CN115518999A - Preparation method of zirconium or zirconium alloy thin-wall square tube - Google Patents

Preparation method of zirconium or zirconium alloy thin-wall square tube Download PDF

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Publication number
CN115518999A
CN115518999A CN202211480926.6A CN202211480926A CN115518999A CN 115518999 A CN115518999 A CN 115518999A CN 202211480926 A CN202211480926 A CN 202211480926A CN 115518999 A CN115518999 A CN 115518999A
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zirconium
raw material
tube
pipe
square tube
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CN115518999B (en
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田航
周军
李宇力
李新意
丁郁航
孙涛涛
马天洋
周宣
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Xi'an Western New Zirconium Technology Co ltd
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Xi'an Western New Zirconium Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C37/00Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
    • B21C37/06Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of tubes or metal hoses; Combined procedures for making tubes, e.g. for making multi-wall tubes
    • B21C37/15Making tubes of special shape; Making tube fittings
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00Energy generation of nuclear origin
    • Y02E30/30Nuclear fission reactors

Abstract

The invention discloses a method for preparing a zirconium or zirconium alloy thin-wall square tube, which comprises the following steps: 1. selecting a zirconium or zirconium alloy seamless circular pipe as a raw material pipe according to the specification of a target product zirconium or zirconium alloy thin-wall square pipe; 2. performing nondestructive flaw detection, straightening and end face flattening on the raw material pipe to obtain a raw material pipe blank; 3. customizing a special hole pattern to roll-bend and form the raw material pipe blank, then rolling to obtain a seamless square pipe, and sawing a U-shaped tail and a debugging section; 4. deoiling, and performing orthopedic heat treatment to obtain the zirconium or zirconium alloy thin-wall square pipe. The invention adopts the high-precision seamless circular tube as the raw material tube and combines the roll bending forming process, overcomes the problems of uneven microstructure, structural strength, surface quality and dimensional precision caused by welding seams generated by welding plates in the existing square tube preparation process, can effectively improve the dimensional precision of the zirconium or zirconium alloy thin-wall square tube only by controlling the dimensional tolerance of the raw material tube, and has the advantages of easy control, flexibility and convenience in the forming process.

Description

Preparation method of zirconium or zirconium alloy thin-wall square tube
Technical Field
The invention belongs to the technical field of material forming, and particularly relates to a preparation method of a zirconium or zirconium alloy thin-wall square tube.
Background
Zirconium or zirconium alloy has good processing performance and very low thermal neutron absorption cross section, and is always used as the preferred material for nuclear reactor cladding tubes and structural components. Meanwhile, because of the excellent acid-base corrosion resistance, zirconium or zirconium alloy plays an important role as a corrosion-resistant part in the chemical industry. Zirconium or zirconium alloy thin-walled square tubes are often used for internal structural members of nuclear reactors, such as zirconium element cassettes. The zirconium element cassettes are the main components of the cryogenic and boiling water reactors, protect the fuel bundle and constitute the fuel assembly coolant channels, and the gaps between every 4 zirconium element cassettes constitute 1 control rod channel. In order to ensure that the fuel assembly is smoothly inserted into the zirconium element box and the control rod can freely move up and down in the whole service life of the reactor, and ensure the safety of the reactor, the surface quality and the dimensional precision of the zirconium element box are strictly required.
At present, the preparation method of the zirconium or zirconium alloy thin-wall square tube mainly takes plates as raw materials, one method is to weld one plate material roll into a round tube and then pre-press, roll or draw the round tube into a square tube, and the other method is to bend two plate materials into a U-shaped square groove and weld the two U-shaped square grooves into a square tube. Patent publication No. CN1050692A discloses a method for manufacturing a zirconium alloy thin-wall square tube, and the patent adopts a method of rolling, welding, stretching and core rod annealing to manufacture the square tube. The patent publication No. CN106623487A discloses a method for preparing a zirconium element box, which adopts a multi-time shape-correcting mode to process the position to be corrected of a square tube, and the preparation method of the square tube is as described above. The square tubes prepared by the above patents all use plates as raw materials, finished products all need to be welded, and one or two welding seams exist, so that the microstructure, the structural strength, the surface quality and the dimensional accuracy are not uniform.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing a zirconium or zirconium alloy thin-wall square tube aiming at the defects of the prior art. The method adopts a high-precision seamless circular tube as a raw material tube and combines a roll bending forming process, overcomes the problems of nonuniform microstructure, structural strength, surface quality and dimensional precision caused by welding seams generated by welding plates in the existing preparation process of the zirconium alloy square tube, effectively improves the dimensional precision of the zirconium or zirconium alloy thin-wall square tube, and is easy to control, flexible and convenient in forming process.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: the preparation method of the zirconium or zirconium alloy thin-wall square tube is characterized by comprising the following steps of:
selecting a zirconium or zirconium alloy seamless circular pipe as a raw material pipe according to the specification of a target product zirconium or zirconium alloy thin-wall square pipe; the thickness, thickness tolerance and perimeter of the raw material pipe are consistent with those of a target product zirconium or zirconium alloy thin-wall square pipe under the condition of reserving surface treatment allowance, the perimeter error of the raw material pipe and the target product zirconium or zirconium alloy thin-wall square pipe is within +/-3 mm, and the raw material pipe is in a complete recrystallization annealing state;
step two, performing nondestructive inspection on the raw material pipe selected in the step one, then straightening the raw material pipe meeting the requirements of nondestructive inspection standards until the straightness is not more than 0.8mm/1000mm, and flattening the end face to obtain a raw material pipe blank;
step three, customizing a special hole pattern according to the specification of a target product, namely a zirconium or zirconium alloy thin-wall square tube, adjusting the number of working racks in roll bending forming equipment, the roll distances and included angles of transverse and longitudinal working rolls and the torsion angles of straightening rolls, then performing roll bending forming on the raw material tube blank obtained in the step two, stopping the machine at any time in the initial roll bending forming stage to measure and observe the size, form tolerance, R angle and torsion condition of the square tube at an outlet, correspondingly debugging the roll distances and included angles of the transverse and longitudinal working rolls and the torsion angles of the straightening rolls according to the measurement and observation results until the appearance meets the design requirements, then rolling according to the debugged parameters to obtain a seamless square tube, and sawing off the head, debugging section and tail part with uneven deformation in the seamless square tube;
fourthly, after the seamless square tube sawn and cut in the third step is subjected to oil removal treatment, performing shape righting heat treatment until the straightness is not more than 0.5mm/1000mm to obtain a zirconium or zirconium alloy thin-wall square tube; the outer side length of the zirconium or zirconium alloy thin-wall square tube ranges from 40mm to 200mm, and the wall thickness ranges from 1mm to 5mm.
According to the specification of a target product, a completely recrystallized and annealed zirconium or zirconium alloy seamless circular tube with thickness, thickness tolerance and perimeter meeting requirements is selected as a raw material tube, nondestructive flaw detection, straightening and end face flattening are sequentially carried out to obtain a raw material tube blank, then the raw material tube blank is subjected to roll bending forming to obtain a seamless square tube, and the seamless square tube is subjected to head and tail cutting and then to oil removal and shape righting heat treatment sequentially to obtain a zirconium or zirconium alloy thin-wall square tube. The invention combines the seamless pipe material with roll bending forming, firstly adopts the rolling, spinning, drawing and other modes to obtain the high-precision seamless pipe material as the raw material pipe, ensures the high-precision requirements of the finished thin-wall square pipe on the wall thickness uniformity and the external dimension, then adopts the roll bending forming mode, utilizes the characteristics of basically unchanged wall thickness and perimeter of the roll bending forming to obtain the seamless square pipe meeting the requirements of the finished product, and overcomes the problems of welding seams generated by welding plates and uneven microstructure, structural strength, surface quality and size precision caused by the welding seams in the existing square pipe preparation process.
In addition, compared with the traditional rolling of the steel square pipe, the method strictly controls the perimeter error between the raw material pipe and the target product zirconium or zirconium alloy thin-wall square pipe to be within +/-3 mm, so that the high precision of the cross section side length, the R angle and the form and position tolerance of the target product zirconium or zirconium alloy thin-wall square pipe is ensured, and the precision of the target product zirconium or zirconium alloy thin-wall square pipe meets the strict requirement of the nuclear field; meanwhile, the nondestructive inspection is carried out on the raw material pipe before the working procedure, the probability of crack extension and expansion in the roll bending forming process is effectively reduced, and the product percent of pass is improved.
In the first step of the present invention, when the selected raw material pipe is in an incompletely recrystallized state, it is necessary to perform a recrystallization heat treatment.
Generally, in the third step of the method, the raw material tube blank is lengthened by welding and then is subjected to roll bending forming, so that the deformation continuity in the roll bending forming process is further ensured, and the preparation efficiency is improved.
Generally, in the fourth step of the invention, the seamless square tube after the orthopedic heat treatment is subjected to internal and external surface treatment, so that the surface of the tube has no color difference and presents metallic luster.
The preparation method of the zirconium or zirconium alloy thin-wall square pipe is characterized in that in the step one, the raw material pipe is a spinning pipe, a rolled pipe or a drawn pipe. According to the invention, the circular tube is selected as the raw material tube, the processing mode of the raw material tube can be rolling, spinning or drawing, the processing advantages of the three processing modes are fully exerted, and different preparation and use requirements are met. Particularly, the spinning tube is adopted to realize high dimensional accuracy, the cost of the tool and the die is low, and the spinning tube is suitable for the production requirements of small batch and multiple specifications; the adoption of the rolled tube breaks through the limit of a tool and a die on the length, is beneficial to cutting off the head and tail ends after the square tube is formed and keeping longer effective length after a debugging section, meets the requirement of multiple scales and improves the yield; and the adoption of the drawing pipe integrates the advantages of low cost, high precision and no limit on the length of the tool and the die.
The preparation method of the zirconium or zirconium alloy thin-wall square pipe is characterized in that the nondestructive flaw detection mode in the step two is ultrasonic flaw detection or hydrostatic test flaw detection. The nondestructive inspection mode of the invention can effectively find longitudinal and transverse damages on the inner and outer surfaces of the raw material pipe, does not damage the circular pipe, and ensures the flexibility of flaw detection.
The preparation method of the zirconium or zirconium alloy thin-wall square pipe is characterized in that in the third step, the number of the special hole patterns is 5 to 8, and the corresponding roll bending forming comprises 5 to 8 passes of continuous deformation. The invention selects proper special hole patterns according to the different target products, further selects the continuous deformation times, and finally reaches the requirements of the size specification and the form and position tolerance of the target product square pipe, thereby being flexible, convenient and easy to adjust. In actual operation, few-pass deformation such as 5-pass deformation is selected for a raw material pipe with low strength and moderate wall thickness to improve the roll bending forming efficiency, and multi-pass deformation such as 8-pass deformation is selected for a raw material pipe with high strength, high thickness and easy irregular deformation to reduce the single-pass deformation.
The preparation method of the zirconium or zirconium alloy thin-wall square tube is characterized in that in the fourth step, the shape-righting heat treatment is carried out by adopting a vertical vacuum annealing furnace depending on dead weight or balance weight, or the inside of the seamless square tube after oil removal treatment is carried out by adopting a combined supporting die and a horizontal vacuum annealing furnace, and the numerical value of the vacuum degree of the shape-righting heat treatment is less than 1 multiplied by 10 -3 Pa, the temperature is 500-700 ℃, and the heat preservation time is 1.5h-3h. The invention adopts the vertical vacuum annealing furnace to carry out the shape righting heat treatment depending on the dead weight or the balance weight, can efficiently correct the bending of the seamless square tube and release the processing stress, is suitable for the shape righting of the processing-state seamless square tube of which the size basically accords with the target product, and preferably adopts a combined supporting die and a horizontal vacuum annealing furnace to carry out the shape righting heat treatment in a heating expansion mode when the size of the processing-state seamless square tube has larger out-of-tolerance or the target product has extremely high requirement on the action tolerance, thereby being beneficial to improving the size precision of the zirconium or zirconium alloy thin-wall square tube.
Compared with the prior art, the invention has the following advantages:
1. the invention adopts the high-precision seamless circular tube as the raw material tube and combines the roll bending forming process, overcomes the problems of uneven microstructure, structural strength, surface quality and dimensional precision caused by welding seams generated by welding plates in the existing square tube preparation process, can effectively improve the dimensional precision of the zirconium or zirconium alloy thin-wall square tube only by controlling the dimensional tolerance of the raw material tube, and has the advantages of easy control, flexibility and convenience in the forming process.
2. Compared with the traditional forming modes such as bending welding and the like, the roll bending forming process can realize continuous production after equipment is debugged, and generally thousands of square pipes can be produced by a single device every day, so that the yield and the productivity of the zirconium or zirconium alloy thin-wall square pipes are greatly improved.
3. The invention adopts a spinning pipe, a rolled pipe or a drawn pipe as a raw material pipe, and matches circular pipe processing modes such as spinning, rolling, drawing and the like, so that the advantages of different circular pipe preparation modes are fully exerted, and the production of the zirconium or zirconium alloy thin-wall square pipe under different requirements is met.
4. Compared with the prior art that the steel square pipe is mainly used for buildings and vehicles, has low requirements on dimensional accuracy and is mostly a welded pipe, the invention adopts a high-accuracy raw material pipe, strictly controls the section perimeter of the raw material pipe, finely debugs process parameters in the roll bending forming process, and rolls according to the debugging result, thereby greatly improving the dimensional accuracy of the zirconium or zirconium alloy thin-wall square pipe.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1a is a schematic end view of a Zr-4 thin-walled square tube prepared in example 1 of the present invention.
FIG. 1b is a schematic side view of a Zr-4 thin-walled square tube prepared in example 1 of the present invention.
FIG. 2 is a metallographic structure drawing of a thin-walled square tube of Zr-Sn-Nb-Fe alloy prepared in example 2 of the present invention.
FIG. 3 is a side view of a Zr-2.5Nb alloy thin-walled square tube subjected to oil removal treatment in example 3 of the present invention.
Detailed Description
Example 1
The embodiment comprises the following steps:
selecting a Zr-4 seamless circular tube as a raw material tube according to the specification of a target product Zr-4 thin-wall square tube; the specification of the target product Zr-4 thin-wall square tube is that the side length of the cross section is 40mm, the wall thickness is 2mm, the length is 3000mm, and the R angle is 3.5mm, the principle that the perimeter and the wall thickness are not changed before and after roll bending forming is considered, and the subsequent pickling allowance is combined, the size (the outer diameter is multiplied by the wall thickness and the length) of a raw material tube Zr-4 seamless circular tube is selected to be phi 58mm multiplied by 2.05mm multiplied by 6800mm (double ruler), wherein the length of the raw material tube is 800mm larger than the double size of the target product Zr-4 thin-wall square tube, and the raw material tube is reserved as a head and tail cutting section and a debugging section; the Zr-4 seamless circular tube of the raw material tube is a rolled tube with small diameter and long length, and recrystallization annealing treatment is carried out after rolling forming to ensure that the tube is in a complete recrystallization annealing state;
step two, performing nondestructive flaw detection on the Zr-4 seamless circular tube of the raw material tube selected in the step one, performing acid washing treatment on the inner surface and the outer surface of the Zr-4 seamless circular tube of the raw material tube exceeding the standard flaw until the standard flaw requirement is met, straightening the Zr-4 seamless circular tube of the raw material tube meeting the standard flaw requirement until the straightness is not more than 0.8mm/1000mm, and flattening the end face to obtain a Zr-4 tube blank; the nondestructive inspection is ultrasonic inspection, the standard flaw is a U-shaped flaw, the depth is 0.2 +/-0.02 (mm), the width is 0.4 +/-0.04 (mm), and the length is 3 +/-0.3 (mm);
step three, considering that the strength of a target product Zr-4 thin-wall square pipe is moderate and the wall thickness is moderate, customizing 5 special hole patterns, adjusting the number of working racks, the roll distances and the included angles of transverse and longitudinal working rolls and the torsion angles of straightening rolls in roll bending forming equipment, then carrying out 5-pass roll bending forming on the Zr-4 pipe blank obtained in the step two, stopping the machine at any time in the initial stage of roll bending forming to measure and observe the size, form tolerance, R angle and torsion conditions of the square pipe at an outlet, correspondingly debugging the roll distances and the included angles of the transverse and longitudinal working rolls and the torsion angles of the straightening rolls according to the measurement and observation results, stopping debugging until the appearance meets the design requirements, so that the four sides of the pipe are flat and the R angle is uniform, then rolling is carried out according to the debugged parameters to obtain a seamless Zr-4 square pipe, and sawing off the head, debugging section and tail which are not uniform in the seamless Zr-4 square pipe;
step four, deoiling the sawed seamless Zr-4 square tube in the step three, and then performing orthopedic heat treatment, specifically, punching the top of the seamless Zr-4 square tube by using a vertical vacuum annealing furnace and relying on a balance weight, hanging the seamless Zr-4 square tube on a material rack, punching the bottom of the seamless Zr-4 square tube and adding a heavy object, wherein the value of the vacuum degree of the orthopedic heat treatment is less than 1 x 10 -3 Pa, at 630 deg.C for 1.5h, performing inner and outer surface pickling with HNO as pickling solution 3 The solution and HF solution, obtaining Zr-4 thin-wall square tube with the outer side length of 40mm and the wall thickness of 2mm, as shown in figure 1a and figure 1 b.
Through detection, the surface roughness Ra of the Zr-4 thin-wall square tube prepared by the embodiment is less than 0.5 mu m, the wall thickness deviation is consistent with that of a raw material tube, the straightness is not more than 0.5mm/1000mm, the grain size reaches 12 grades, the tensile strength is more than 400MPa, the yield strength is more than 300MPa, and the use requirement is completely met.
Example 2
The embodiment comprises the following steps:
selecting a Zr-Sn-Nb-Fe alloy seamless circular tube as a raw material tube according to the specification of a target product Zr-Sn-Nb-Fe alloy thin-wall square tube; the target product Zr-Sn-Nb-Fe alloy thin-wall square tube is characterized in that the side length of the cross section is 70mm, the wall thickness is 1mm, the length is 4500mm, and the R angle is 2.5mm, the principle that the perimeter and the wall thickness are not changed before and after roll bending forming is considered and the subsequent pickling allowance is combined, the size (the outer diameter multiplied by the wall thickness multiplied by the length) of a Zr-Sn-Nb-Fe alloy seamless circular tube of a raw material tube is phi 94mm multiplied by 1.05mm multiplied by 5300mm, wherein the length of the raw material tube is 800mm larger than that of the target product Zr-Sn-Nb-Fe alloy thin-wall square tube and is reserved as a head and tail cutting and debugging section; the Zr-Sn-Nb-Fe alloy seamless circular tube of the raw material tube is a rolled tube with a small diameter and a long length, and is subjected to recrystallization annealing treatment after being rolled and formed to be in a complete recrystallization annealing state;
step two, performing nondestructive flaw detection on the Zr-Sn-Nb-Fe alloy seamless circular tube of the raw material tube selected in the step one, performing inner surface honing and outer surface polishing treatment on the Zr-Sn-Nb-Fe alloy seamless circular tube of the raw material tube exceeding the standard flaw until the Zr-Sn-Nb-Fe alloy seamless circular tube meets the standard flaw requirement, straightening the Zr-Sn-Nb-Fe alloy seamless circular tube of the raw material tube meeting the standard flaw requirement until the straightness is not more than 0.8mm/1000mm, and flattening the end surface to obtain a Zr-Sn-Nb-Fe alloy tube blank; the nondestructive inspection is ultrasonic inspection, the standard flaw is a U-shaped flaw, the depth is 0.1 +/-0.01 (mm), the width is 0.2 +/-0.02 (mm), and the length is 3 +/-0.3 (mm);
step three, considering that the target product Zr-Sn-Nb-Fe alloy thin-wall square tube has high strength and thin wall thickness, customizing 8 pairs of special hole patterns, adjusting the number of working frames, the roll distances and included angles of transverse and longitudinal working rolls and the torsion angles of straightening rolls in roll bending forming equipment, then carrying out 8-pass roll bending forming on the Zr-Sn-Nb-Fe alloy tube blank obtained in the step two, stopping the machine at the initial stage of roll bending forming to measure and observe the size, form and position tolerance, R angle and torsion conditions of the square tube at an outlet, correspondingly debugging the roll distances and included angles of the transverse and longitudinal working rolls and the torsion angles of the straightening rolls according to the measurement and observation results until the shape meets the design requirements, stopping debugging to enable the four sides of the tube to be smooth and the R angle to be uniform, then rolling according to the debugged parameters to obtain a seamless Zr-Sn-Nb-Fe alloy square tube, and sawing off the head, debugging section and tail of the seamless Zr-Sn-Nb-Fe alloy square tube with non-uniform deformation;
step four, deoiling the sawed seamless Zr-Sn-Nb-Fe alloy square tube in the step three, and then carrying out orthopedic heat treatment, specifically, carrying out orthopedic heat treatment by using a combined supporting die and a horizontal vacuum annealing furnace in the interior of the seamless Zr-Sn-Nb-Fe alloy square tube after the deoiling treatment, wherein the vacuum degree value of the orthopedic heat treatment is less than 1 x 10 -3 Pa, 580 deg.C, holding for 2.5h, performing inner and outer surface pickling with HNO as pickling solution 3 The solution and the HF solution are mixed to obtain the Zr-Sn-Nb-Fe alloy thin-wall square tube with the outer side length of 70mm and the wall thickness of 1 mm.
Through detection, the surface roughness Ra of the Zr-Sn-Nb-Fe alloy thin-wall square tube prepared by the embodiment is less than 0.5 mu m, the wall thickness deviation is consistent with that of a raw material tube, the straightness is not more than 0.5mm/1000mm, the grain size reaches 12.5 grade, the tensile strength is more than 420MPa, the yield strength is more than 330MPa, and the use requirement is completely met.
Fig. 2 is a metallographic structure diagram of the Zr-Sn-Nb-Fe alloy thin-walled square tube prepared in this example, and it can be seen from fig. 2 that the Zr-Sn-Nb-Fe alloy thin-walled square tube obtained by rolling the Zr-Sn-Nb-Fe alloy seamless circular tube into a square tube is still in a completely recrystallized state, the grain size reaches 12.5 level, and the Zr-Sn-Nb-Fe alloy thin-walled square tube has no obvious difference from the Zr-Sn-Nb-Fe alloy seamless circular tube, has no processing structure, and is beneficial to the performance stability of the Zr-Sn-Nb-Fe alloy thin-walled square tube in subsequent use.
Example 3
The embodiment comprises the following steps:
step one, selecting a Zr-2.5Nb alloy seamless circular tube as a raw material tube according to the specification of a target product Zr-2.5Nb alloy thin-wall square tube; the target product Zr-2.5Nb alloy thin-wall square tube is specified as that the side length of the cross section is 120mm, the wall thickness is 3.2mm, the length is 3000mm, and the R angle is 5.5mm, the principle that the perimeter and the wall thickness are not changed before and after roll bending forming is considered, and the subsequent pickling allowance is combined, the size (the outer diameter multiplied by the wall thickness multiplied by the length) of a Zr-2.5Nb alloy seamless circular tube of a raw material tube is selected to be phi 163.8mm multiplied by 3.25mm multiplied by 4300mm, wherein the length of the raw material tube is 800mm larger than that of the target product Zr-2.5Nb alloy thin-wall square tube, and the raw material tube is reserved as a head and tail cutting and a debugging section; the raw material tube Zr-2.5Nb alloy seamless circular tube is a drawn tube with a larger diameter and a longer length, and is subjected to recrystallization annealing treatment after being drawn and formed to be in a complete recrystallization annealing state;
secondly, performing nondestructive flaw detection on the Zr-2.5Nb alloy seamless circular tube of the raw material tube selected in the first step, straightening the Zr-2.5Nb alloy seamless circular tube of the raw material tube meeting the requirements of nondestructive flaw detection standards until the straightness is not more than 0.8mm/1000mm, and flattening the end face to obtain a Zr-2.5Nb alloy tube blank; the nondestructive testing is hydrostatic testing, the testing pressure is 26MPa to 28MPa, the pressure maintaining time is more than 30s, the Zr-2.5Nb alloy seamless circular tube has no water leakage and bulge during the pressure maintaining period, and the pressure drop during the pressure maintaining period is not more than 1MPa;
step three, considering that the target product Zr-2.5Nb alloy thin-wall square tube has high strength and moderate wall thickness, customizing 8 pairs of special hole patterns, adjusting the number of working frames, the roll spacing and the included angle of transverse and longitudinal working rolls and the torsion angle of a straightening roll in roll bending forming equipment, then carrying out 8-pass roll bending forming on the Zr-2.5Nb alloy tube blank obtained in the step two, stopping the machine at the initial stage of roll bending forming to measure and observe the size, the form and position tolerance, the R angle and the torsion condition of the square tube at an outlet, correspondingly debugging the roll spacing and the included angle of the transverse and longitudinal working rolls and the torsion angle of the straightening roll according to the measurement and observation results, stopping debugging until the shape meets the design requirements, so that the four sides of the tube are smooth and the R angle is uniform, then rolling according to the debugged parameters to obtain a seamless Zr-2.5Nb alloy square tube, and sawing off the head, the debugging section and the tail which are not uniform in the seamless Zr-2.5Nb alloy square tube, as shown in figure 3;
step four, deoiling the sawed seamless Zr-2.5Nb alloy square tube in the step three, and then carrying out shape-righting heat treatment, specifically, punching the upper end of the seamless Zr-2.5Nb alloy square tube and hanging the upper end on a material rack by using a vertical vacuum annealing furnace and relying on self weight, wherein the vacuum degree value of the shape-righting heat treatment is less than 1 multiplied by 10 -3 Pa, 700 ℃ and 3h of heat preservation time, and then carrying out acid washing on the inner surface and the outer surface, wherein the acid washing solution adopted by the acid washing is HNO 3 The solution and HF solution are mixed to obtain the Zr-2.5Nb alloy thin-wall square tube with the outer side length of 120mm and the wall thickness of 3.2 mm.
Through detection, the surface roughness Ra of the Zr-2.5Nb alloy thin-wall square tube prepared by the embodiment is less than 0.5 mu m, the wall thickness deviation is consistent with that of a raw material tube, the straightness does not exceed 0.6mm/1000mm, the grain size reaches 12 grades, the tensile strength is more than 500MPa, the yield strength is more than 400MPa, and the use requirement is completely met.
Example 4
The embodiment comprises the following steps:
selecting a Zr-1Nb alloy seamless circular tube as a raw material tube according to the specification of a target product Zr-1Nb alloy thin-wall square tube; the specification of the target product Zr-1Nb alloy thin-wall square tube is that the cross section side length is 150mm, the wall thickness is 4mm, the length is 1500mm, and the R angle is 7mm, the principle that the perimeter and the wall thickness are not changed before and after roll bending forming is considered, the subsequent pickling allowance is combined, the size (the outer diameter is multiplied by the wall thickness and multiplied by the length) of a Zr-1Nb alloy seamless circular tube of a raw material tube is selected to be phi 205mm multiplied by 4.05mm multiplied by 2000mm, wherein the length of the raw material tube is 500mm larger than that of the target product Zr-1Nb alloy thin-wall square tube and is reserved as a head-tail cutting and debugging section; the Zr-1Nb alloy seamless circular tube as the raw material tube is a spinning tube with larger diameter and shorter length, and recrystallization annealing treatment is carried out after spinning forming to ensure that the tube is in a complete recrystallization annealing state;
step two, performing nondestructive flaw detection on the Zr-1Nb alloy seamless circular tube of the raw material tube selected in the step one, performing acid pickling treatment on the inner surface and the outer surface of the Zr-1Nb alloy seamless circular tube of the raw material tube exceeding the nondestructive flaw detection standard until the standard flaw detection requirement is met, straightening the Zr-1Nb alloy seamless circular tube of the raw material tube meeting the nondestructive flaw detection standard requirement until the straightness is not more than 0.8mm/1000mm, and flattening the end face to obtain a Zr-1Nb alloy tube blank; the nondestructive inspection is manual ultrasonic inspection, the standard flaw is a U-shaped flaw, the depth is 0.4 +/-0.04 (mm), the width is 0.2 +/-0.02 (mm), and the length is 2 +/-0.2 (mm);
thirdly, welding and lengthening the Zr-1Nb alloy pipe blanks obtained in the two steps by adopting argon arc welding and fixing the Zr-1Nb alloy pipe blanks through a special tool, ensuring that the straightness of the welded and lengthened Zr-1Nb alloy pipe blanks does not exceed 1mm/1000mm, considering that the Zr-1Nb alloy thin-wall square pipe as a target product has low strength and moderate wall thickness, customizing 6 pairs of special hole patterns, adjusting the number of working frames, the roll distances and included angles of transverse and longitudinal working rolls and the torsion angle of a straightening roll in roll bending forming equipment, then carrying out 6-pass roll bending forming on the welded and lengthened Zr-1Nb alloy pipe blanks, stopping debugging at any time in the initial stage of roll bending forming to measure and observe the size, deformation tolerance, R angle and torsion condition of the outlet square pipe, correspondingly debugging the roll distances and included angles of the transverse and longitudinal working rolls and the torsion angle of the straightening roll according to the measurement and observation results until the appearance meets the design requirements, so that the four sides of the pipe fittings are smooth and the R angle are uniform, then carrying out seamless rolling according to obtain the seamless rolling of the Zr-1Nb alloy pipe blanks after debugging, and removing the head and the uneven sections of the Zr-1Nb alloy welded and the lengthened square pipe blanks;
step four, deoiling the sawed seamless Zr-1Nb alloy square tube in the step three, and then carrying out shape-righting heat treatment, specifically, a vertical vacuum annealing furnace is adopted to be based on dead weight and counterweight, the upper end of the seamless Zr-1Nb alloy square tube is punched and hung on a material rack, the bottom of the seamless Zr-1Nb alloy square tube is punched and hung with a counterweight, and the value of the vacuum degree of the shape-righting heat treatment is less than 1 multiplied by 10 -3 Pa, the temperature is 550 ℃, the heat preservation time is 2h, then the inner and outer surfaces are pickled, the pickling solution adopted by the pickling is HNO 3 The solution and HF solution are mixed to obtain the Zr-1Nb alloy thin-wall square tube with the outer side length of 150mm and the wall thickness of 4 mm.
Through detection, the surface roughness Ra of the Zr-1Nb alloy thin-wall square tube prepared by the embodiment is less than 0.5 mu m, the wall thickness deviation is consistent with that of a raw material tube, the straightness does not exceed 0.5mm/1000mm, the grain size reaches 13 grades, the tensile strength is greater than 480MPa, the yield strength is greater than 280MPa, and the use requirement is completely met.
Example 5
The embodiment comprises the following steps:
selecting a Zr702 alloy seamless circular tube as a raw material tube according to the specification of a target product Zr702 alloy thin-wall square tube; the specification of the target product Zr702 alloy thin-wall square tube is 200mm in side length of a cross section, 5mm in wall thickness, 1300mm in length and 8.5mm in R angle, the principle that the circumference and the wall thickness are not changed before and after roll bending forming is considered, the subsequent pickling allowance is combined, the size (outer diameter multiplied by the wall thickness multiplied by the length) of a Zr702 alloy seamless circular tube of a raw material tube is selected to be phi 271.6mm multiplied by 5.05mm multiplied by 1800mm, wherein the length of the raw material tube is 500mm larger than that of the target product Zr702 alloy thin-wall square tube and is reserved as a head and tail cutting and debugging section; the raw material tube Zr702 alloy seamless circular tube is a spinning tube with a larger diameter and a shorter length, and is subjected to recrystallization annealing treatment after rolling forming to be in a complete recrystallization annealing state;
step two, performing nondestructive inspection on the Zr702 alloy seamless circular tube of the raw material tube selected in the step one, performing acid washing treatment on the inner surface and the outer surface of the Zr702 alloy seamless circular tube of the raw material tube exceeding the nondestructive inspection standard until the Zr702 alloy seamless circular tube meets the nondestructive inspection standard requirement, straightening the Zr702 alloy seamless circular tube of the raw material tube meeting the nondestructive inspection standard requirement until the straightness is not more than 0.8mm/1000mm, and flattening the end surface to obtain a Zr702 alloy tube blank; the nondestructive inspection is manual ultrasonic inspection, the standard flaw is a U-shaped flaw, the depth is 0.5 +/-0.05 (mm), the width is 0.4 +/-0.04 (mm), and the length is 3 +/-0.3 (mm);
thirdly, welding and lengthening the Zr702 alloy pipe blanks obtained in the two second steps by adopting argon arc welding and fixing the Zr702 alloy pipe blanks through a special tool, ensuring that the straightness of the welded and lengthened Zr702 alloy pipe blanks does not exceed 0.8mm/1000mm, considering that the Zr702 alloy thin-wall square pipe is low in strength and moderate in wall thickness as a target product, customizing 6 pairs of special hole patterns, adjusting the number of working frames, the roll distances and the included angles of transverse and longitudinal working rolls and the torsion angles of straightening rolls in roll bending forming equipment, then carrying out 6-pass roll bending forming on the welded and lengthened Zr702 alloy pipe blanks, stopping the machine at any time at the initial stage of roll bending forming to measure and observe the size, form and position tolerance, the R angle and the torsion conditions of the outlet square pipe, correspondingly adjusting the roll distances and the included angles of the transverse and longitudinal working rolls and the torsion angles of the straightening rolls according to the measurement and observation results, stopping the adjustment until the appearance meets the design requirements, so that the four sides of the pipe fittings are flat and the R angle is uniform, then rolling is carried out to obtain seamless Zr702 alloy square pipe blanks, and cutting off the head and tail parts of the seamless Zr alloy pipe blanks, and the welded and the uneven sections;
step four, deoiling the sawn seamless Zr702 alloy square tube in the step three, and then carrying out orthopedic heat treatment, specifically, a vertical vacuum annealing furnace is adopted to be carried out by depending on a counterweight, the upper end of the seamless Zr702 alloy square tube is punched and hung on a material rack, the bottom of the seamless Zr702 alloy square tube is punched and hung with a counterweight, and the numerical value of the vacuum degree of the orthopedic heat treatment is less than 1 multiplied by 10 -3 Pa, 500 ℃ and the heat preservation time of 2.5h, then carrying out acid cleaning on the inner surface and the outer surface, wherein the acid cleaning solution adopted by the acid cleaning is HNO 3 The solution and the HF solution are mixed to obtain the Zr702 alloy thin-wall square tube with the outer side length of 200mm and the wall thickness of 5mm.
Through detection, the surface roughness Ra of the Zr702 alloy thin-wall square tube prepared by the embodiment is less than 0.5 mu m, the wall thickness deviation is consistent with that of a raw material tube, the straightness does not exceed 0.5mm/1000mm, the grain size reaches 11 grade, the tensile strength is greater than 400MPa, the yield strength is greater than 210MPa, and the use requirement is completely met.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modifications, alterations and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.

Claims (5)

1. The preparation method of the zirconium or zirconium alloy thin-wall square tube is characterized by comprising the following steps of:
selecting a zirconium or zirconium alloy seamless round pipe as a raw material pipe according to the specification of a target product, namely a zirconium or zirconium alloy thin-wall square pipe; the thickness, thickness tolerance and perimeter of the raw material pipe are consistent with those of a target product zirconium or zirconium alloy thin-wall square pipe under the condition of reserving surface treatment allowance, the perimeter error of the raw material pipe and the target product zirconium or zirconium alloy thin-wall square pipe is within +/-3 mm, and the raw material pipe is in a complete recrystallization annealing state;
step two, performing nondestructive inspection on the raw material pipe selected in the step one, then straightening the raw material pipe meeting the requirements of nondestructive inspection standards until the straightness is not more than 0.8mm/1000mm, and flattening the end face to obtain a raw material pipe blank;
step three, customizing a special hole pattern according to the specification of a target product, namely a zirconium or zirconium alloy thin-wall square tube, adjusting the number of working racks in roll bending forming equipment, the roll distances and included angles of transverse and longitudinal working rolls and the torsion angles of straightening rolls, then performing roll bending forming on the raw material tube blank obtained in the step two, stopping the machine at any time in the initial roll bending forming stage to measure and observe the size, form tolerance, R angle and torsion condition of the square tube at an outlet, correspondingly debugging the roll distances and included angles of the transverse and longitudinal working rolls and the torsion angles of the straightening rolls according to the measurement and observation results until the appearance meets the design requirements, then rolling according to the debugged parameters to obtain a seamless square tube, and sawing off the head, debugging section and tail part with uneven deformation in the seamless square tube;
fourthly, after the seamless square tube sawn and cut in the third step is subjected to oil removal treatment, performing shape righting heat treatment until the straightness is not more than 0.5mm/1000mm to obtain a zirconium or zirconium alloy thin-wall square tube; the outer side length of the zirconium or zirconium alloy thin-wall square tube ranges from 40mm to 200mm, and the wall thickness ranges from 1mm to 5mm.
2. The method according to claim 1, wherein the raw material pipe in the first step is a spun pipe, a rolled pipe or a drawn pipe.
3. The method for manufacturing thin-walled square tubes of zirconium or zirconium alloy according to claim 1, wherein the nondestructive inspection in the second step is ultrasonic inspection or hydrostatic test inspection.
4. The method for manufacturing the zirconium or zirconium alloy thin-walled square tube according to claim 1, wherein the number of the special hole patterns in the third step is 5 to 8, and the corresponding roll bending forming comprises 5 to 8 passes of continuous deformation.
5. The method for preparing thin-walled square tubes of zirconium or zirconium alloy according to claim 1, wherein the step four isThe shape-righting heat treatment is carried out by a vertical vacuum annealing furnace depending on dead weight or balance weight, or the interior of the seamless square tube after the oil removal treatment is carried out by using a combined supporting mould and a horizontal vacuum annealing furnace, and the numerical value of the vacuum degree of the shape-righting heat treatment is less than 1 multiplied by 10 -3 Pa, the temperature is 500-700 ℃, and the heat preservation time is 1.5h-3h.
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