CN111889534A - Preparation method of nuclear zirconium alloy anisotropic wire - Google Patents
Preparation method of nuclear zirconium alloy anisotropic wire Download PDFInfo
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- CN111889534A CN111889534A CN201910367853.1A CN201910367853A CN111889534A CN 111889534 A CN111889534 A CN 111889534A CN 201910367853 A CN201910367853 A CN 201910367853A CN 111889534 A CN111889534 A CN 111889534A
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- 229910001093 Zr alloy Inorganic materials 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000005097 cold rolling Methods 0.000 claims abstract description 73
- 238000000034 method Methods 0.000 claims abstract description 34
- 230000008569 process Effects 0.000 claims abstract description 16
- 239000002344 surface layer Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000000137 annealing Methods 0.000 claims description 44
- 238000001035 drying Methods 0.000 claims description 32
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 24
- 239000010410 layer Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 13
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- 230000007547 defect Effects 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 238000005238 degreasing Methods 0.000 claims description 9
- 238000001125 extrusion Methods 0.000 claims description 6
- 239000003929 acidic solution Substances 0.000 claims description 5
- 238000005098 hot rolling Methods 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 238000012545 processing Methods 0.000 abstract description 14
- 238000005260 corrosion Methods 0.000 abstract description 6
- 230000007797 corrosion Effects 0.000 abstract description 6
- 239000000446 fuel Substances 0.000 description 8
- 238000005096 rolling process Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 239000013527 degreasing agent Substances 0.000 description 4
- 238000005237 degreasing agent Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- XLYOFNOQVPJJNP-ZSJDYOACSA-N Heavy water Chemical compound [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
- B21C37/04—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire
- B21C37/047—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire of fine wires
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C16/00—Alloys based on zirconium
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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
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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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
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/186—High-melting or refractory metals or alloys based thereon of zirconium or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/08—Iron or steel
- C23G1/086—Iron or steel solutions containing HF
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Abstract
The method discloses a preparation method of a zirconium alloy special-shaped wire for nuclear use, which comprises the following steps: heating the zirconium alloy bar blank; forming the heated zirconium alloy bar blank to obtain a first blank; carrying out surface layer treatment on the first blank to obtain a second blank; performing at least one first cold rolling treatment on the second blank to obtain a third blank; and carrying out second cold rolling treatment on the third blank to obtain the zirconium alloy wire. The method adopts the four-roller cold rolling wire preparation process with convenient operation and strong process controllability, so that the zirconium alloy rod blank is in a three-dimensional compressive stress state during processing, the deformation amount of cold rolling pass processing is large, and the zirconium alloy wire obtained by the method has the advantages of precise size, good corrosion resistance, certain strength and processing plasticity.
Description
Technical Field
The invention relates to the technical field of material preparation, in particular to a preparation method of a zirconium alloy special-shaped wire for a nuclear.
Background
The nuclear fuel assembly for the heavy water reactor consists of a zirconium alloy pressure pipe and a fuel rod bundle, wherein the fuel rod bundle consists of a plurality of fuel single rods (elements), the fuel rod bundle and the pressure pipe are isolated by a supporting pad punched by a zirconium alloy rectangular wire, and the fuel single rods (elements) are isolated by an isolating block punched by a zirconium alloy rectangular wire. The supporting pads and the isolating blocks have the functions of ensuring the smoothness of a heat exchange channel in the fuel assembly, preventing the single fuel rods (elements) from contacting with each other and being related to the safety of the fuel assembly, so that the zirconium alloy rectangular wire material is required to have precise size, good corrosion resistance and certain processing plasticity. The traditional processing method is die drawing or roller die drawing, the wire is in a two-direction pressing and one-direction drawing stress state, and the pass processing deformation of the wire is small. In addition, the drawing of the die has the problems that the processing stress of the inner fillet of the die is large, the abrasion is large, the die is easy to break, and the wire material is easy to have surface bonding defects; the problems of roller die drawing are that the round corners of rectangular wires are not easy to fill, and the dimensional accuracy does not meet the technical requirements.
Disclosure of Invention
The embodiment of the invention aims to enable a zirconium alloy bar blank to be in a three-dimensional compressive stress state during processing by adopting a four-roller cold rolling wire preparation process with convenient operation and strong process controllability, and the deformation amount of cold rolling pass processing is large.
In order to solve the technical problems, the embodiment of the invention provides a preparation method of a zirconium alloy special-shaped wire for a nuclear, which comprises the following steps:
heating the zirconium alloy bar blank;
carrying out forming treatment on the heated zirconium alloy bar blank to obtain a first blank;
carrying out surface layer treatment on the first blank to obtain a second blank;
carrying out at least one time of first cold rolling treatment on the second blank to obtain a third blank;
and carrying out second cold rolling treatment on the third blank to obtain the zirconium alloy wire.
Further, the heated zirconium alloy bar blank is subjected to forming treatment to obtain a first blank; wherein the forming process comprises:
carrying out multi-pass hot rolling on the heated zirconium alloy bar blank by using a section mill to obtain a first blank; or
And carrying out one-step forming extrusion on the heated zirconium alloy bar blank by using extrusion equipment to obtain the first blank.
Further, carrying out surface layer treatment on the surface of the first blank to obtain a second blank; wherein the surface layer treatment comprises:
removing the surface oxide layer and/or the surface defect layer of the first blank after the forming treatment;
and carrying out first-stage acid washing, rinsing and drying treatment on the first blank subjected to the surface oxide layer or surface defect layer removal treatment to obtain the second blank.
Further, performing at least one time of first cold rolling treatment on the second blank to obtain a third blank; wherein the first cold rolling process comprises:
performing a first-stage cold rolling treatment on the second blank by using a four-roller section mill;
carrying out oil removal and degreasing treatment on the second blank subjected to the first-stage cold rolling treatment;
drying the second blank after oil removal and degreasing treatment;
and carrying out first-stage vacuum annealing treatment on the dried second blank to obtain a third blank.
Further, the first-stage cold rolling treatment is multi-pass cold rolling treatment; wherein,
the pass cold rolling deformation rate is 13-19%;
the total rate of deformation is less than or equal to 70%.
Further, performing second cold rolling treatment on the third blank to obtain a fourth blank; wherein the second cold rolling process comprises:
performing second-stage cold rolling treatment on the third blank by using a four-roller section mill;
performing second-stage vacuum annealing treatment on the third blank subjected to the second-stage cold rolling treatment;
and carrying out second-stage acid washing, rinsing and drying treatment on the third blank subjected to the second-stage vacuum annealing treatment to obtain the zirconium alloy wire.
Further, the third blank is subjected to a second-stage cold rolling treatment by using a four-roller section mill; wherein in the second stage cold rolling treatment, the cold rolling deformation rate is less than or equal to 10%.
Further, the temperature of the vacuum annealing treatment is 600-700 ℃;
the time of the vacuum annealing treatment is 210 min;
the vacuum degree of the vacuum annealing treatment is less than 1 multiplied by 10-2Pa。
Further, the acid solution used for pickling comprises: nitric acid, hydrofluoric acid and water; and/or
The rinsing time is 10min-20 min; and/or
The drying time is 30-60 min, and the drying temperature is 93-120 ℃.
Further, in the acidic solution, the proportion of the nitric acid is 10% -45%; the proportion of the hydrofluoric acid is 1% -5%; the balance being water.
The technical scheme of the embodiment of the invention has the following beneficial technical effects:
the zirconium alloy rod blank is in a three-dimensional compressive stress state during processing by adopting a four-roller cold rolling wire preparation process with convenient operation and strong process controllability, the deformation amount of cold rolling pass processing is large, and the zirconium alloy wire obtained by using the method has the advantages of precise size, good corrosion resistance, certain strength and processing plasticity.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing a zirconium alloy special-shaped wire for a core according to an embodiment of the invention;
FIG. 2 is a flowchart illustrating a step S300 according to an embodiment of the present invention;
FIG. 3 is a flowchart of step S400 according to an embodiment of the present invention;
fig. 4 is a flowchart illustrating step S500 according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings in conjunction with the following detailed description. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
The zirconium alloy of the embodiment of the invention comprises the following chemical components (mass fraction): 1.20 to 1.70 percent of Sn, 0.18 to 0.24 percent of Fe, 0.07 to 0.13 percent of Cr, 0.28 to 0.37 percent of Fe and Cr, 0.09 to 0.15 percent of O, 0.0080 to 0.0160 percent of C, 0.0080 to 0.0120 percent of Si and zirconium as a matrix.
FIG. 1 is a schematic flow chart of a method for preparing a zirconium alloy profiled wire for a core in an embodiment of the invention.
Referring to fig. 1, an embodiment of the present invention provides a method for preparing a zirconium alloy specially-shaped wire for a core, including the following steps:
and S100, heating the zirconium alloy bar blank. First, a zirconium alloy rod blank was heated using an electric furnace.
Optionally, the heating temperature range is 650-750 ℃, and the heating time range is 45-60 min.
Optionally, the diameter range of the zirconium alloy bar blank is phi 86 mm-phi 30 mm.
And S200, forming the heated zirconium alloy rod blank to obtain a first blank. After the zirconium alloy bar blank is heated, the zirconium alloy bar blank is placed on a section mill for molding treatment, and a first blank with the diameter of phi 8 mm-phi 13mm is obtained.
And S300, performing surface layer treatment on the first blank to obtain a second blank.
And S400, performing at least one first cold rolling treatment on the second blank to obtain a third blank.
And S500, carrying out second cold rolling treatment on the third blank to obtain the zirconium alloy wire.
In one embodiment of the present invention, the step S200 of forming the heated zirconium alloy rod blank to obtain the first blank includes: and (3) carrying out multi-pass hot rolling on the heated zirconium alloy bar blank by using a section mill to obtain a first blank.
In another embodiment of the present invention, the step S200 of forming the heated zirconium alloy rod blank to obtain the first blank includes: and carrying out one-step forming extrusion on the heated zirconium alloy bar blank by using extrusion equipment to obtain a first blank.
Fig. 2 is a flowchart illustrating step S300 according to an embodiment of the present invention.
Referring to fig. 2, in step S300, performing a surface layer treatment on the surface of the first blank to obtain a second blank includes the following steps:
s310, removing the surface oxidation layer and/or the surface defect layer of the first blank after the forming treatment. Wherein, the surface defect layer comprises surface defects of the bonding and folding stool.
S320, performing first-stage acid washing, rinsing and drying treatment on the first blank subjected to the surface oxide layer or surface defect layer removing treatment to obtain a second blank.
Optionally, in step S320, the acidic solution used in the first-stage acid washing includes: nitric acid, hydrofluoric acid and water. Preferably, the proportion of the nitric acid is 10-45%; the proportion of the hydrofluoric acid is 1-5%; the balance being water.
Optionally, the rinsing time with deionized water is 10min-20 min.
Optionally, the drying time is 30min-60min, and the drying temperature is 93 ℃ -120 ℃.
Fig. 3 is a flowchart illustrating step S400 according to an embodiment of the present invention.
Referring to fig. 3, in step S400, the first cold rolling process is performed at least once on the second blank to obtain a third blank, including the following steps:
and S410, performing first-stage cold rolling treatment on the second blank by using a four-roller section mill.
Optionally, in step S410, the first stage cold rolling process is a multi-pass cold rolling process. Wherein, the pass cold rolling deformation rate is 13-19%; the total rate of deformation is less than or equal to 70%. The second billet is cooled using rolling lubricant.
And S420, performing oil removal and degreasing treatment on the second blank subjected to the first-stage cold rolling treatment.
And S430, drying the second blank after oil removal and degreasing treatment.
And S440, carrying out first-stage vacuum annealing treatment on the dried second blank to obtain a third blank.
Optionally, in the first-stage vacuum annealing treatment performed in step S440, the temperature range of the vacuum annealing treatment is 600 ℃ to 700 ℃; the time of vacuum annealing treatment is 210 min; the vacuum degree of the vacuum annealing treatment is less than 1 multiplied by 10-2Pa。
Fig. 4 is a flowchart illustrating step S500 according to an embodiment of the present invention.
Referring to fig. 4, in step S500, the second cold rolling process is performed on the third blank to obtain a fourth blank, including the following steps:
and S510, performing second-stage cold rolling treatment on the third blank by using a four-roller section mill.
Optionally, in step S510, a four-high rolling mill is used to perform a second stage cold rolling process on the third blank, and the second stage cold rolling deformation rate is less than or equal to 10%.
S520, performing second-stage vacuum annealing treatment on the third blank subjected to the second-stage cold rolling treatment to obtain a semi-finished zirconium alloy wire.
The second stage of vacuum annealing treatment is carried out in the step S520, and the temperature range of the vacuum annealing treatment is 600-700 ℃; the time of vacuum annealing treatment is 60min-210 min; the vacuum degree of the vacuum annealing treatment is less than 1 multiplied by 10-2Pa. Annealing at a lower temperature when the cumulative working deformation is larger and annealing at a higher temperature when the cumulative working deformation is smaller. When the annealing material is more, the annealing time is longer in order to make the temperature of the annealing material uniform; when the annealing material is less, the annealing time is shorter in order to make the annealing material temperature uniform.
S530, carrying out second-stage acid washing, rinsing and drying on the third blank subjected to the second-stage vacuum annealing treatment to obtain the zirconium alloy wire.
Optionally, in step S530, the acidic solution used in the second-stage acid washing includes: nitric acid, hydrofluoric acid and water. Preferably, the proportion of the nitric acid is 10-45%; the proportion of the hydrofluoric acid is 1-5%; the balance being water.
Optionally, the rinsing time with deionized water is 10min-20 min.
Optionally, the drying time is 30min-60min, and the drying temperature is 93 ℃ -120 ℃. The zirconium alloy blank has a large diameter, and is easy to rinse and dry, so that the rinsing time is short, and the drying temperature and time are low.
In a preferred embodiment of the invention, the preparation process of the zirconium alloy wire is as follows:
in the step S100, an electric furnace is used for heating the zirconium-4 alloy bar blank with the diameter of phi 60mm at the temperature of 700 +/-50 ℃ for 45-60 min.
In step S200, the heated zirconium-4 alloy bar blank is placed on a section rolling mill to be subjected to multi-pass hot rolling, and a first blank with the diameter of phi 13mm is obtained.
In step S300, the surface oxide layer and/or the surface defect layer of the first blank is removed, then the first blank is cleaned with an acidic solution containing nitric acid and hydrofluoric acid (45% nitric acid, 5% hydrofluoric acid, and the balance water), and finally rinsed with deionized water and dried (drying time is 30min, drying temperature is 93 ℃), so as to obtain a second blank.
In the step S400, the process is performed,
and (3) carrying out first stage first cold rolling treatment on the second blank: and (3) carrying out multi-pass cold rolling on the second blank by using a four-roller section mill, wherein the pass cold rolling deformation rate is 13-19%, the accumulated total deformation rate is 66.2%, and the rolling size is 7.56±0.25mm×7.56±0.25mm; then, the second blank is placed in an alkaline degreasing agent for degreasing, and is dried (the drying time is 30min, and the drying temperature is 93 ℃); finally, vacuum annealing treatment is carried out, the annealing temperature is 650 ℃, the annealing time is 210min, and the vacuum pressure is less than 1 multiplied by 10-2Pa。
And (3) carrying out second-time first cold rolling treatment on the second blank: and (3) carrying out multi-pass cold rolling on the second blank by using a four-roller section mill, wherein the pass cold rolling deformation rate is 13-19%, the accumulated total deformation rate is 59.7%, and the rolling size is 4.8±0.25mm×4.8± 0.25mm; then, the second blank is placed in an alkaline degreasing agent for degreasing, and is dried (the drying time is 45min, and the drying temperature is 100 ℃); finally, vacuum annealing treatment is carried out, the annealing temperature is 650 ℃, the annealing time is 210min, and the vacuum pressure is less than 1 multiplied by 10-2Pa。
And (3) carrying out third first cold rolling treatment on the second blank: and (3) carrying out multi-pass cold rolling on the second blank by using a four-roller section mill, wherein the pass cold rolling deformation rate is 13-19%, the accumulated total deformation rate is 55.6%, and the rolling size is 3.2±0.25mm×3.2± 0.25mm; then, the second blank is placed in an alkaline degreasing agent for degreasing, and is dried (the drying time is 45min, and the drying temperature is 100 ℃); finally, vacuum annealing treatment is carried out, the annealing temperature is 650 ℃, the annealing time is 210min, and the vacuum pressure is less than 1 multiplied by 10-2Pa。
And (3) performing fourth first cold rolling treatment on the second blank: and (3) carrying out multi-pass cold rolling on the second blank by using a four-roller section mill, wherein the pass cold rolling deformation rate is 13-19%, the accumulated total deformation rate is 51.7%, and the rolling size is 1.66±0.25mm×2.98±0.25mm; then the second blank is put into an alkaline degreasing agent for degreasingAnd drying (drying time is 60min, drying temperature is 93 ℃); finally, vacuum annealing treatment is carried out, the annealing temperature is 650 ℃, the annealing time is 210min, and the vacuum pressure is less than 1 multiplied by 10-2Pa。
And performing four times of first cold rolling treatment on the second blank to obtain a third blank.
In step S500, the second-stage cold rolling treatment is performed on the third billet, and the second-stage cold rolling treatment has a cold rolling deformation rate of 9.5% and a rolling size of 1.56±0.25mm×2.87±0.25mm; vacuum annealing at 600 deg.C for 210min under a vacuum pressure of less than 1 × 10-2Pa; and (3) cleaning the third blank by using an acid solution (25% nitric acid, 3% hydrofluoric acid and the balance water) containing nitric acid and hydrofluoric acid, finally rinsing by using deionized water (the rinsing time is 10-20 min) and drying (the drying time is 60min and the drying temperature is 120 ℃) to obtain the zirconium-4 alloy wire. Wherein the diameter removal amount of the acid washing is 0.01mm-0.02 mm.
Sampling and detecting the zirconium-4 alloy wire, and detecting the bending performance, uniform corrosion, grain size and macrostructure.
The performance test data of the zirconium alloy special-shaped wire for the core prepared by the embodiment are shown in the table 1.
TABLE 1 results of performance test data of zirconium alloy wire for nuclear applications in accordance with the embodiments of the present invention
As can be seen from Table 1, the zirconium alloy wire prepared by the above embodiment meets the technical requirements of products, the macroscopic structure is qualified by inspection, and the room-temperature tensile and uniform corrosion resistance properties are qualified.
The embodiment of the invention aims to provide a preparation method of a zirconium alloy special-shaped wire for a nuclear, which comprises the following steps: heating the zirconium alloy bar blank; forming the heated zirconium alloy bar blank to obtain a first blank; carrying out surface layer treatment on the first blank to obtain a second blank; performing at least one first cold rolling treatment on the second blank to obtain a third blank; and carrying out second cold rolling treatment on the third blank to obtain the zirconium alloy wire. The technical scheme has the following beneficial effects:
the zirconium alloy rod blank is in a three-dimensional compressive stress state during processing by adopting a four-roller cold rolling wire preparation process with convenient operation and strong process controllability, the deformation amount of cold rolling pass processing is large, and the zirconium alloy wire obtained by using the method has the advantages of precise size, good corrosion resistance, certain strength and processing plasticity.
It is to be understood that the above-described embodiments of the present invention are merely illustrative of or explaining the principles of the invention and are not to be construed as limiting the invention. Therefore, any modification, equivalent replacement, improvement and the like made without departing from the spirit and scope of the present invention should be included in the protection scope of the present invention. Further, it is intended that the appended claims cover all such variations and modifications as fall within the scope and boundaries of the appended claims or the equivalents of such scope and boundaries.
Claims (10)
1. A preparation method of a zirconium alloy special-shaped wire for a nuclear is characterized by comprising the following steps:
heating the zirconium alloy bar blank;
carrying out forming treatment on the heated zirconium alloy bar blank to obtain a first blank;
carrying out surface layer treatment on the first blank to obtain a second blank;
carrying out at least one time of first cold rolling treatment on the second blank to obtain a third blank;
and carrying out second cold rolling treatment on the third blank to obtain the zirconium alloy wire.
2. The method for preparing the zirconium alloy specially-shaped wire for the core as claimed in claim 1, wherein the heated zirconium alloy rod blank is subjected to a forming treatment to obtain a first blank; wherein the forming process comprises:
carrying out multi-pass hot rolling on the heated zirconium alloy bar blank by using a section mill to obtain a first blank; or
And carrying out one-step forming extrusion on the heated zirconium alloy bar blank by using extrusion equipment to obtain the first blank.
3. The method for preparing the zirconium alloy special-shaped wire for the core as claimed in claim 1, wherein the surface layer treatment is performed on the first blank to obtain a second blank; wherein the surface layer treatment comprises:
removing the surface oxide layer and/or the surface defect layer of the first blank after the forming treatment;
and carrying out first-stage acid washing, rinsing and drying treatment on the first blank subjected to the surface oxide layer or surface defect layer removal treatment to obtain the second blank.
4. The method for preparing the zirconium alloy special-shaped wire for the core as claimed in claim 1, wherein the second blank is subjected to at least one first cold rolling treatment to obtain a third blank; wherein the first cold rolling process comprises:
performing a first-stage cold rolling treatment on the second blank by using a four-roller section mill;
carrying out oil removal and degreasing treatment on the second blank subjected to the first-stage cold rolling treatment;
drying the second blank after oil removal and degreasing treatment;
and carrying out first-stage vacuum annealing treatment on the dried second blank to obtain a third blank.
5. The method for preparing a zirconium alloy shaped wire for a core according to claim 4,
the first stage cold rolling treatment is multi-pass cold rolling treatment; wherein,
the pass cold rolling deformation rate is 13-19%;
the total rate of deformation is less than or equal to 70%.
6. The method for preparing the zirconium alloy special-shaped wire for the nuclear, according to claim 1, wherein the third blank is subjected to a second cold rolling treatment to obtain a fourth blank; wherein the second cold rolling process comprises:
performing second-stage cold rolling treatment on the third blank by using a four-roller section mill;
performing second-stage vacuum annealing treatment on the third blank subjected to the second-stage cold rolling treatment;
and carrying out second-stage acid washing, rinsing and drying treatment on the third blank subjected to the second-stage vacuum annealing treatment to obtain the zirconium alloy wire.
7. The method for preparing a zirconium alloy shaped wire for a core according to claim 6,
the third blank is subjected to second-stage cold rolling treatment by using a four-roller section mill; wherein in the second stage cold rolling treatment, the cold rolling deformation rate is less than or equal to 10%.
8. The method for preparing a zirconium alloy shaped wire for a core according to claim 4 or 6,
the temperature of the vacuum annealing treatment is 600-700 ℃;
the time of the vacuum annealing treatment is 60min-210 min;
the vacuum degree of the vacuum annealing treatment is less than 1 multiplied by 10-2Pa。
9. The method for preparing the zirconium alloy profiled wire for the core as claimed in claim 3 or 6, wherein the acid solution used for the acid washing comprises: nitric acid, hydrofluoric acid and water; and/or
The rinsing time is 10min-20 min; and/or
The drying time is 30-60 min, and the drying temperature is 93-120 ℃.
10. The method for preparing a zirconium alloy shaped wire for a core in accordance with claim 9, wherein in the acidic solution,
the proportion of the nitric acid is 10-45%;
the proportion of the hydrofluoric acid is 1% -5%;
the balance being water.
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