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CN113385624A - Preparation process of high-performance zirconium alloy die forging - Google Patents

Preparation process of high-performance zirconium alloy die forging Download PDF

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Publication number
CN113385624A
CN113385624A CN202110509087.5A CN202110509087A CN113385624A CN 113385624 A CN113385624 A CN 113385624A CN 202110509087 A CN202110509087 A CN 202110509087A CN 113385624 A CN113385624 A CN 113385624A
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blank
diameter end
zirconium
preparation
preparation process
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CN113385624B (en
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孙敏
段晓辉
孙子城
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Baoji Yixin Metals Product Works
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Baoji Yixin Metals Product Works
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21JFORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J5/00Methods for forging, hammering, or pressing; Special equipment or accessories therefor
    • B21J5/002Hybrid process, e.g. forging following casting
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21HMAKING PARTICULAR METAL OBJECTS BY ROLLING, e.g. SCREWS, WHEELS, RINGS, BARRELS, BALLS
    • B21H1/00Making articles shaped as bodies of revolution
    • B21H1/06Making articles shaped as bodies of revolution rings of restricted axial length
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/03Making non-ferrous alloys by melting using master alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C16/00Alloys based on zirconium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing 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
    • C22F1/18High-melting or refractory metals or alloys based thereon
    • C22F1/186High-melting or refractory metals or alloys based thereon of zirconium or alloys based thereon
    • 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

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  • Crystallography & Structural Chemistry (AREA)
  • Forging (AREA)

Abstract

The invention discloses a preparation process of a high-performance zirconium alloy die forging, which comprises the steps of material preparation, ingot preparation, forging, cylindrical boss blank preparation, punching, ring grinding and hole expanding and annealing. And in the mechanical preparation process, a preparation die and a ring rolling die are selected to prepare the finished die forging. The preparation process comprises the steps of strictly controlling the material selection and further controlling the weight ratio of each raw material to prepare a high-performance zirconium alloy die forging blank, specifically preparing the zirconium alloy die forging with high precision size by a multistep preparation method and adopting different dies, and effectively limiting deformation bulges on two side walls of the dies in the process of rolling and deforming the intermediate blank by the rolling dies so as to gradually reduce the wall thickness of the intermediate blank, further limiting and avoiding the deformation state of the side walls of the intermediate blank under the external rolling force, avoiding the operation and difficulty of repairing the intermediate blank again in the later period after the deformation bulges, and reducing the influence of deformation on the mechanical property of a finished product.

Description

Preparation process of high-performance zirconium alloy die forging
Technical Field
The invention relates to the technical field of zirconium alloy preparation, in particular to a preparation process of a high-performance zirconium alloy die forging.
Background
An alloy is a metallic material having metallic characteristics formed by alloying (melting, mechanical alloying, sintering, vapor deposition, etc.) two or more metallic elements or other non-metallic elements added on a metallic basis. Different metal elements and different preparation processes can prepare alloy finished products with various physical characteristics so as to meet the use requirements under different environments.
Zirconium element easily absorbs hydrogen, nitrogen and oxygen, has strong affinity to oxygen, and has the advantages of good corrosion resistance and plasticity, easy processing and the like. Zirconium absorbs a large amount of gas such as oxygen, hydrogen, and nitrogen when heated, and is useful as a hydrogen storage material. The zirconium alloy is a non-ferrous alloy formed by adding other elements by taking zirconium as a matrix. The main alloy elements include tin, niobium, iron, etc. The zirconium alloy has good corrosion resistance and moderate mechanical property in high-temperature and high-pressure water and steam at the temperature of 300-400 ℃. After the zirconium alloy is prepared into the die forging, the overall mechanical property of the zirconium alloy die forging is further reduced due to the applied force of mechanical processing.
Disclosure of Invention
Aiming at the existing problems, the invention aims to provide a preparation process of a high-performance zirconium alloy die forging, which comprises two steps of blank preparation and mechanical forming preparation, and improves the mechanical property of the original alloy on the basis of more characteristic advantages of the original alloy, thereby integrally improving the excellent performance of the blank prepared from the zirconium alloy. And in the process of preparing the die forging piece by mechanical forming, the deformation of the die forging blank is effectively reduced, so that the mechanical property equivalent to that of the prepared blank is ensured.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: the preparation process of the high-performance zirconium alloy die forging is characterized by comprising the following steps of:
s1, preparing the ingredients
Selecting sponge zirconium with the O content of less than or equal to 0.05 percent and the Fe content of less than or equal to 0.05 percent, zirconium oxide, zirconium-niobium alloy and iron nails, wherein the weight ratio of the sponge zirconium to the zirconium oxide to the zirconium-niobium alloy is 96-97 percent, the zirconium oxide to the zirconium-niobium alloy is 0.4-0.6 percent, the zirconium-niobium alloy is 2.5-3.5 percent and the iron nails are 0.05-0.06 percent;
s2, preparing cast ingot
The sponge zirconium, the zirconia, the zirconium-niobium alloy and the iron nail are mixed according to the weight ratio and then melted into the specification of
Figure BDA0003059600370000021
The cast ingot has the O content of 0.14 to 0.16 percent and the Fe content of 0.08 to 0.1 percent;
s3 forging
First-stage forging: heating the cast ingot to 1010-1030 ℃, preserving heat for 360-400 min, shaping to □ 500 × 900mm by adopting a quick forging machine, upsetting to 500mm height along the length direction, reversely drawing to □ 500 × 900mm, circularly performing three times of upsetting and drawing, and finally rounding to 35500 × 900mm
Figure BDA0003059600370000022
Obtaining a fire blank;
forging with two heats: charging the first-fire blank into a furnace, heating to 830-850 ℃, preserving heat for 360-400 min, upsetting to 500mm high at 800mm, then drawing to 800mm high along the original direction, circularly upsetting for three times in the way, and finally forming to □ 350 multiplied by 1850mm to obtain a second-fire blank;
forging with three heats: grinding and heating the blank of the second fire to 820-830 ℃, and then shaping to
Figure BDA0003059600370000023
Obtaining an initial blank;
s4, preparing a cylindrical boss blank
Selecting a preparation die to upset the initial blank to a small-diameter end
Figure BDA0003059600370000024
The large diameter end is
Figure BDA0003059600370000031
The cylindrical boss blank;
s5, punching
Heating the cylindrical boss blank to 820 ℃, tempering and preserving heat for 120-150 min, and punching
Figure BDA0003059600370000032
And finally reaming by using a punching core to
Figure BDA0003059600370000033
While obtaining a small diameter end of
Figure BDA0003059600370000034
The large diameter end is
Figure BDA0003059600370000035
The intermediate blank of (3);
s6 reaming of grinding ring
Heating the intermediate blank to 810-820 ℃, and adopting a vertical ring rolling machine with a ring rolling die (1) matched with the intermediate blank to roll the intermediate blank
Figure BDA0003059600370000036
To the middle hole
Figure BDA0003059600370000037
While obtaining a small diameter end of
Figure BDA0003059600370000038
The large diameter end is
Figure BDA0003059600370000039
The finished blank of (1);
s7 annealing
Heating the finished blank to 650-680 ℃, preserving heat for 120-150 min, discharging and air cooling to a finished product state.
Preferably, in step S4, the preparation mold is provided with a small diameter end matching the cylindrical boss blank
Figure BDA00030596003700000310
And a height of 77mm, and a fitting large-diameter end
Figure BDA00030596003700000311
The outer diameter of the cylindrical tube.
Preferably, the fixed cover of ring rolling mould is established on the main roll of vertical ring rolling machine, the ring rolling mould have in proper order cooperate with the first ring rolling portion and the second ring rolling portion of the global contact of little diameter end and major diameter end of middle blank to the width of first ring rolling portion and second ring rolling portion in proper order with the height of the little diameter end and the major diameter end of middle blank equals.
Preferably, before the intermediate blank is rolled to the finished blank, deformation preventing devices for preventing the intermediate blank from axially deforming at the small-diameter end and the large-diameter end under the external rolling force are arranged at both sides of the intermediate blank.
Preferably, the deformation preventing device comprises shaft sleeves which are symmetrically and rotatably sleeved on the central shafts on two sides of the middle blank, each shaft sleeve is provided with a central shaft perpendicular to the central shafts, the central shafts on two sides are sequentially provided with a first compression roller and a second compression roller which are attached to the outer wall of the small-diameter end and the outer wall of the large-diameter end of the middle blank and rotate, and the lengths of the first compression roller and the second compression roller are sequentially greater than the heights of the small-diameter end and the large-diameter end of the middle blank.
Preferably, the main rollers on two sides of the ring rolling die are also rotatably sleeved with shaft sleeves, and the shaft sleeves are provided with limiting rods which move along the length direction of the central shaft, penetrate through the central shaft and are used for limiting the first compression roller and the second compression roller to rotate around the central shaft.
Preferably, the end faces of the first pressing roller and the second pressing roller, which are close to the mandrel, are both set to be arc faces containing the shaft sleeves at close positions, and in the containing state, the side edge faces of the first pressing roller and the second pressing roller, which are close to the mandrel, are close to the circumferential face of the mandrel.
Preferably, the part of the mandrel, which is in contact with the middle hole of the intermediate blank, is a first stage, the parts on two sides of the first step section are second stages, the diameter of the first stage is larger than that of the second stage, and the side end face side lines of the first pressing roller and the second pressing roller, which are close to the mandrel, are overlapped with the two side faces of the first stage.
The invention has the beneficial effects that: the preparation process is characterized in that the blank of the zirconium alloy die forging with high performance is prepared by strictly controlling the material selection and further controlling the weight ratio of each raw material. Specifically, through a multistep preparation method and different dies, a zirconium alloy die forging with a high precision size is prepared, and in the process of rolling and deforming the intermediate blank through the rolling die, deformation protrusions on two side walls of the die are effectively limited, so that the wall thickness of the die is gradually reduced, the deformation state of the side wall of the intermediate blank under the external rolling force is further limited and stopped, the operation and difficulty that the side wall needs to be repaired again in the later stage after the deformation protrusions are generated are avoided, and the influence of the side wall deformation on the mechanical property of a finished product is reduced.
Drawings
FIG. 1 is a schematic view of the preparation process of the present invention.
FIG. 2 is an enlarged view of the counterbore of FIG. 1 according to the invention.
Fig. 3 is a cross-sectional view of the first press roll and the second press roll of fig. 2 according to the present invention.
FIG. 4 is an enlarged view of the invention at A in FIG. 3.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the following further describes the technical solution of the present invention with reference to the drawings and the embodiments.
Example one
The preparation process of the high-performance zirconium alloy die forging piece shown in the attached drawings 1-4 comprises the following steps:
s1, preparing the ingredients
Selecting sponge zirconium with 0.045% of O content and 0.045% of Fe content, zirconium oxide, zirconium-niobium alloy and iron nails, wherein the weight ratio of the sponge zirconium to the zirconium oxide is 97%, the zirconium oxide is 0.4%, the zirconium-niobium alloy is 2.55%, and the iron nails are 0.05%;
s2, preparing cast ingot
The sponge zirconium, the zirconia, the zirconium-niobium alloy and the iron nail are mixed according to the weight ratio and then melted into the specification of
Figure BDA0003059600370000051
The ingot of (1), the oxygen content of which is 0.15, the Fe content of which is 0.08%;
s3 forging
First-stage forging: heating the cast ingot to 1030 deg.C, maintaining the temperature for 400min, shaping to □ 500 × 900mm by using rapid forging machine (preferably with 6300T tonnage), upsetting to 500mm height along its length direction, reversely drawing to □ 500 × 900mm, repeating the process for three times of upsetting, and finally rounding to 35500 × 900mm
Figure BDA0003059600370000061
Obtaining a fire blank;
forging with two heats: charging the first-fire blank into a furnace, heating to 850 ℃, preserving heat for 400min, upsetting (preferably adopting a 2500T quick forging machine), upsetting to 500mm high below 800mm, then drawing to 800mm high along the original direction, circularly upsetting for three times in such a way, and finally forming □ 350 multiplied by 1850mm to obtain a second-fire blank;
forging with three heats: grinding the blank, heating to 830 deg.C, and shaping
Figure BDA0003059600370000062
(preferably using 800T oil press) to obtain an initial billet;
s4, preparing a cylindrical boss blank
Selecting a preparation die to upset the initial blank to a small-diameter end
Figure BDA0003059600370000063
The large diameter end is
Figure BDA0003059600370000064
The cylindrical boss blank;
specifically, the preparation mold is provided with a small-diameter end matched with the cylindrical boss blank
Figure BDA0003059600370000065
And a height of 77mm, and a fitting large-diameter end
Figure BDA0003059600370000066
The outer diameter of the cylindrical tube structure (the preparation mold shown in fig. 1). With one end of the initial blank passing through the preparation die
Figure BDA0003059600370000067
In the through hole, a lower upsetting external force is applied to the top end of the initial blank, and the specification and the size of the preparation die are limited until the initial blank is formed into a small-diameter end
Figure BDA0003059600370000068
The large diameter end is
Figure BDA0003059600370000069
The preparation die can be designed and manufactured according to the design size of the cylindrical boss blank so as to form the cylindrical boss blank with the design size by one-time upsetting.
S5, punching
Heating the cylindrical boss blank to 820 ℃, tempering and preserving heat for 150min, and punching
Figure BDA00030596003700000610
And finally reaming by using a punching core to
Figure BDA00030596003700000611
While obtaining a small diameter end of
Figure BDA00030596003700000612
The large diameter end is
Figure BDA0003059600370000071
The intermediate blank of (3);
s6 reaming of grinding ring
Heating the intermediate blank to 820 ℃, using a vertical ring mill having a ring mill die 1 for engaging the intermediate blank
Figure BDA0003059600370000072
To the middle hole
Figure BDA0003059600370000073
While obtaining a small diameter end of
Figure BDA0003059600370000074
The large diameter end is
Figure BDA0003059600370000075
The finished blank of (1);
specifically, as shown in fig. 2, the ring rolling die 1 is fixedly sleeved on a main roller 10 of the vertical ring rolling machine, the ring rolling die 1 has a first ring rolling part 1a and a second ring rolling part 1b which are sequentially matched with the small-diameter end and the large-diameter end of the intermediate blank to be in circumferential contact, and the widths of the first ring rolling part 1a and the second ring rolling part 1b are sequentially equal to the heights of the small-diameter end and the large-diameter end of the intermediate blank. The middle hole has an inner diameter of
Figure BDA0003059600370000076
The whole cover of middle blank establish on the dabber 20 of ring rolling machine, through the ring rolling machine effect make main roll 10 drive ring rolling mould 1 orientation middle blank direction is close to make first ring rolling portion 1a hug closely on the global of the little diameter end of middle blank, second ring rolling portion 1b hugs closely simultaneously on global of the big diameter end of middle blank, through ring rolling machine drive main roll 10 after that, and drive ring rolling mould 1 and rotate, and simultaneously through the rotation of dabber 20's support drive middle blank, be close to dabber 20 direction through main roll 10 gradually in the pivoted, make ring rolling mould 1 constantly exert the pressure to middle blank, make middle blank take place deformation, its little diameter end and major diameter endThe wall thickness of the end is gradually reduced, and the diameter of the middle hole is gradually increased until the hole in the ring is gradually reduced
Figure BDA0003059600370000077
Is reamed to
Figure BDA0003059600370000078
While obtaining a small diameter end of
Figure BDA0003059600370000079
The large diameter end is
Figure BDA00030596003700000710
The finished blank is obtained.
Because the first ring rolling part 1a and the second ring rolling part 1b of the ring rolling mould apply force to the small diameter end and the large diameter end of the middle blank in the radial direction and generate deformation, in the deformation process, the outer side walls of the small-diameter end and the large-diameter end of the intermediate blank are provided with axial micro-deformation (outward bulge), which causes errors in the various dimensions of the entire finished blank from the design dimensions, so that in order to avoid intermediate blanks during rolling by the ring rolling die, the outer side walls of the small-diameter end and the large-diameter end are kept from deforming, and only the radial peripheral surface is allowed to deform, so that the size of the final finished blank is the same as the design size, before the intermediate blank is rolled to the finished blank, deformation preventing devices for preventing the intermediate blank from axially deforming at the small-diameter end and the large-diameter end under the state of external rolling force are arranged at the two sides of the intermediate blank. Through this prevent that deformation device restricts the both sides wall of middle blank, effectually prevents its deformation, and then guarantees the dimensional requirement after middle blank rolls into finished product blank.
Specifically, the deformation preventing device comprises shaft sleeves 2 which are symmetrically and rotatably sleeved on the central shafts 20 on two sides of the middle blank, a central shaft 3 perpendicular to the central shafts 20 is arranged on each shaft sleeve 2, and a first compression roller 4 and a second compression roller 5 which are attached to the outer wall of the small-diameter end and the outer wall of the large-diameter end of the middle blank and rotate are sequentially arranged on the central shafts 3 on two sides. When rolling ring mould 1 and rolling the in-process of middle blank in the rotation, middle blank rotates with rolling ring mould 1 under the support of dabber 20 in step, and axle sleeve 2 rotates for dabber 20, and then keep the position of first compression roller 4 and second compression roller 5 unchangeable relatively, the lateral wall that can form middle blank just can carry out effectual restriction's effect to the deformation state when rolling formation deformation, and under first compression roller 4 and the effect of second compression roller 5 pivoted, keep leveling of middle blank lateral wall, and reduce the contact friction to middle blank lateral wall. Because first compression roller 4 and second compression roller 5 laminate in proper order on the minor diameter end outer wall and the major diameter end outer wall of middle blank, to this outer wall deformation in the process of rolling restrict in real time and level and smooth the restoration simultaneously for when minor diameter end and major diameter end radial thickness reduce, its axial width keeps unchangeable, and then guarantees that the finished product blank after rolling has higher size precision.
In order to make the first compression roller 4 and the second compression roller 5 can fully and effectively limit the deformation of the two side walls of the middle blank, the lengths of the first compression roller 4 and the second compression roller 5 are sequentially greater than the heights of the small-diameter end and the large-diameter end of the middle blank, so that the small-diameter end and the large-diameter end can be sequentially limited in the heights of the first compression roller 4 and the second compression roller 5. Since the main roller 10 gradually leans against the mandrel 20 during the rolling process, in order to avoid the mutual interference between the first roller 4 and the main roller 10 and the second roller 5, it is preferable to ensure that the lengths of the first roller 4 and the second roller 5 are not contacted with the main roller 10 when the intermediate blank is rolled to the finished blank.
After the first compression roller 4 and the second compression roller 5 contact the deformation of the side wall of the middle blank, due to the fact that the shaft sleeve 2 rotates around the mandrel 20, the deformation protrusion can block the first compression roller 4 and the second compression roller 5, and then the first compression roller 4 and the second compression roller 5 are driven to rotate around the mandrel 20 under the rotation of the respective shaft sleeve 2, so that the deformation protrusion cannot be effectively limited and the side wall cannot be flattened, therefore, in order to enable the first compression roller 4 and the second compression roller 5 to effectively overcome the blocking effect of the deformation protrusion, the shaft sleeve 2 is also rotatably sleeved on the main rollers 10 on the two sides of the ring rolling die 1, and the shaft sleeve 2 is provided with a limiting rod 6 which moves along the length direction of the middle shaft 3, penetrates through the middle shaft 3 and is used for limiting the first compression roller 4 and the second compression roller 5 to rotate around the mandrel 20. Through inserting gag lever post 6 in axle sleeve 2, restrict first compression roller 4 and second compression roller 5's rotation, and then can effectually overcome the bellied hindrance effect of deformation, make the lateral wall of middle blank form smooth surface structure. Because the limiting rod 6 is movably arranged in the middle shaft 3 in a penetrating way, the main roller 10 synchronously moves towards the middle shaft 3 in the process of approaching the core shaft 20, and the rolling force applied to the movement of the main roller 10 is not influenced. Meanwhile, under the limiting state of the limiting rod 6, the first pressing roller 4 and the second pressing roller 5 are tightly attached to the position of the side wall of the middle blank, which is deformed due to the external rolling force, so that the deformation of the side wall of the middle blank can be timely and effectively limited, the difficulty of deformation bump repairing is reduced, the side wall of the middle blank is subjected to the processes of deformation of two sides in the process of repairing the middle blank again after the middle blank is deformed is reduced, and the influence on the mechanical property of the middle blank and even the mechanical property of a finished product in the two deformation processes is further reduced. The limiting rod 6 can be separated from the central shaft 3 under the action that the main roller 10 is far away from the mandrel 20, so that the assembly of the intermediate blank and the disassembly of the finished blank are facilitated.
Since the central hole of the intermediate blank is tightly attached to the peripheral surface of the mandrel 20, in order to effectively limit the deformation of the bottom portion of the side wall of the intermediate blank close to the mandrel 20 (the portion is subject to the rolling force of the rolling ring die 1 and also subject to the rolling external force transmitted by the intermediate blank body, so that the portion is easy to accumulate rolling deformation and cause a large deformation), as shown in fig. 4, the end surfaces of the first pressing roller 4 and the second pressing roller 5 close to the mandrel 20 are both set to be arc surfaces 101 including the sleeve 2 at close positions, and in the included state, the side end surface side lines of the first pressing roller 4 and the second pressing roller 5 close to the mandrel 20 are close to the peripheral surface of the mandrel 20. That is, when this arcwall face 101 can contain partial axle sleeve 2, can make the bottom of first compression roller 4 and second compression roller 5 further downwardly extending be close to dabber 20 global (preferred, can leave less turning gap between the two), and then make first compression roller 4 and second compression roller 5 can be effectual be close to the effectual restriction of the accumulated deformation ability in bottom of dabber 20 to middle blank lateral wall, and level and smooth the restoration, make the lateral wall homoenergetic of whole middle blank obtain deformation restriction and level and smooth prosthetic effect, improve the shaping quality of finished product blank.
In order to further perform the above-mentioned repair operation of completely and completely limiting the deformation and the flat surface of the side wall of the intermediate blank near the bottom of the side wall of the mandrel 20, as shown in fig. 4, the portion of the mandrel 20 contacting the central hole of the intermediate blank is a first stage 20a, the portions on both sides of the first stage 20a are second stages 20b, the diameter of the first stage 20a is larger than that of the second stage 20b, and the side end surface lines of the first pressing roll 4 and the second pressing roll 5 near the mandrel 20 are overlapped with the two sides of the first stage 20 a. That is, the bottoms of the first press roll 4 and the second press roll 5 extend into the side walls on both sides of the first stage 20a, and are simultaneously matched in the rolling state, the tops of the first press roll 4 and the second press roll 5 are respectively overlapped with the side walls of the first ring rolling part 1a and the second ring rolling part 1b, and in this state, the small-diameter end side wall of the intermediate blank is completely contained in the range formed by the side wall of the first stage 20a, the first press roll 4 and the first ring rolling part 1a, and the large-diameter end side wall is completely contained in the range formed by the other side wall of the first stage 20a, the second press roll 5 and the second ring rolling part 1b, so that the small-diameter end side wall is completely contacted with the first press roll 4, and the large-diameter side wall is completely contacted with the second press roll 5, and further, the complete deformation and convex limitation and flat surface repairing operation on both side walls of the intermediate blank are realized. Under the action of the range formed by the two sides, the peripheral surface of the large and small diameter ends is completely limited in the range, so that under the action of the rolling external force, the large and small diameter ends can only allow the wall thickness to be reduced, and the large and small diameter ends are quickly formed to a finished blank state. Further improving the forming quality and the precision size of the finished blank, and reducing the operation procedures and the operation difficulty of the later grinding.
S7 annealing
Heating the finished blank to 680 ℃, preserving heat for 150min, discharging and air cooling to a finished product state.
Example two
A preparation process of a high-performance zirconium alloy die forging comprises the following steps:
s1, preparing the ingredients
Selecting sponge zirconium with the O content of 0.05 percent and the Fe content of 0.05 percent, zirconium oxide, zirconium-niobium alloy and iron nails, wherein the weight ratio of the sponge zirconium to the zirconium oxide to the zirconium-niobium alloy is 96.5 percent, the zirconium oxide to the zirconium-niobium alloy is 0.5 percent, the zirconium-niobium alloy to the iron nails is 2.95 percent, and the iron nails are 0.05 percent;
s2, preparing cast ingot
The sponge zirconium, the zirconia, the zirconium-niobium alloy and the iron nail are mixed according to the weight ratio and then melted into the specification of
Figure BDA0003059600370000121
The oxygen content of the cast ingot is 0.16 percent, and the Fe content is 0.08 percent;
s3 forging
First-stage forging: heating the cast ingot to 1020 deg.C, maintaining the temperature for 380min, shaping to □ 500 × 900mm by using rapid forging machine, upsetting to 500mm height along its length direction, reversely drawing to □ 500 × 900mm, repeating the process for three times of upsetting, and finally rounding to obtain round billet
Figure BDA0003059600370000122
Obtaining a fire blank;
forging with two heats: charging the first-fire blank into a furnace, heating to 840 ℃, preserving heat for 380min, upsetting to 500mm high at 800mm high, then drawing to 800mm high along the original direction, circularly upsetting for three times in the way, and finally forming □ 350 multiplied by 1850mm to obtain a second-fire blank;
forging with three heats: grinding the blank, heating to 825 deg.C, and shaping
Figure BDA0003059600370000123
Obtaining an initial blank;
s4, preparing a cylindrical boss blank
Selecting a preparation die to upset the initial blank to a small-diameter end
Figure BDA0003059600370000124
The large diameter end is
Figure BDA0003059600370000125
The specific preparation method of the cylindrical boss blank is the same as that of the embodiment I.
S5, punching
Heating the cylindrical boss blank to 820 deg.C, tempering and maintaining for 135min, and punching
Figure BDA0003059600370000126
And finally reaming by using a punching core to
Figure BDA0003059600370000127
While obtaining a small diameter end of
Figure BDA0003059600370000128
The large diameter end is
Figure BDA0003059600370000129
The intermediate blank of (3);
s6 reaming of grinding ring
Heating the intermediate blank to 815 ℃, and using a vertical ring rolling mill having a ring rolling die 1 for engaging the intermediate blank
Figure BDA00030596003700001210
To the middle hole
Figure BDA00030596003700001211
While obtaining a small diameter end of
Figure BDA0003059600370000131
The large diameter end is
Figure BDA0003059600370000132
The concrete ring-rolling broaching operation mode of the finished blank is as described in the first embodiment.
S7 annealing
Heating the finished blank to 660 ℃, preserving heat for 130min, discharging and air cooling to a finished product state.
EXAMPLE III
A preparation process of a high-performance zirconium alloy die forging comprises the following steps:
s1, preparing the ingredients
Selecting sponge zirconium with the O content of 0.04 percent and the Fe content of 0.04 percent, zirconium oxide, zirconium-niobium alloy and iron nails, wherein the weight ratio of the sponge zirconium to the zirconium oxide to the zirconium-niobium alloy is 96 percent, the zirconium oxide to the zirconium-niobium alloy is 0.6 percent, the zirconium-niobium alloy to the iron nails is 3.34 percent, and the iron nails are 0.06 percent;
s2, preparing cast ingot
The sponge zirconium, the zirconia, the zirconium-niobium alloy and the iron nail are mixed according to the weight ratio and then melted into the specification of
Figure BDA0003059600370000133
The ingot of (1), the oxygen content of which is 0.14%, the Fe content of which is 0.1%;
s3 forging
First-stage forging: heating the cast ingot to 1010 deg.C, maintaining the temperature for 360min, shaping to □ 500 × 900mm by using a rapid forging machine, upsetting to 500mm height along the length direction, reversely drawing to □ 500 × 900mm, repeatedly performing three times of upsetting and drawing, and finally rounding to obtain the final product
Figure BDA0003059600370000134
Obtaining a fire blank;
forging with two heats: charging the first-fire blank into a furnace, heating to 830 ℃, preserving heat for 360min, upsetting to 500mm high at 800mm high, then drawing to 800mm high along the original direction, circularly upsetting for three times in the way, and finally forming to □ 350 multiplied by 1850mm to obtain a second-fire blank;
forging with three heats: grinding the blank, heating to 820 deg.C, and shaping
Figure BDA0003059600370000142
Obtaining an initial blank;
s4, preparing a cylindrical boss blank
Selecting a preparation die to upset the initial blank to a small straightThe diameter end is
Figure BDA0003059600370000143
The large diameter end is
Figure BDA0003059600370000144
The specific preparation method of the cylindrical boss blank is the same as that of the embodiment I.
S5, punching
Heating the cylindrical boss blank to 820 ℃, tempering and preserving heat for 120min, and punching
Figure BDA0003059600370000145
And finally reaming by using a punching core to
Figure BDA0003059600370000146
While obtaining a small diameter end of
Figure BDA0003059600370000147
The large diameter end is
Figure BDA0003059600370000148
The intermediate blank of (3);
s6 reaming of grinding ring
Heating the intermediate blank to 810 ℃, using a vertical ring mill having a ring mill die 1 for engaging the intermediate blank
Figure BDA0003059600370000149
To the middle hole
Figure BDA00030596003700001410
While obtaining a small diameter end of
Figure BDA00030596003700001411
The large diameter end is
Figure BDA00030596003700001412
The concrete ring-rolling broaching operation mode of the finished blank is as described in the first embodiment.
S7 annealing
Heating the finished blank to 650 ℃, preserving heat for 120min, discharging and air cooling to a finished product state.
The following table shows the measured data values of the mechanical properties of the finished zirconium alloy die forgings prepared in the first to third examples (corresponding to sample numbers 1 to 3 in the table respectively):
Figure BDA0003059600370000141
Figure BDA0003059600370000151
the principle of the invention is as follows: the preparation process is used for preparing the zirconium alloy die forging with high performance by strictly controlling the material selection and further controlling the weight ratio of each raw material. Specifically, through a multistep preparation method and different dies, a zirconium alloy die forging with a high precision size is prepared, and in the process of rolling and deforming the intermediate blank through the rolling die, deformation protrusions on two side walls of the die are effectively limited, so that the wall thickness of the die is gradually reduced, the deformation state of the side wall of the intermediate blank under the external rolling force is further limited and stopped, the operation and difficulty that the side wall needs to be repaired again in the later stage after the deformation protrusions are generated are avoided, and the influence of the side wall deformation on the mechanical property of a finished product is reduced.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (8)

1. The preparation process of the high-performance zirconium alloy die forging is characterized by comprising the following steps of:
s1, preparing the ingredients
Selecting sponge zirconium with the O content of less than or equal to 0.05 percent and the Fe content of less than or equal to 0.05 percent, zirconium oxide, zirconium-niobium alloy and iron nails, wherein the weight ratio of the sponge zirconium to the zirconium oxide to the zirconium-niobium alloy is 96-97 percent, the zirconium oxide to the zirconium-niobium alloy is 0.4-0.6 percent, the zirconium-niobium alloy is 2.5-3.5 percent and the iron nails are 0.05-0.06 percent;
s2, preparing cast ingot
The sponge zirconium, the zirconia, the zirconium-niobium alloy and the iron nail are mixed according to the weight ratio and then melted into the specification of
Figure FDA0003059600360000011
The cast ingot has the O content of 0.14 to 0.16 percent and the Fe content of 0.08 to 0.1 percent;
s3 forging
First-stage forging: heating the cast ingot to 1010-1030 ℃, preserving heat for 360-400 min, adopting a quick forging machine to shape the cast ingot to □ 500 x 900mm in circumference, upsetting the cast ingot to 500mm height along the length direction, reversely drawing the cast ingot to □ 500 x 900mm, circularly performing three times of upsetting and drawing, and finally rounding the cast ingot to 35500 x 900mm
Figure FDA0003059600360000012
Obtaining a fire blank;
forging with two heats: charging the first-fire blank into a furnace, heating to 830-850 ℃, preserving heat for 360-400 min, upsetting to 500mm high at 800mm, then drawing to 800mm high along the original direction, circularly upsetting for three times in the way, and finally forming to □ 350 multiplied by 1850mm to obtain a second-fire blank;
forging with three heats: grinding and heating the blank of the second fire to 820-830 ℃, and then shaping to
Figure FDA0003059600360000013
Obtaining an initial blank;
s4, preparing a cylindrical boss blank
Selecting a preparation die to upset the initial blank to a small-diameter end
Figure FDA0003059600360000021
The large diameter end is
Figure FDA0003059600360000022
The cylindrical boss blank;
s5, punching
Heating the cylindrical boss blank to 820 ℃, tempering and preserving heat for 120-150 min, and punching
Figure FDA0003059600360000023
And finally reaming by using a punching core to
Figure FDA0003059600360000024
While obtaining a small diameter end of
Figure FDA0003059600360000025
The large diameter end is
Figure FDA0003059600360000026
The intermediate blank of (3);
s6 reaming of grinding ring
Heating the intermediate blank to 810-820 ℃, and adopting a vertical ring rolling machine with a ring rolling die (1) matched with the intermediate blank to roll the intermediate blank
Figure FDA0003059600360000027
To the middle hole
Figure FDA0003059600360000028
While obtaining a small diameter end of
Figure FDA0003059600360000029
The large diameter end is
Figure FDA00030596003600000210
The finished blank of (1);
s7 annealing
Heating the finished blank to 650-680 ℃, preserving heat for 120-150 min, discharging and air cooling to a finished product state.
2. The preparation process of the high-performance zirconium alloy die forging piece according to claim 1, characterized in that: in step S4, the preparation mold is provided with a small diameter end matched with the cylindrical boss blank
Figure FDA00030596003600000211
And a height of 77mm, and a fitting large-diameter end
Figure FDA00030596003600000212
The outer diameter of the cylindrical tube.
3. The preparation process of the high-performance zirconium alloy die forging piece according to claim 2, characterized in that: the fixed cover of stone roller mould (1) is established on main roll (10) of vertical stone roller, stone roller mould (1) have in proper order cooperate with the first stone roller portion (1a) and the second stone roller portion (1b) of the global contact of little diameter end and major diameter end of middle blank to the width of first stone roller portion (1a) and second stone roller portion (1b) in proper order with the height of the little diameter end and the major diameter end of middle blank equals.
4. The preparation process of the high-performance zirconium alloy die forging piece according to claim 3, characterized in that: before the intermediate blank is rolled to the finished blank, deformation preventing devices for preventing the intermediate blank from axially deforming at the small-diameter end and the large-diameter end under the state of external rolling force are arranged at the two sides of the intermediate blank.
5. The preparation process of the high-performance zirconium alloy die forging piece according to claim 4, characterized in that: the deformation prevention device comprises shaft sleeves (2) which are symmetrically and rotatably sleeved on mandrels (20) on two sides of the middle blank, a middle shaft (3) perpendicular to the mandrel (20) is arranged on each shaft sleeve (2), first compression rollers (4) and second compression rollers (5) which are attached to the outer walls of the small-diameter end and the large-diameter end of the middle blank and rotate are sequentially arranged on the middle shafts (3) on two sides, and the lengths of the first compression rollers (4) and the second compression rollers (5) are sequentially greater than the heights of the small-diameter end and the large-diameter end of the middle blank.
6. The preparation process of the high-performance zirconium alloy die forging piece according to claim 5, characterized in that: the main rollers (10) on the two sides of the ring rolling die (1) are also rotatably sleeved with shaft sleeves (2), and limiting rods (6) which are arranged in the shaft sleeves (2) in a penetrating mode along the length direction of the shaft (3) and used for limiting the first pressing roller (4) and the second pressing roller (5) to rotate around the core shaft (20) are arranged on the shaft sleeves (3).
7. The preparation process of the high-performance zirconium alloy die forging piece according to claim 6, characterized in that: the end faces, close to the mandrel (20), of the first pressing roller (4) and the second pressing roller (5) are both set to be arc-shaped faces (101) containing the shaft sleeves (2) at close positions, and in the containing state, the side edge faces, close to the mandrel (20), of the first pressing roller (4) and the second pressing roller (5) are close to the circumferential face of the mandrel (20).
8. The preparation process of the high-performance zirconium alloy die forging piece according to claim 7, characterized in that: the part of the mandrel (20) contacting with the middle hole of the intermediate blank is a first stage (20a), the parts on two sides of the first stage (20a) are second stages (20b), the diameter of the first stage (20a) is larger than that of the second stage (20b), and the side edge face lines of the first pressing roller (4) and the second pressing roller (5) close to the mandrel (20) are overlapped with two side faces of the first stage (20 a).
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Publication number Priority date Publication date Assignee Title
US3480430A (en) * 1965-08-27 1969-11-25 Commissariat Energie Atomique Zirconium alloy
EP0071193B1 (en) * 1981-07-29 1988-06-01 Hitachi, Ltd. Process for producing zirconium-based alloy
CN101947648A (en) * 2010-11-03 2011-01-19 西安泵阀总厂有限公司 Method for producing large zirconium and zirconium alloy casting
CN105483442A (en) * 2015-12-07 2016-04-13 西部新锆核材料科技有限公司 Zr-Nb alloy for nuclear reactor fuel cladding and preparation method of Zr-Nb alloy
CN106238639A (en) * 2016-07-28 2016-12-21 柳州科尔特锻造机械有限公司 A kind of process of zircaloy steel forging
CN108914015A (en) * 2018-08-10 2018-11-30 中航卓越锻造(无锡)有限公司 The super-huge forging special-shape ring of low-alloy high-strength HI high impact function and its forging method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3480430A (en) * 1965-08-27 1969-11-25 Commissariat Energie Atomique Zirconium alloy
EP0071193B1 (en) * 1981-07-29 1988-06-01 Hitachi, Ltd. Process for producing zirconium-based alloy
CN101947648A (en) * 2010-11-03 2011-01-19 西安泵阀总厂有限公司 Method for producing large zirconium and zirconium alloy casting
CN105483442A (en) * 2015-12-07 2016-04-13 西部新锆核材料科技有限公司 Zr-Nb alloy for nuclear reactor fuel cladding and preparation method of Zr-Nb alloy
CN106238639A (en) * 2016-07-28 2016-12-21 柳州科尔特锻造机械有限公司 A kind of process of zircaloy steel forging
CN108914015A (en) * 2018-08-10 2018-11-30 中航卓越锻造(无锡)有限公司 The super-huge forging special-shape ring of low-alloy high-strength HI high impact function and its forging method

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