CN110878406A - Processing method of strengthened zirconium alloy strip and zirconium alloy strip - Google Patents
Processing method of strengthened zirconium alloy strip and zirconium alloy strip Download PDFInfo
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- CN110878406A CN110878406A CN201910286013.2A CN201910286013A CN110878406A CN 110878406 A CN110878406 A CN 110878406A CN 201910286013 A CN201910286013 A CN 201910286013A CN 110878406 A CN110878406 A CN 110878406A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The invention discloses a zirconium alloy strip processing method which comprises the steps of carrying out first forging treatment on a pretreated zirconium alloy cast ingot in a β phase region to obtain a zirconium alloy forging blank with a first thickness, adjusting the zirconium alloy forging blank to form a preset angle with a liquid level, carrying out quenching treatment at a first temperature to obtain a zirconium alloy plate blank, carrying out surface machining treatment on the zirconium alloy plate blank to obtain a zirconium alloy plate blank with metallic color, carrying out rolling and annealing treatment on the zirconium alloy plate blank with the metallic color in sequence, carrying out hot rolling and cold rolling for at least two times in sequence, and finally carrying out annealing treatment after the hot rolling and each cold rolling process are finished to obtain a zirconium alloy strip finished product.
Description
Technical Field
The invention belongs to the technical field of preparation of zirconium alloy materials, and particularly relates to a processing method of a zirconium alloy strip.
Background
The zirconium alloy has the advantages of low thermal neutron absorption cross section, high thermal conductivity, good corrosion resistance and the like, so the zirconium alloy is a structural material widely applied in the nuclear industry, wherein a zirconium alloy strip is mainly used for manufacturing a positioning lattice, stress relaxation of the positioning lattice under the neutron irradiation condition can cause the reduction of the clamping force of the lattice on a fuel rod, the friction between the lattice and the fuel rod is caused, and the damage is caused to a reactor. However, at present, in order to enhance the mechanical properties of the zirconium alloy in a completely recrystallized state, the content of alloy components is increased, and other technical methods for obviously improving the strength of the zirconium alloy under the condition that the alloy components are not changed do not exist.
Disclosure of Invention
The invention aims to provide a method for processing a zirconium alloy strip, which solves the problem of poor mechanical property of the zirconium alloy strip.
In order to solve the problems, the first aspect of the invention provides a zirconium alloy strip processing method which comprises the steps of carrying out first forging treatment on a pretreated zirconium alloy cast ingot in a phase β region to obtain a zirconium alloy forging blank with a first thickness, adjusting the zirconium alloy forging blank to form a preset angle with a liquid level, carrying out quenching treatment at a first temperature to obtain a zirconium alloy plate blank, carrying out surface machining treatment on the zirconium alloy plate blank to obtain a metallic zirconium alloy plate blank, carrying out rolling and annealing treatment on the metallic zirconium alloy plate blank in sequence, carrying out hot rolling and cold rolling in sequence at least twice, and carrying out annealing treatment after the hot rolling and each cold rolling process are finished to obtain a finished zirconium alloy strip.
Further, the step of performing first forging treatment on the pretreated zirconium alloy ingot in a phase β region to obtain a first-thickness zirconium alloy forging blank is further followed by the steps of:
and performing second forging treatment on the zirconium alloy forging blank with the first thickness in a phase region of β to obtain a zirconium alloy forging blank with a second thickness.
Further, the first forging process specifically comprises: preserving the heat of the pretreated zirconium alloy ingot for a first time at a second temperature, and cogging and forging to obtain a zirconium alloy forging blank with a first thickness; the second forging treatment specifically comprises the following steps: and keeping the temperature of the rough blank of the zirconium alloy plate with the first thickness for a second time at a third temperature, and cogging and forging to obtain a forged blank of the zirconium alloy with the second thickness.
Further, the first thickness is 100-150 mm; the second thickness is 30-50 mm; the second temperature is 950-1150 ℃; the third temperature is 800-1000 ℃; the first time period is greater than 3.5 hours; the second time period (T ═ 1.2 xh +30) is divided into 10 hours; t: and (5) keeping the temperature for h, namely the thickness of the plate blank.
Further, the preset angle is 30-90 degrees; the first temperature is 950-1150 ℃.
Further wherein the surfacing single edge removal is greater than 4 mm.
Further, the rolling and annealing treatment are sequentially performed on the zirconium alloy plate blank in the metallic color, at least two times of hot rolling and at least two times of cold rolling are sequentially performed, and finally the annealing treatment is performed after the hot rolling and each cold rolling are completed, so that the zirconium alloy strip finished product is obtained, and the method specifically comprises the following steps: carrying out hot rolling treatment on the zirconium alloy plate blank in the metallic color, wherein the total hot rolling processing rate is 80-97%, and obtaining a hot-rolled zirconium alloy plate blank; carrying out atmospheric annealing on the hot-rolled zirconium alloy plate blank to obtain a zirconium alloy plate; performing first cold rolling or repeated cold rolling treatment on the zirconium alloy plate for multiple times to obtain a cold-rolled zirconium alloy plate; welding, coiling and vacuum annealing are carried out on the cold-rolled zirconium alloy plate to obtain a zirconium alloy coiled material; performing final cold rolling treatment on the zirconium alloy coiled material, wherein the total processing amount after all cold rolling is 45-70%, and obtaining a semi-finished strip; and carrying out continuous oil removing and annealing treatment on the semi-finished strip to obtain a finished zirconium alloy strip.
Further, the hot rolling treatment specifically comprises the following steps: keeping the temperature T of a zirconium alloy plate blank in a metallic color at 550-750 ℃ to be 1.2 Xh + 30-1.2 Xh +90 min; t: and (5) keeping the temperature for h, namely the thickness of the plate blank, and then carrying out hot rolling to obtain the hot-rolled zirconium alloy plate blank.
Further, the atmospheric annealing specifically comprises: and (3) keeping the temperature T of the hot-rolled zirconium alloy plate blank to be 1.2 Xh + 30-1.2 Xh +90 min at the temperature of 600-750 ℃, wherein h is the stacking thickness of the plate, and carrying out atmospheric annealing.
Further, the vacuum annealing specifically comprises: the cold-rolled zirconium alloy plate is kept at the temperature of 600 ℃ for 1.2 Xh +30 min-1.2 Xh +90 min, h is the stacking thickness of the plate, and the vacuum degree is more than 0.9X 10-2Vacuum annealing is carried out under Pa.
Further, the continuous annealing specifically comprises: and carrying out continuous annealing at 625-675 ℃, wherein the speed of the continuous annealing is 0.3-1.5 m/min.
Further, the first cold rolling treatment specifically comprises: carrying out surface treatment on the zirconium alloy plate, wherein the surface treatment adopts sand blasting and acid pickling, the sand blasting gravel is silicon carbide particles, the acid pickling gravel is mixed solution of hydrofluoric acid, nitric acid and water, and the mixture ratio is 35-45 percent of HNO3+3％～8％HF+H2O, obtaining a zirconium alloy plate with a clean surface; and carrying out plate type cold rolling on the zirconium alloy plate with the clean surface, welding into coils, carrying out vacuum annealing, and carrying out coil cold rolling to obtain the cold-rolled zirconium alloy strip.
In another aspect, the invention provides a zirconium alloy strip, which is characterized by being processed by the method.
The technical scheme of the invention has the following beneficial technical effects:
(1) the process flow is simple, the controllability of process parameters is strong, and the method is easy to apply to industrial production;
(2) the strength of the zirconium alloy strip is obviously improved under the condition that the alloy components are not changed;
(3) has excellent corrosion resistance, plasticity and the like.
Drawings
FIG. 1 is a flow chart of a method of processing a zirconium alloy strip according to a first embodiment of the present invention;
FIG. 2 is a flow diagram of a method of processing a zirconium alloy strip according to another embodiment of the present invention;
FIG. 3 is a flow chart of a rolling and annealing process according to yet another embodiment of the present invention;
FIG. 4 is a flow chart of a first cold rolling process according to yet another embodiment of the present invention;
FIG. 5 is an electron microscopic structural view of a zirconium alloy strip produced 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.
It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
FIG. 1 is a flow chart of a method of processing a zirconium alloy strip according to a first embodiment of the present invention.
According to an embodiment of the present application, a zirconium alloy strip processing method is provided, as shown in fig. 1, specifically including:
s1, forging the pretreated zirconium alloy ingot in a β phase region to obtain a zirconium alloy forging blank with a first thickness;
s2: adjusting the zirconium alloy forging blank to form a preset angle with the liquid level, and quenching at a first temperature to obtain a zirconium alloy plate blank;
s3: performing surface machining treatment on the zirconium alloy plate blank to obtain a zirconium alloy plate blank in a metallic color;
s4: and sequentially rolling and annealing the zirconium alloy plate blank in the metallic color, and sequentially performing at least two times of hot rolling and at least two times of cold rolling, wherein after each time of rolling, the annealing treatment is performed to obtain a zirconium alloy strip finished product.
The pretreated zirconium alloy ingot in the step S1 is to treat the dust impurities on the surface of the zirconium alloy ingot clean, the impurities which are difficult to remove can be removed by mechanical processing and washing, and the β phase region is a high-temperature stable phase.
The surfacing treatment in the step S3 comprises an upper surface, a lower surface and a side surface, and specifically comprises the steps of milling the upper surface and the lower surface by a milling machine to remove surface oxide skin and a quenching lath tissue layer, and ensuring that the surface of the plate blank is smooth and metallic after the treatment.
The zirconium alloy strip manufactured by the method has the advantages of simple process, strong controllability of process parameters, easy application to industrial production, obvious improvement of the strength of the zirconium alloy strip under the condition of unchanged alloy components, excellent corrosion resistance, excellent plasticity and the like.
Optionally, the step of performing a first forging treatment on the pretreated zirconium alloy ingot in a phase β region to obtain a zirconium alloy forging blank with a first thickness is further followed by:
and performing second forging treatment on the zirconium alloy forging blank with the first thickness in a phase region of β to obtain a zirconium alloy forging blank with a second thickness.
FIG. 2 is a flow chart of a method of processing a zirconium alloy strip according to another embodiment of the present invention.
In an alternative embodiment, the step of subjecting the pretreated zirconium alloy ingot to a first forging treatment in the β phase region to obtain a first thickness zirconium alloy forging blank is further followed by the step of subjecting the first thickness zirconium alloy forging blank to a second forging treatment in the β phase region to obtain a second thickness zirconium alloy forging blank, as shown in fig. 2, specifically comprising:
s1, forging the pretreated zirconium alloy ingot in a β phase region to obtain a zirconium alloy forging blank with a first thickness;
s2, performing secondary forging treatment on the zirconium alloy forging blank with the first thickness in a β phase region to obtain a zirconium alloy forging blank with a second thickness;
s3: adjusting the zirconium alloy forging blank with the second thickness to form a preset angle with the liquid level, and quenching at a first temperature to obtain a zirconium alloy plate blank;
s4: performing surface machining treatment on the zirconium alloy plate blank to obtain a zirconium alloy plate blank in a metallic color;
s5: and sequentially rolling and annealing the zirconium alloy plate blank in the metallic color, and sequentially performing at least two times of hot rolling and at least two times of cold rolling, wherein after each time of rolling, the annealing treatment is performed to obtain a zirconium alloy strip finished product.
Optionally, the first forging process specifically includes: preserving the heat of the pretreated zirconium alloy ingot for a first time at a second temperature, and cogging and forging to obtain a zirconium alloy forging blank with a first thickness; the second forging treatment specifically comprises the following steps: and keeping the temperature of the rough blank of the zirconium alloy plate with the first thickness for a second time at a third temperature, and cogging and forging to obtain a forged blank of the zirconium alloy with the second thickness.
Optionally, the first thickness is 100-150 mm, preferably 110-120 mm; the second thickness is 30-50 mm, preferably 40 mm; the second temperature is 950-1150 ℃; the third temperature is 800-1000 ℃; the first time period is greater than 3.5 hours; the second time (T is 1.2 × h +30) is divided into 10 hours; t: and (h) keeping the temperature for h, wherein the thickness of the stacked plates is. Under the condition, the forging can improve the structure and the mechanical property of the zirconium alloy. After the zirconium alloy ingot is deformed by forging and processing, because of metal deformation and recrystallization, original thick dendritic crystals and columnar crystal grains are changed into equiaxial recrystallization structures with thinner crystal grains and uniform sizes, original segregation, looseness, air holes, slag inclusion and the like in the zirconium alloy ingot are compacted and welded, the structures become tighter, and the plasticity and mechanical property of the zirconium alloy are improved.
Optionally, the preset angle is an included angle of 30-90 degrees; the first temperature is 950-1150 ℃. And (2) carrying out water quenching on the zirconium alloy plate under the condition that the temperature is 950-1150 ℃, wherein the temperature of the plate blank is 30-90 ℃ with the water surface when the plate blank enters water, the transfer time of quenching is less than 60 seconds, and the temperature of the water before entering the water is not higher than 36 ℃.
Optionally, the single-edge removal amount of the surfacing machining is more than 4 mm. After treatment, the surface of the zirconium alloy plate blank is smooth and is in metallic color.
The zirconium alloy strip manufactured by the method has the advantages that the strength of the zirconium alloy strip is obviously improved under the condition that the alloy components are not changed, and the zirconium alloy strip has excellent corrosion resistance, plasticity and the like.
Fig. 3 is a flow chart of a rolling and annealing process according to yet another embodiment of the present invention.
As shown in fig. 3, in an alternative embodiment, the rolling and annealing treatments are sequentially performed on a zirconium alloy slab in a metallic color, and at least two hot rolling and at least two cold rolling are sequentially performed, and the final hot rolling and each cold rolling are performed with an annealing treatment to obtain a zirconium alloy strip finished product, which specifically includes: s41, carrying out hot rolling treatment on the zirconium alloy plate blank with the metallic color, wherein the total hot rolling processing rate is 80-97%, and obtaining the zirconium alloy plate blank subjected to hot rolling treatment; s42, carrying out atmospheric annealing on the zirconium alloy plate blank subjected to hot rolling treatment to obtain a zirconium alloy plate; s43, performing first cold rolling or repeated cold rolling treatment on the zirconium alloy plate for multiple times to obtain a cold-rolled zirconium alloy plate; s44, welding and coiling the cold-rolled zirconium alloy sheet, and performing vacuum annealing to obtain a zirconium alloy coil; s45, carrying out final cold rolling treatment on the zirconium alloy coil, wherein the total processing amount after all cold rolling is 45-70%, and obtaining a semi-finished strip; and S46, carrying out continuous oil removing and annealing treatment on the semi-finished strip to obtain a finished zirconium alloy strip. Wherein the final hot rolling is a second hot rolling.
The zirconium alloy strip manufactured by the method has the advantages that the strength of the zirconium alloy strip is obviously improved under the condition that the alloy components are not changed, and the zirconium alloy strip has excellent corrosion resistance, plasticity and the like.
Optionally, the hot rolling treatment specifically comprises: keeping the temperature T of a zirconium alloy plate blank in a metallic color at 550-750 ℃ to be 1.2 Xh + 30-1.2 Xh +90 min; t: and (5) keeping the temperature for h, namely the thickness of the plate blank, and then carrying out hot rolling to obtain the hot-rolled zirconium alloy plate blank.
Optionally, the atmospheric annealing specifically comprises: and (3) keeping the temperature T of the hot-rolled zirconium alloy plate blank to be 1.2 Xh + 30-1.2 Xh +90 min at the temperature of 600-750 ℃, wherein h is the stacking thickness of the plate, and carrying out atmosphere annealing.
Optionally, the vacuum annealing specifically comprises: cold rolling zirconium alloy plate at 600 deg.c for 1.2 Xh + 30-1.2 Xh +90 min, and the stacking thickness of the plate should be greater than 0.9X 10-2Vacuum annealing is carried out under Pa.
Optionally, the continuous annealing specifically comprises: and carrying out continuous annealing at 625-675 ℃, wherein the speed of the continuous annealing is 0.3-1.5 m/min.
Fig. 4 is a flowchart of a first cold rolling process according to still another embodiment of the present invention.
As shown in fig. 4, in an alternative embodiment, the first cold rolling process specifically includes: 431, performing surface treatment on the zirconium alloy plate, wherein the surface treatment adopts sand blasting and acid pickling, grit used in the sand blasting is silicon carbide particles, the acid pickling is mixed solution of hydrofluoric acid, nitric acid and water, and the mixture ratio is 35-45% of HNO3+3％～8％HF+H2O, obtaining a zirconium alloy plate with a clean surface; and S432, carrying out plate type cold rolling on the clean zirconium alloy plate on the surface, welding and coiling, carrying out vacuum annealing, and carrying out coil cold rolling on the coil to obtain a cold-rolled zirconium alloy strip. Specifically, the zirconium alloy plate is subjected to sand blasting and acid pickling treatment to remove defects such as surface oxide scale, metal and nonmetal pressing-in, and the removal amount is more than 0.3 mm. Then, cold rolling the zirconium alloy plate on a cold rolling mill from 3-4 mm to 1.2-1.5 mm, wherein the pass deformation is 3-8%, and the total deformation is 45-70%, removing oil from the cold-rolled plate, and completely removing oil stains on the surface of the plate.
The zirconium alloy strip manufactured by the method has the advantages that the strength of the zirconium alloy strip is obviously improved under the condition that the alloy components are not changed, and the zirconium alloy strip has excellent corrosion resistance, plasticity and the like.
Optionally, the surface oiled plate is subjected to heat preservation for 2.5 hours at the temperature of 600-650 ℃ for vacuum annealing, and the vacuum degree of the vacuum annealing furnace is not more than 1.0 multiplied by 10-2And (6) handkerchief.
Optionally, the zirconium alloy sheet subjected to vacuum annealing is subjected to strip cold rolling on a cold rolling mill from 1.2-1.5 mm to 0.4-0.6 mm, the pass deformation is 1-5%, and the total deformation is 50-66%.
Optionally, the zirconium alloy strip subjected to the second cold rolling is coiled on continuous oil removing annealing equipment for continuous oil removing annealing, the annealing temperature is 625-750 ℃, and the zirconium alloy strip with a uniform structure can be prepared after heat preservation for 3-10 minutes.
In an optional embodiment, the processing technology for improving the mechanical property of the zirconium alloy strip comprises the following steps:
the method comprises the steps of cogging and forging zirconium alloy cast ingots in a β phase region to obtain forged slabs with the thickness of 100-150 mm, performing secondary forging on the zirconium alloy slabs with the thickness of 100 mm to 30-50 mm at the temperature of 800-900 ℃, performing water quenching on the forged slabs at the temperature of 1000-1100 ℃, wherein the slab is required to form an included angle of 30-90 ℃ with a water surface when being put into water, performing surface treatment on the slabs to completely remove a surface oxide layer (the surface treatment removal amount is more than 8 mm) to enable the surfaces of the slabs to be bright metallic, performing hot rolling on the zirconium alloy slabs after the surface treatment at the temperature of 550-750 ℃ to obtain hot rolled plates with the thickness of 3-4 mm, wherein the hot rolling pass deformation amount is 10-30%, performing heat treatment on the hot rolled plates by adopting an atmospheric annealing or vacuum annealing process, performing annealing at the annealing temperature of not less than 600 ℃, performing continuous annealing at the holding time T of 1.2 x h +30 min-1.2 x h +90 min, performing continuous annealing at the temperature of 1.5-675 ℃ to obtain cold rolled plates, and performing continuous annealing at the mechanical annealing at the temperature of 650-675 mm to obtain zirconium alloy strips with the thickness of 2 x h, and performing continuous annealing at the cold rolling time of 1.6 mm.
In another aspect, the invention provides a zirconium alloy strip processed by the method of the above embodiment. The technical problem to be solved by the invention is that the mechanical property of the zirconium alloy in a complete recrystallization state is improved by adopting a hot rolling mill annealing process which is matched with the process of reducing the quenching thickness and the water inlet angle of a plate blank under the condition of using the zirconium alloy with the same alloy grade, namely under the condition of keeping the alloy content unchanged.
Examples
Example 1
Cleaning the surface of a zirconium alloy cast ingot, then carrying out cogging forging after heat preservation for 3.5 hours at the forging temperature of 1000 ℃, and forging to obtain a zirconium alloy plate blank with the thickness of 110 mm; keeping the temperature of a zirconium alloy plate blank with the thickness of 110 mm at the forging temperature of 800 ℃ for 2 hours, then cogging and forging to obtain a zirconium alloy plate blank with the thickness of 30 mm; performing water quenching on the forged zirconium alloy plate blank at the temperature of 1000 ℃, wherein the zirconium alloy plate blank forms an included angle of 30 ℃ with the water surface when entering water, the transfer time of quenching is 45 seconds, and the water temperature is 30 ℃ before entering water; performing surface machining treatment on the water-quenched zirconium alloy plate blank, wherein the single-side removal amount is 5 mm, and the surface of the plate blank is smooth and is in a metallic color after the treatment; carrying out heat preservation on a zirconium alloy plate blank in a metallic color at the temperature of 600 ℃ for 1 hour, and then carrying out hot rolling to obtain a plate with the thickness of 3 mm, wherein the processing rate of each hot rolling pass is 10-30%, the total processing rate of the hot rolling is 84%, the extension direction of the blank is the length direction of the plate blank in the rolling process, and the temperature of the plate blank is 590 ℃ in the rolling process; preserving the heat of the hot-rolled zirconium alloy plate blank for 2.5 hours at the temperature of 600 ℃, and carrying out atmospheric annealing; carrying out sand blasting and acid washing treatment on the annealed zirconium alloy plate to remove defects such as surface oxide skin, metal and nonmetal pressing and the like, wherein the removing amount is 0.35 mm; cold rolling the zirconium alloy plate subjected to surface treatment on a cold rolling mill from 3 mm to 1.2 mm, wherein the pass deformation is 3-8% and the total deformation is 57%, removing oil from the cold-rolled plate, completely removing oil stains on the surface of the plate, keeping the temperature at 600 ℃ for 2.5 hours, and carrying out vacuum annealing, wherein the vacuum degree of a vacuum annealing furnace is not more than 0.7 x 10 < -2 > Pa; performing strip cold rolling on the zirconium alloy plate subjected to vacuum annealing on a cold rolling mill, wherein the strip is cold-rolled from 1.2 mm to 0.4 mm, the pass deformation is between 1 and 5 percent, and the total deformation is 59 percent; and (3) continuously deoiling and annealing the cold-rolled strip on continuous deoiling and annealing equipment, wherein the annealing temperature is 625 ℃, and the zirconium alloy strip with a uniform structure is prepared after heat preservation for 3 minutes.
Example 2
Cleaning the surface of a zirconium alloy cast ingot, then carrying out cogging forging after keeping the temperature for 4 hours at the forging temperature of 1050 ℃, and forging to obtain a zirconium alloy plate blank with the thickness of 120 mm; keeping the temperature of the zirconium alloy plate blank with the thickness of 120 mm at the forging temperature of 900 ℃ for 2 hours, then cogging and forging to obtain the zirconium alloy plate blank with the thickness of 40 mm; performing water quenching on the forged zirconium alloy plate blank at 1050 ℃, wherein the zirconium alloy plate blank forms an included angle of 60 ℃ with the water surface when entering water, the transfer time of quenching is 41 seconds, and the water temperature is 20 ℃ before entering water; performing surface machining treatment on the zirconium alloy plate blank subjected to water quenching, wherein the single-side removal amount is 5.5 mm, and the surface of the zirconium alloy plate blank is smooth and is in a metal color after treatment; carrying out heat preservation on a zirconium alloy plate blank in a metallic color for 1h at 625 ℃, and then carrying out hot rolling to obtain a plate with the thickness of 3.5 mm, wherein the processing rate of each hot rolling pass is 10-30%, the total hot rolling processing rate is 83%, the extension direction of the blank in the rolling process is the length direction of the zirconium alloy plate blank, the temperature of the zirconium alloy plate blank in the rolling process is 600 ℃, and tempering is carried out for 15 minutes; preserving the heat of the hot-rolled plate blank for 4 hours at the temperature of 625 ℃, and carrying out atmospheric annealing; carrying out sand blasting and acid washing treatment on the annealed zirconium alloy plate to remove defects such as surface oxide skin, metal and nonmetal pressing and the like, wherein the removal amount is 0.4 mm; cold rolling the zirconium alloy plate subjected to surface treatment on a cold rolling mill from 3.5 mm to 1.4 mm, wherein the pass deformation is between 3% and 8%, the total deformation is 60%, removing oil from the cold-rolled zirconium alloy plate, completely removing oil stains on the surface of the plate, keeping the temperature for 2.5 hours at 625 ℃, and performing vacuum annealing, wherein the vacuum degree of a vacuum annealing furnace is not more than 0.8 multiplied by 10 < -2 > Pa; performing strip cold rolling on the zirconium alloy plate subjected to vacuum annealing on a cold rolling mill, and performing cold rolling from 1.4 mm to 0.5 mm, wherein the pass deformation is between 1% and 5%, and the total deformation is 60%; and (3) continuously deoiling and annealing the cold-rolled zirconium alloy strip on continuous deoiling and annealing equipment, wherein the annealing temperature is 700 ℃, and keeping the temperature for 7 minutes to prepare the zirconium alloy strip with uniform structure.
Example 3
Cleaning the surface of a zirconium alloy cast ingot, then carrying out cogging forging after keeping the temperature for 4.5 hours at the forging temperature of 1100 ℃, and forging to obtain a zirconium alloy plate blank with the thickness of 130 mm; performing water quenching on the zirconium alloy plate blank at the temperature of 1100 ℃, wherein the zirconium alloy plate blank forms an included angle of 90 ℃ with the water surface when entering water, the transfer time of quenching is 55 seconds, and the water temperature is 35 ℃ before entering water; performing surface machining treatment on the zirconium alloy plate blank subjected to water quenching, wherein the single-side removal amount is 6 mm, and the surface of the plate blank is smooth and is in a metal color after the treatment; carrying out heat preservation on a metallic zirconium alloy plate blank at the temperature of 650 ℃ for 1 hour, and then carrying out hot rolling to obtain a zirconium alloy plate with the thickness of 4 mm, wherein the processing rate of each hot rolling pass is 10-30%, the total hot rolling processing rate is 89%, the extension direction of the blank in the rolling process is the length direction of the zirconium alloy plate blank, the temperature of the zirconium alloy plate blank in the rolling process is 615 ℃, carrying out tempering, and carrying out tempering and heat preservation for 10 minutes; keeping the temperature of the hot-rolled zirconium alloy plate blank at 650 ℃ for 5 hours, and carrying out atmospheric annealing; carrying out sand blasting and acid washing treatment on the annealed zirconium alloy plate to remove defects such as surface oxide skin, metal and nonmetal pressing and the like, wherein the removing amount is 0.5 mm; cold rolling the zirconium alloy plate subjected to surface treatment on a cold rolling mill from 4 mm to 1.5 mm, wherein the pass deformation is 3-8% and the total deformation is 64%, removing oil from the cold-rolled plate, completely removing oil stains on the surface of the plate, keeping the temperature for 2.5 hours at 650 ℃, and performing vacuum annealing, wherein the vacuum degree of a vacuum annealing furnace is 0.9 multiplied by 10 < -2 > Pa; performing strip cold rolling on the zirconium alloy plate subjected to vacuum annealing on a cold rolling mill, and performing cold rolling from 1.5 mm to 0.6 mm, wherein the pass deformation is between 1% and 5%, and the total deformation is 65%; and (3) continuously deoiling and annealing the cold-rolled zirconium alloy strip on continuous deoiling and annealing equipment, wherein the annealing temperature is 740 ℃, and keeping the temperature for 10 minutes to prepare the zirconium alloy strip with uniform structure.
The zirconium alloy strip prepared by the method is subjected to structure, mechanical property and corrosion performance detection, the mechanical property is shown in table 1 and is obviously about 30 MPa higher than that of the strip produced by the general process, the mechanical property of the strip produced by the general processing process is shown in table 3, the deformation and cracking resistance of the strip is improved, the structure is shown in table 5, 11 grades are obtained according to the ASTME112 standard, and the corrosion performance detection result is shown in table 2.
TABLE 1 results of measurements of the surface physical and chemical properties of zirconium alloy strips prepared by the method
The embodiment provides a process for improving the mechanical property of a zirconium alloy strip, solves the problem of low mechanical property of the conventional zirconium alloy strip, and effectively ensures the grain size grade and the corrosion property of the strip.
The invention aims to protect a zirconium alloy strip processing method which comprises the steps of carrying out first forging treatment on a pretreated zirconium alloy cast ingot in a β phase region to obtain a zirconium alloy forging blank with a first thickness, adjusting the zirconium alloy forging blank to form a preset angle with a liquid level, carrying out quenching treatment at a first temperature to obtain a zirconium alloy plate blank, carrying out surface machining treatment on the zirconium alloy plate blank to obtain a zirconium alloy plate blank with a metallic color, sequentially carrying out rolling and annealing treatment on the zirconium alloy plate blank with the metallic color, and sequentially carrying out hot rolling and cold rolling for at least two times, finally carrying out annealing treatment after the hot rolling and each cold rolling process are finished to obtain a zirconium alloy strip finished product.
In the description of the present invention, it should be noted that the terms "first", "second", and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
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 (13)
1. A zirconium alloy strip processing method, comprising:
performing first forging treatment on the pretreated zirconium alloy ingot in a phase β region to obtain a zirconium alloy forging blank with a first thickness;
adjusting the zirconium alloy forging blank to form a preset angle with the liquid level, and quenching at a first temperature to obtain a zirconium alloy plate blank;
performing surface machining treatment on the zirconium alloy plate blank to obtain a metallic zirconium alloy plate blank;
and sequentially rolling and annealing the zirconium alloy plate blank in the metallic color, and sequentially performing at least two times of hot rolling and at least two times of cold rolling, and finally performing annealing treatment after the hot rolling and each cold rolling process are finished to obtain a zirconium alloy strip finished product.
2. The zirconium alloy strip processing method of claim 1, wherein the step of subjecting the pretreated zirconium alloy ingot to a first forging treatment in the β phase region to obtain a first thickness zirconium alloy forged blank is further followed by the steps of:
and performing second forging treatment on the zirconium alloy forging blank with the first thickness in a phase region of β to obtain a zirconium alloy forging blank with a second thickness.
3. The zirconium alloy strip processing method of claim 2, wherein
The first forging treatment specifically comprises: preserving the heat of the pretreated zirconium alloy ingot for a first time at a second temperature, and cogging and forging to obtain a zirconium alloy forging blank with a first thickness;
the second forging treatment specifically comprises the following steps: and keeping the temperature of the rough blank of the zirconium alloy plate with the first thickness for a second time at a third temperature, and cogging and forging to obtain a forged blank of the zirconium alloy with the second thickness.
4. The zirconium alloy strip processing method of claim 3, wherein
The first thickness is 100-150 mm;
the second thickness is 30-50 mm;
the second temperature is 950-1150 ℃;
the third temperature is 800-1000 ℃;
the first time period is greater than 3.5 hours;
the second time period (T ═ 1.2 xh +30) is divided into 10 hours; t: and (5) keeping the temperature for h, namely the thickness of the plate blank.
5. The zirconium alloy strip processing method of claim 1, wherein
The preset angle is 30-90 degrees;
the first temperature is 950-1150 ℃.
6. The zirconium alloy strip processing method of claim 1, wherein the superfinishing single edge removal is greater than 4 mm.
7. The zirconium alloy strip processing method of claim 1, wherein the rolling and annealing treatments are sequentially performed on the zirconium alloy slab with the metallic color, at least two times of hot rolling and at least two times of cold rolling are sequentially performed, and the final hot rolling and the annealing treatment should be performed after each cold rolling is completed to obtain a finished zirconium alloy strip product, specifically comprising:
carrying out hot rolling treatment on the zirconium alloy plate blank in the metallic color, wherein the total hot rolling processing rate is 80-97%, and obtaining a hot-rolled zirconium alloy plate blank;
carrying out atmospheric annealing on the hot-rolled zirconium alloy plate blank to obtain a zirconium alloy plate;
performing first cold rolling or repeated cold rolling treatment on the zirconium alloy plate for multiple times to obtain a cold-rolled zirconium alloy plate;
welding, coiling and vacuum annealing are carried out on the cold-rolled zirconium alloy plate to obtain a zirconium alloy coiled material;
performing final cold rolling treatment on the zirconium alloy coiled material, wherein the total processing amount after all cold rolling is 45-70%, and obtaining a semi-finished strip;
and carrying out continuous oil removing and annealing treatment on the semi-finished strip to obtain a finished zirconium alloy strip.
8. The zirconium alloy strip processing method of claim 7, wherein the hot rolling treatment is in particular:
keeping the temperature T of a zirconium alloy plate blank in a metallic color at 550-750 ℃ to be 1.2 Xh + 30-1.2 Xh +90 min; t: and (5) keeping the temperature for h, namely the thickness of the plate blank, and then carrying out hot rolling to obtain the hot-rolled zirconium alloy plate blank.
9. The zirconium alloy strip processing method of claim 7, wherein the atmospheric annealing is in particular:
and (3) keeping the temperature T of the hot-rolled zirconium alloy plate blank to be 1.2 Xh + 30-1.2 Xh +90 min at the temperature of 600-750 ℃, wherein h is the stacking thickness of the plate, and carrying out atmospheric annealing.
10. The zirconium alloy strip processing method of claim 7, wherein the vacuum annealing is in particular:
the cold-rolled zirconium alloy plate is kept at the temperature of 600 ℃ for 1.2 Xh +30 min-1.2 Xh +90 min, h is the plateThe thickness of the pile should be greater than 0.9X 10-2Vacuum annealing is carried out under Pa.
11. The zirconium alloy strip processing method according to claim 7, wherein the continuous annealing is in particular:
and carrying out continuous annealing at 625-675 ℃, wherein the speed of the continuous annealing is 0.3-1.5 m/min.
12. The zirconium alloy strip processing method of claim 7, wherein the first cold rolling treatment comprises in particular:
carrying out surface treatment on the zirconium alloy plate, wherein the surface treatment adopts sand blasting and acid pickling, the sand blasting gravel is silicon carbide particles, the acid pickling gravel is mixed solution of hydrofluoric acid, nitric acid and water, and the mixture ratio is 35-45 percent of HNO3+3％～8％HF+H2O, obtaining a zirconium alloy plate with a clean surface;
and carrying out plate type cold rolling on the zirconium alloy plate with the clean surface, welding into coils, carrying out vacuum annealing, and carrying out coil cold rolling to obtain the cold-rolled zirconium alloy strip.
13. A zirconium alloy strip produced by the method of any one of claims 1 to 12.
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| CN112775203A (en) * | 2020-12-23 | 2021-05-11 | 西部新锆核材料科技有限公司 | Preparation method of zirconium or zirconium alloy extruded section |
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| CN103194650A (en) * | 2013-04-10 | 2013-07-10 | 苏州热工研究院有限公司 | Preparation method of Zr-1Nb alloy |
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