CN113319530A - Preparation method of zirconium-niobium alloy plate spring - Google Patents

Preparation method of zirconium-niobium alloy plate spring Download PDF

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CN113319530A
CN113319530A CN202110597500.8A CN202110597500A CN113319530A CN 113319530 A CN113319530 A CN 113319530A CN 202110597500 A CN202110597500 A CN 202110597500A CN 113319530 A CN113319530 A CN 113319530A
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plate spring
zirconium
niobium alloy
blank
die
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CN113319530B (en
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程佳
杨永良
张丹丹
史航
王晨华
赵祥
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Xi'an Pump & Valve General Factory Co ltd
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Xi'an Pump & Valve General Factory Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
    • B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/18—Hardening; Quenching with or without subsequent tempering
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/26—Methods of annealing
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/62—Quenching devices
    • C21D1/673—Quenching devices for die quenching
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0247—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/02—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for springs
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C16/00—Alloys based on zirconium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18—High-melting or refractory metals or alloys based thereon
    • C22F1/186—High-melting or refractory metals or alloys based thereon of zirconium or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/10—Oxidising
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F17/00—Multi-step processes for surface treatment of metallic material involving at least one process provided for in class C23 and at least one process covered by subclass C21D or C22F or class C25
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2261/00—Machining or cutting being involved
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00—Energy generation of nuclear origin
    • Y02E30/30—Nuclear fission reactors

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  • Metallurgy (AREA)
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  • Physics & Mathematics (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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Abstract

The invention belongs to the technical field of plate spring processing, and particularly discloses a preparation method of a zirconium-niobium alloy plate spring, which is used for solving the technical problems of low hardness and strength and poor wear resistance of a zirconium-niobium alloy. The preparation method comprises the following steps: performing mixed smelting on the zirconium and niobium raw materials to obtain a zirconium-niobium alloy; forging or rolling the zirconium-niobium alloy into a plate, and carrying out recrystallization annealing on the plate to obtain a plate blank; processing the plate blank into a plate spring blank; polishing the plate spring blank to obtain a polished plate spring blank; sequentially carrying out solid solution treatment and aging treatment on the polished plate spring blank to obtain a plate spring blank; and performing surface finishing treatment on the plate spring rough blank to obtain the zirconium-niobium alloy plate spring. According to the preparation method of the zirconium-niobium alloy plate spring, the mechanical property and the wear resistance of the zirconium-niobium alloy plate spring are enhanced by controlling the technological parameters such as the temperature and the time of the solution quenching treatment and the aging treatment.

Description

Preparation method of zirconium-niobium alloy plate spring
Technical Field
The embodiment of the application relates to the technical field of plate spring processing, in particular to a preparation method of a zirconium-niobium alloy plate spring.
Background
The plate spring has the characteristics of small installation space, high rigidity, short stroke, high buffering elasticity and the like, and is widely applied to the field of chemical valves. Because the chemical valve is usually applied to the harsh environment in the chemical field, the plate spring is a key component of the chemical valve, and the material of the plate spring has both excellent corrosion resistance and mechanical properties required by the plate spring, the plate spring with good corrosion resistance and excellent mechanical properties needs to be prepared to meet the performance requirements of the chemical valve.
Zirconium and zirconium alloy show excellent corrosion resistance in various acid and alkali media, and can be used as corrosion-resistant structural materials for processing chemical valves. The plate spring is used as a key part of the chemical valve, and the overall corrosion resistance and the material of the plate spring and the chemical valve are consistent, namely the zirconium and zirconium alloy valves need to be matched with the zirconium alloy plate spring.
However, zirconium alloy has problems of poor wear resistance and low hardness and strength, and it is difficult to satisfy the requirements of acid and alkali corrosion resistance and mechanical properties such as hardness and strength when used for manufacturing a plate spring. Simultaneously, the bore specification kind of chemical industry valve is more, and manufacturing enterprise needs order the leaf spring according to the specification demand, and it is little to cause the purchase volume of appointed specification kind easily, leads to the purchase degree of difficulty of leaf spring big and the expense high.
Disclosure of Invention
The embodiment of the application provides a preparation method of a zirconium-niobium alloy plate spring, and solves the technical problems of poor wear resistance, low hardness and low strength of the zirconium alloy plate spring.
In order to achieve the technical purpose, the embodiment of the application adopts the following technical scheme:
in a first aspect, a method for manufacturing a zirconium-niobium alloy plate spring according to an embodiment of the present application includes the following steps:
performing mixed smelting on the zirconium and niobium raw materials to obtain a zirconium-niobium alloy;
forging or rolling the zirconium-niobium alloy into a plate, and carrying out recrystallization annealing on the plate to obtain a plate blank;
processing the plate blank into a plate spring blank;
polishing the plate spring blank to obtain a polished plate spring blank;
sequentially carrying out solid solution treatment and aging treatment on the polished plate spring blank to obtain a plate spring blank;
and performing surface finishing treatment on the plate spring rough blank to obtain the zirconium-niobium alloy plate spring.
With reference to the first aspect, as a further improvement of the embodiment of the present application, the polishing process of the plate spring blank includes:
and polishing the upper surface and the lower surface of the plate spring blank until the Ra is 0.4-0.8.
With reference to the first aspect, as a further improvement of the embodiments of the present application, before the solution treatment, the method further includes:
and assembling the polishing plate spring blank in a special concave-convex composite tool die for the plate spring so as to prevent the polishing plate spring blank from deforming in the heat treatment process.
With reference to the first aspect, as a further improvement of the embodiment of the present application, the temperature of the solution treatment is 870-930 ℃ and the time is 30-40 min.
In combination with the first aspect, as a further improvement of the embodiment of the present application, the temperature of the solution treatment is 870 ℃, and the time is 30 min.
With reference to the first aspect, as a further improvement of the embodiment of the present application, the temperature of the aging treatment is 450-.
In combination with the first aspect, as a further improvement of the embodiment of the present application, the temperature of the aging treatment is 450 ℃ and the time is 60 min.
With reference to the first aspect, as a further improvement of the embodiment of the present application, the concave-convex composite tooling die special for the plate spring includes a lower die and an upper die;
the lower die is positioned below the upper die, a groove is formed in the end part, close to the upper die, of the lower die, and a first flow guide hole penetrating through the groove is formed in the lower die; a boss is arranged at the end part of the upper die close to the lower die, and the upper die is provided with a second flow guide hole penetrating through the boss;
and in a matched die state, the boss is embedded into the groove and forms a die cavity with the groove, and a plate spring die can be installed in the die cavity.
With reference to the first aspect, as a further improvement of the embodiment of the present application, the upper die is provided with a first through hole penetrating through upper and lower end surfaces of the upper die, and an inner thread is formed on an inner wall of the first through hole; the lower die is provided with a second through hole penetrating through the upper end face of the lower die, and an internal thread is formed on the inner wall of the second through hole;
and in a mold closing state, the first through hole is communicated with the second through hole.
With reference to the first aspect, as a further improvement of the embodiment of the present application, before performing the surface finishing treatment, the method further includes:
and carrying out surface pre-oxidation treatment on the plate spring rough blank so as to enable the hardness of the plate spring rough blank to reach 220-275 HB.
With reference to the first aspect, as a further improvement of the embodiment of the present application, after the surface pre-oxidation treatment is performed, the hardness of the plate spring blank is 220-275 HB.
In a second aspect, on the basis of the research on the preparation method of the zirconium-niobium alloy plate spring, the embodiment of the application also provides a zirconium-niobium alloy for preparing the plate spring, and the zirconium-niobium alloy is prepared from the following components in percentage by weight:
97-98% of zirconium; 2 to 3 percent of niobium.
In combination with the second aspect, in some possible embodiments of the examples herein, the zirconium-niobium alloy is prepared from a 98% zirconium component and a 2% niobium component.
In combination with the second aspect, in some possible embodiments of the examples herein, the zirconium-niobium alloy is prepared from 97% of a zirconium component and 3% of a niobium component.
In combination with the second aspect, in some possible embodiments of the examples herein, the zirconium-niobium alloy is prepared from 97.5% of a zirconium component and 2.5% of a niobium component.
Compared with the prior art, the beneficial effects or advantages of the embodiment of the application include:
according to the preparation method of the zirconium-niobium alloy plate spring, the zirconium-niobium alloy is used as a raw material to be forged or rolled to form a plate, the plate is recrystallized and annealed to form a plate spring blank, and the plate spring blank is subjected to polishing treatment, solution treatment and aging treatment, so that the mechanical properties such as hardness and strength, the wear resistance and the corrosion resistance of the zirconium-niobium alloy plate spring are improved.
According to the preparation method of the zirconium-niobium alloy plate spring provided by the embodiment of the application, the mechanical property, the wear resistance and the corrosion resistance of the plate spring are enhanced by controlling the technological parameters such as the temperature, the time and the like of solution quenching and aging treatment. The test result shows that the Brinell hardness of the zirconium-niobium alloy plate spring prepared in the embodiment of the application reaches 220-; particularly, the thickness of the oxide film formed on the surface of the plate spring reaches 109 mu m, so that the wear resistance and the acid-base corrosion resistance of the plate spring are obviously improved.
In summary, the preparation method of the zirconium-niobium alloy plate spring provided by the embodiment of the application can obviously improve the mechanical properties such as strength, elasticity and the like of the zirconium-niobium alloy plate spring, and can improve the wear resistance and corrosion resistance of the zirconium-niobium alloy plate spring. Meanwhile, the preparation method is simple and efficient in process, high in program operation controllability and stable in product quality, is suitable for production and processing of small-batch multi-specification plate springs, can realize self-control of chemical valve processing enterprises, does not need special purchase of small-batch multi-specification plate springs, and reduces production and processing cost of the enterprises.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings used in the description of the embodiments will be briefly introduced below. It is obvious that the drawings in the following description are only some of the embodiments described in the present application, and that other drawings can be derived from these drawings by a person skilled in the art without inventive effort.
Fig. 1 is a flowchart of a method for manufacturing a zirconium-niobium alloy plate spring according to an embodiment of the present disclosure;
fig. 2 is a front perspective view of a concave-convex composite tooling die special for a plate spring provided in the embodiment of the present application;
fig. 3 is a side perspective view of a concave-convex composite tooling die special for a plate spring according to an embodiment of the present application;
reference numerals: 1-lower mould; 2, mounting a mold; 10-a groove; 11-a second via; 20-boss; 21-a first via; 100-a first flow guide hole; 200-second diversion holes.
Detailed Description
In order to make the technical solutions better understood by those skilled in the art, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. It should be apparent that the described embodiments are only some of the embodiments of the present application, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
In the description of the embodiments of the present application, it should be noted that the terms "upper", "lower", "bottom", "top", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only used for convenience in describing the embodiments of the present application and simplifying the description, but do not indicate or imply that the referred devices or elements must have a specific orientation, be configured and operated in a specific orientation, and thus, should not be construed as limiting the present application. The term "connected" is to be understood broadly, for example, as being fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the embodiments of the present application can be understood by those of ordinary skill in the art according to specific situations.
As shown in fig. 1, the method for manufacturing a zirconium-niobium alloy plate spring provided in this embodiment specifically includes the following steps.
S101: and carrying out mixed smelting on the zirconium and niobium raw materials to obtain the zirconium-niobium alloy.
S102: forging or rolling the zirconium-niobium alloy into a plate, and carrying out recrystallization annealing on the plate to obtain a plate blank.
S103: and processing the plate blank into a plate spring blank, specifically, taking the plate blank as a raw material, and performing linear cutting and processing to form the plate spring blank according to the inner and outer diameter sizes of the plate spring.
S104: and polishing the plate spring blank to obtain a polished plate spring blank.
S105: and sequentially carrying out solid solution treatment and aging treatment on the polished plate spring blank to obtain a plate spring blank.
S106: and performing surface finishing treatment on the plate spring rough blank to obtain the zirconium-niobium alloy plate spring.
The solution heat treatment is a heat treatment process for heating a zirconium-niobium alloy polished plate spring blank to a high-temperature single-phase region and keeping the temperature constant, so that an excess phase is fully dissolved in a solid solution, and then rapidly cooling to obtain a supersaturated solid solution.
The aging treatment refers to a heat treatment process that zirconium-niobium alloy polished plate spring blanks are subjected to solution treatment, quenched at high temperature or deformed by cold working to a certain degree, and then placed at higher temperature or room temperature to keep the shape and size of the blanks, and the performance of the blanks changes along with time.
According to the preparation method of the zirconium-niobium alloy plate spring, the zirconium-niobium alloy is forged or rolled to form a plate, the plate is recrystallized and annealed and then processed into a plate spring blank, and the plate spring blank is sequentially subjected to polishing treatment, solution treatment and aging treatment, so that the mechanical properties such as hardness and strength, the wear resistance and the acid and alkali corrosion resistance of the zirconium-niobium alloy plate spring are improved.
It should be understood by those skilled in the art that the surface roughness of the plate spring blank affects the stability of the oxide film formed on the surface of the plate spring blank, in particular, the residual stress in the oxide film increases with the increase of the surface roughness, so that the oxide film is easy to fall off on the surface of the rough plate spring blank, the uniformity and thickness of the oxide film formed on the surface of the machined plate spring are affected, and the hardness and wear resistance of the plate spring are affected. Therefore, in the embodiment, before the plate spring blank is subjected to the solution treatment and the aging treatment, the plate spring blank is subjected to the polishing treatment, so that the surface of the plate spring blank is ensured to be formed with a dense, uniform and stable-quality oxidation film. The inventors have found, in the study of the effect of the surface roughness of the zirconium-niobium alloy on the stability of the oxide film, that when the surface Ra of the zirconium-niobium alloy is 0.4 to 0.8, the thickness and properties of the oxide film formed on the surface thereof exhibit great advantages. Therefore, the polishing treatment of the leaf spring blank according to the embodiment of the application comprises the following steps: and polishing the surface of the plate spring blank to Ra of 0.4-0.8.
It should be understood by those skilled in the art that the blank of the plate spring made of zirconium-niobium alloy is easy to deform during the heat treatment process, so that the specification quality of the machined zirconium-niobium alloy plate spring does not meet the corresponding requirement. Therefore, in order to avoid deformation of the plate spring blank during the heat treatment, the embodiment of the present application further includes, before performing the solution treatment: and assembling the polishing plate spring blank in a special concave-convex composite tool die for the plate spring.
Of course, after the polished plate spring blank is assembled in the plate spring-dedicated concave-convex composite tooling die for heat treatment, the plate spring blank should be disassembled from the plate spring-dedicated concave-convex composite tooling die and then surface finish-treated. Wherein, the surface finish treatment refers to the process steps of polishing and trimming the rough blank of the plate spring.
Based on the preparation method of the zirconium-niobium alloy plate spring, the embodiment of the application also provides a concave-convex composite tool die special for the plate spring, as shown in fig. 2 and 3.
Referring to fig. 2 to 3, the concave-convex composite tooling die special for the plate spring comprises a lower die 1 and an upper die 2, wherein the lower die 1 is positioned below the upper die 2, a groove 10 is formed in the end part, close to the upper die 2, of the lower die 1, and the lower die 1 is provided with a first flow guide hole 100 penetrating through the groove 10; a boss 20 is arranged at the end part of the upper die 2 close to the lower die 1, and the upper die 2 is provided with a second flow guide hole 200 penetrating through the boss 20; in the clamped state, the boss 20 is inserted into the recess 10 and forms a mold cavity with the recess 20, in which a leaf spring mold can be mounted.
The utility model provides a special unsmooth compound frock mould of leaf spring, including bed die 1 and last mould 2, set up recess 10 and the first water conservancy diversion hole 100 that runs through recess 10 through the upper end at bed die 1 to set up boss 20 and the second water conservancy diversion hole 200 that runs through boss 20 at last mould 2 lower tip, thereby under the compound die state boss 20 imbed in the recess 10 and with form the die cavity between the recess 20, can install the leaf spring mould in the die cavity. This special unsmooth compound frock mould of leaf spring can compress tightly two upper and lower surfaces and interior outer disc of leaf spring mould, prevents effectively that the leaf spring mould from being heated the deformation.
With reference to fig. 2 to 3, the upper mold 2 is provided with a first through hole 21 penetrating through the upper and lower end surfaces, and an inner wall of the first through hole 21 is formed with an internal thread; the lower die 1 is provided with a second through hole 11 penetrating through the upper end face of the lower die, and an internal thread is formed on the inner wall of the second through hole 11; in the clamped state, the first through hole 21 communicates with the second through hole 11.
It will be understood by those skilled in the art that the mechanical properties, wear resistance and corrosion resistance of the zirconium-niobium alloy are related to the microstructure (such as the type, size and distribution of the second phase particles) after heat treatment, and the microstructure depends on the solution quenching conditions during heat treatment, intermediate annealing, final annealing and other factors, so that the control of the temperature and time of the solution quenching treatment has an important influence on the improvement of the mechanical properties, wear resistance and acid-base corrosion resistance of the zirconium-niobium alloy plate spring. However, in the research of the temperature and time of the solution quenching treatment on the acid and alkali corrosion resistance of the zirconium-niobium alloy plate spring, the inventor finds that when the temperature of the solution quenching treatment of the zirconium-niobium alloy plate spring is 870-930 ℃ and the time is 30-40min, the generated beta-Nb can be stabilized, and the comprehensive improvement of the mechanical property, the wear resistance and the corrosion resistance of the zirconium-niobium alloy plate spring can be realized. Therefore, the temperature of the solution quenching treatment is controlled to 870-930 ℃ for 30-40min, and particularly the temperature of the solution quenching treatment is controlled to 870 ℃ for 30 min.
Table 1 shows the results of the measurements of the mechanical properties and the surface hardness of the zirconium-niobium alloy plate spring in different solution quenching temperature treatments and time periods.
TABLE 1 mechanical properties and surface hardness of zirconium-niobium alloy leaf springs under different solution quenching conditions
Figure BDA0003091658170000071
Figure BDA0003091658170000081
As can be seen from Table 1, when the temperature of solution quenching is 870-plus 930 ℃ and the holding time is 30-40min, the mechanical properties (yield strength and tensile strength) of the zirconium-niobium alloy plate spring are better, and the hardness reaches 226-plus 246 HB; when the temperature of solution quenching is lower than 870 ℃ (such as 700 ℃), the mechanical property (yield strength and tensile strength) and hardness of the zirconium-niobium alloy plate spring are far lower than those of a zirconium-niobium alloy bar; when the solution quenching temperature is higher than 930 ℃ (such as 1050 ℃), the mechanical properties (yield strength and tensile strength) and hardness of the zirconium-niobium alloy plate spring are equivalent to those of a zirconium-niobium alloy bar material. Therefore, the mechanical property and the wear resistance of the zirconium-niobium alloy plate spring are enhanced by controlling the technological parameters such as the temperature of solution quenching, the heat preservation time and the like.
It will be appreciated by those skilled in the art that the temperature of the aging treatment has a significant effect on the acid and alkali corrosion resistance of the zirconium-niobium alloy leaf spring, but the zirconium-niobium alloy undergoes a peritectic reaction at 610 ℃, and aging treatment above this temperature leaves Nb-rich β -Zr and deteriorates the acid and alkali corrosion resistance of the zirconium-niobium alloy leaf spring, so the temperature of the aging treatment is typically below 600 ℃. In view of this, the temperature of the aging treatment of the zirconium-niobium alloy is selected to be 580 ℃, the microstructure of the aging treatment temperature is alpha-Zr which is nearly completely recrystallized, and the beta-Nb which is dispersed finely is precipitated in the crystal grain boundary and matrix of the alpha-Zr, so that the structure without the beta-Zr has higher acid-base corrosion resistance. However, the inventor creatively discovers in the research of the aging treatment of the zirconium-niobium alloy plate spring that the acid and alkali corrosion resistance of the zirconium-niobium alloy plate spring is better when the temperature of the aging treatment is controlled to be 450-500 ℃ and the time is controlled to be 45-60min on the basis that the temperature of the solution quenching is 870-930 ℃ and the time is 30-40 min. Meanwhile, the mechanical property test result shows that the zirconium-niobium alloy plate spring has excellent yield strength, tensile strength, elongation, reduction of area and hardness after the aging treatment at the temperature and the heat preservation time. Therefore, the temperature of the aging treatment is controlled to be 450-500 ℃ for 45-60min, and particularly the temperature of the aging treatment is controlled to be 450 ℃ for 60 min.
Wherein, table 2 shows the test results of the mechanical properties and wear resistance of the zirconium-niobium alloy plate spring at different aging treatment temperatures.
TABLE 2 mechanical and wear resistance of zirconium-niobium alloy leaf springs at different aging temperatures
Figure BDA0003091658170000091
As can be seen from Table 2, when the temperature of solution quenching is 870-930 ℃, the heat preservation time is 30-40min, the temperature of aging treatment is 450-500 ℃, and the heat preservation time is 45-60min, the mechanical properties (yield strength, tensile strength) and the hardness of the zirconium-niobium alloy plate spring perform best in the same ratio; when the temperature of solution quenching is lower than 870 ℃ (such as 700 ℃) and the temperature of aging treatment is lower than 450 ℃ (such as 400 ℃), the mechanical properties (yield strength and tensile strength) of the zirconium-niobium alloy plate spring are improved compared with that of a zirconium-niobium alloy bar, but the hardness of the zirconium-niobium alloy plate spring is poorer; when the temperature of solution quenching is higher than 930 ℃ (1050 ℃ for example) and the temperature of aging treatment is higher than 500 ℃ (550 ℃ for example), the mechanical properties (yield strength and tensile strength) of the zirconium-niobium alloy plate spring are improved compared with those of a zirconium-niobium alloy bar material, but the hardness of the zirconium-niobium alloy plate spring is poorer. Therefore, the method and the device have the advantages that the mechanical property and the wear resistance of the zirconium-niobium alloy plate spring are enhanced by reasonably controlling the temperature and the heat preservation time of the solution quenching treatment, the temperature and the heat preservation time of the aging treatment and other process parameters.
It will be appreciated by those skilled in the art that pre-oxidation of the zircaloy leaf spring in air can form a dense oxide film on its surface, which has high hardness and wear resistance. Therefore, the embodiment of the application further comprises the step of performing surface pre-oxidation treatment on the zirconium-niobium alloy plate spring rough blank before performing the surface finishing treatment, so that the hardness of the plate spring rough blank reaches 220-275 HB.
In addition, table 3 shows the results of the test of the zirconium-niobium alloy plate spring prepared in the examples of the present application for corrosion resistance to sulfuric acid, specifically, the corrosion rate in various concentrations of sulfuric acid at a temperature of 100 ℃.
TABLE 3 sulfuric acid corrosion resistance of zirconium-niobium alloy leaf springs
Figure BDA0003091658170000101
Note: the corrosion rate is less than 0.05 mm/year, which is excellent; the corrosion rate is good at 0.05-5 mm/year.
As can be seen from table 3, the sulfuric acid corrosion resistance of the zirconium-niobium alloy plate spring prepared in the examples of the present application is significantly better than that of the zirconium-niobium alloy rod. Therefore, the embodiment of the application realizes the enhancement of the sulfuric acid corrosion resistance of the zirconium-niobium alloy plate spring by controlling the technological parameters such as the temperature, the heat preservation time and the like of the solution quenching treatment.
On the basis of research on a preparation method of a zirconium-niobium alloy plate spring, the embodiment of the application also provides a zirconium-niobium alloy for preparing the plate spring, and the zirconium-niobium alloy is prepared from the following components in percentage by weight: 97-98% of zirconium; 2 to 3 percent of niobium.
It will be appreciated by those skilled in the art that the appropriate niobium content and choice of solution temperature and aging temperature will optimize the corrosion resistance of the zirconium-niobium alloy. Therefore, under the control of the technological parameters of solution treatment, aging treatment temperature, heat preservation time and the like, the zirconium-niobium alloy plate spring prepared by adopting 97-98% of zirconium component and 2-3% of niobium component has optimal corrosion resistance and creep resistance, namely the zirconium component and the niobium component in the proportion can be used for solution strengthening the performance of the zirconium-niobium alloy.
In some possible embodiments of the examples herein, the zirconium-niobium alloy is prepared with a 98% zirconium component and a 2% niobium component.
In some possible embodiments of the examples herein, the zirconium-niobium alloy is prepared with a zirconium component of 97% and a niobium component of 3%.
In some possible embodiments of the examples herein, the zirconium-niobium alloy is prepared with a zirconium component of 97.5% and a niobium component of 2.5%.
The technical solution of the present invention will be described in more detail with reference to the following embodiments.
Example 1
Embodiment 1 provides a method for manufacturing a zirconium-niobium alloy plate spring, including the following steps.
S101: the zirconium and niobium raw materials are mixed and smelted according to the weight ratio of 97:3 to obtain the zirconium-niobium alloy.
S102: forging or rolling the zirconium-niobium alloy into a plate, and carrying out recrystallization annealing on the plate to obtain a plate blank.
S103: and the plate blank is used as a raw material, and is processed into a plate spring blank by linear cutting according to the inner and outer diameter sizes of the plate spring.
S104: and polishing the plate spring blank to obtain a polished plate spring blank, and assembling the polished plate spring blank in a special concave-convex composite tool die for the plate spring.
S105: in a box-type air furnace, carrying out solid solution quenching treatment, aging treatment and surface pre-oxidation treatment on the whole special concave-convex composite tool die for the plate spring, which is assembled with the polished plate spring blank, in sequence to obtain a plate spring blank with the hardness of 220-275HB, wherein the temperature of solid solution quenching is 870 ℃ and the time is 30 min; the temperature of the aging treatment is 450 ℃ and the time is 60 min.
S106: and disassembling a plate spring rough blank from a special concave-convex composite tool die for the plate spring, and performing surface finishing treatment on the plate spring rough blank to obtain the zirconium-niobium alloy plate spring.
Example 2
Embodiment 2 provides a method for manufacturing a zirconium-niobium alloy plate spring, which includes the following steps.
S101: the zirconium and niobium raw materials are mixed and smelted according to the weight ratio of 98:2 to obtain the zirconium-niobium alloy.
S102: forging or rolling the zirconium-niobium alloy into a plate, and carrying out recrystallization annealing on the plate to obtain a plate blank.
S103: and the plate blank is used as a raw material, and is processed into a plate spring blank by linear cutting according to the inner and outer diameter sizes of the plate spring.
S104: and polishing the plate spring blank to obtain a polished plate spring blank, and assembling the polished plate spring blank in a special concave-convex composite tool die for the plate spring.
S105: in a box-type air furnace, carrying out solid solution quenching treatment, aging treatment and surface pre-oxidation treatment on the whole special concave-convex composite tool die for the plate spring, which is assembled with the polished plate spring blank, in sequence to obtain a plate spring blank with the hardness of 220-275HB, wherein the temperature of solid solution quenching is 930 ℃ and the time is 40 min; the temperature of the aging treatment is 500 ℃ and the time is 45 min.
S106: and disassembling a plate spring rough blank from a special concave-convex composite tool die for the plate spring, and performing surface finishing treatment on the plate spring rough blank to obtain the zirconium-niobium alloy plate spring.
Example 3
Embodiment 3 provides a method for manufacturing a zirconium-niobium alloy plate spring, including the following steps.
S101: the zirconium and niobium raw materials are mixed and smelted according to the weight ratio of 97.5:2.5 to obtain the zirconium-niobium alloy.
S102: forging or rolling the zirconium-niobium alloy into a plate, and carrying out recrystallization annealing on the plate to obtain a plate blank.
S103: and the plate blank is used as a raw material, and is processed into a plate spring blank by linear cutting according to the inner and outer diameter sizes of the plate spring.
S104: and polishing the plate spring blank to obtain a polished plate spring blank, and assembling the polished plate spring blank in a special concave-convex composite tool die for the plate spring.
S105: in a box-type air furnace, carrying out solid solution quenching treatment, aging treatment and surface pre-oxidation treatment on the whole special concave-convex composite tool die for the plate spring, which is assembled with the polished plate spring blank, in sequence to obtain a plate spring blank with the hardness of 220-275HB, wherein the temperature of solid solution quenching is 870 ℃ and the time is 30 min; the temperature of the aging treatment is 500 ℃, and the time is 60 min.
S106: and disassembling a plate spring rough blank from a special concave-convex composite tool die for the plate spring, and performing surface finishing treatment on the plate spring rough blank to obtain the zirconium-niobium alloy plate spring.
The zirconium-niobium alloy plate springs prepared in examples 1 to 3 were subjected to performance tests, and the test results are shown in table 4.
TABLE 4 mechanical Properties and wear resistance indices of the Zr-Nb alloy plate springs prepared in examples 1 to 3
Figure BDA0003091658170000131
As can be seen from table 4, the mechanical properties and wear resistance (hardness) of the zirconium-niobium alloy plate spring prepared in examples 1 to 3 of the present application are significantly improved compared to those of a zirconium-niobium alloy bar. Specifically, the yield strength of the zirconium-niobium alloy plate spring prepared in the embodiment of the application is improved by 20.8-29.4% compared with that of a zirconium-niobium alloy bar; the compressive strength of the zirconium-niobium alloy plate spring prepared in the embodiment of the application is improved by 2.9-14.2% compared with that of a zirconium-niobium alloy bar; compared with a zirconium-niobium alloy bar, the hardness of the zirconium-niobium alloy plate spring prepared in the embodiment of the application is improved by 54.4-58.5%, and the wear resistance of the zirconium-niobium alloy plate spring prepared in the embodiment of the application is improved by 54.4-58.5% compared with that of the zirconium-niobium alloy bar. Therefore, the preparation method of the zirconium-niobium alloy plate spring provided by the embodiment of the application can obviously improve the mechanical property and the wear resistance of the zirconium-niobium alloy.
Meanwhile, the test results show that the surface oxide film thickness of the zirconium-niobium alloy plate spring prepared in example 1 of the present application is 109 μm, and the hardness reaches 566.9 HV.
In addition, the present application example also studies the elastic properties of the zirconium-niobium alloy plate spring and the zirconium-niobium alloy plate blank prepared in example 1, and the specific test results are shown in tables 5 to 6. Wherein, table 5 shows the spring property of the zirconium-niobium alloy plate spring prepared in example 1; table 6 shows the spring properties of the zirconium-niobium alloy sheet blank.
TABLE 5 spring performance of the zirconium-niobium alloy plate spring prepared in example 1
Figure BDA0003091658170000141
As can be seen from table 5, the elastic performance of the zirconium-niobium alloy plate spring prepared in this example 1 is significantly higher than the design requirement, wherein the elastic performance of the spring compressed by 1.18mm is improved by 13.7% compared with the design requirement; the elastic performance of the compression of 1.57mm is improved by 20.0 percent compared with the design requirement. Therefore, the elastic performance of the zirconium-niobium alloy plate spring is obviously improved by controlling parameters such as the temperature and time of solution quenching, the temperature and time of aging treatment and the like in the zirconium-niobium alloy heat treatment process and performing pre-oxidation treatment after the aging treatment.
TABLE 6 elasticity Properties of zirconium-niobium alloy sheet Material
Figure BDA0003091658170000142
As can be seen from Table 6, the elastic properties of the zirconium-niobium alloy plate blank are all lower than the design requirements, wherein the elastic property of the zirconium-niobium alloy plate blank compressed by 1.18mm is different from the design requirements by 251.5N; the spring performance for compression of 1.57mm is 151.5N different than the design requirement.
As can be seen from comparison between tables 5 and 6, in the examples of the present application, by controlling parameters such as the temperature and time of solution quenching during the heat treatment of the zirconium-niobium alloy, the temperature and time of aging treatment, and the like, and performing pre-oxidation treatment after the aging treatment, the elastic properties of the zirconium-niobium alloy plate blank are significantly improved. Wherein, the elastic performance of the compression of 1.18mm is improved by 37.8 percent in the same ratio; the elastic performance of the compression of 1.57mm is improved by 29.8 percent in the same ratio.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.

Claims (10)

1. A method for manufacturing a zirconium-niobium alloy plate spring is characterized by comprising the following steps of:
performing mixed smelting on the zirconium and niobium raw materials to obtain a zirconium-niobium alloy;
forging or rolling the zirconium-niobium alloy into a plate, and carrying out recrystallization annealing on the plate to obtain a plate blank;
processing the plate blank into a plate spring blank;
polishing the plate spring blank to obtain a polished plate spring blank;
sequentially carrying out solid solution treatment and aging treatment on the polished plate spring blank to obtain a plate spring blank;
and performing surface finishing treatment on the plate spring rough blank to obtain the zirconium-niobium alloy plate spring.
2. The method of manufacturing a zirconium-niobium alloy leaf spring of claim 1, wherein the polishing the leaf spring blank comprises:
and polishing the surface of the plate spring blank to Ra of 0.4-0.8.
3. The method of manufacturing a zirconium-niobium alloy plate spring according to claim 1, further comprising, before the solution treatment:
and assembling the polishing plate spring blank in a special concave-convex composite tool die for the plate spring so as to prevent the polishing plate spring blank from deforming in the solution treatment process.
4. The method for preparing a Zr-Nb alloy plate spring as claimed in claim 3, wherein the solution treatment temperature is 870-930 ℃ and the time is 30-40 min.
5. The method of manufacturing a zirconium-niobium alloy plate spring according to claim 4, wherein the temperature of the solution treatment is 870 ℃ for 3 min.
6. The method for preparing a zirconium-niobium alloy plate spring as claimed in claim 3, wherein the temperature of the aging treatment is 450-500 ℃ and the time is 45-60 min.
7. The method of manufacturing a zirconium-niobium alloy plate spring according to claim 6, wherein the aging treatment is performed at a temperature of 450 ℃ for 60 min.
8. The method for manufacturing a zirconium-niobium alloy plate spring according to claim 3, wherein the concave-convex composite tool die specially used for the plate spring comprises a lower die and an upper die;
the lower die is positioned below the upper die, a groove is formed in the end part, close to the upper die, of the lower die, and a first flow guide hole penetrating through the groove is formed in the lower die; a boss is arranged at the end part of the upper die close to the lower die, and the upper die is provided with a second flow guide hole penetrating through the boss;
and in a matched die state, the boss is embedded into the groove and forms a die cavity with the groove, and a plate spring die can be installed in the die cavity.
9. The method for manufacturing a zirconium-niobium alloy plate spring according to claim 8, wherein the upper die is provided with a first through hole penetrating through upper and lower end surfaces thereof, and an internal thread is formed on an inner wall of the first through hole; the lower die is provided with a second through hole penetrating through the upper end face of the lower die, and an internal thread is formed on the inner wall of the second through hole;
and in a mold closing state, the first through hole is communicated with the second through hole.
10. The method of manufacturing a zirconium-niobium alloy plate spring according to any one of claims 1 to 9, further comprising, before performing the surface finishing treatment:
and carrying out surface pre-oxidation treatment on the plate spring rough blank so as to enable the hardness of the plate spring rough blank to reach 220-275 HB.
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