Step 05) described sheet material blank is carried out cold working after process annealing processing and the process annealing;
Step 06) repeated several times step 05), to described sheet material blank shape size conforms processing request, obtains sheet material;
Step 07) described 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, 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 Fe, Cr, the Cu alloying element of trace between 0.15%-1.25%, surplus is Zr.
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| CN113667914B (en) * | 2021-08-09 | 2022-04-19 | 燕山大学 | Method for preparing high-strength pure zirconium through cold deformation |
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