CN113862516B - Preparation method of high-strength titanium alloy strip for catering appliances - Google Patents
Preparation method of high-strength titanium alloy strip for catering appliances Download PDFInfo
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- CN113862516B CN113862516B CN202111224768.3A CN202111224768A CN113862516B CN 113862516 B CN113862516 B CN 113862516B CN 202111224768 A CN202111224768 A CN 202111224768A CN 113862516 B CN113862516 B CN 113862516B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- 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
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- 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
- C21D8/0221—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
- C21D8/0226—Hot rolling
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- 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
- C21D8/0221—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
- C21D8/0236—Cold rolling
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- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/16—Remelting metals
- C22B9/20—Arc remelting
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- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F2003/145—Both compacting and sintering simultaneously by warm compacting, below debindering temperature
Abstract
The invention discloses a preparation method of a high-strength titanium alloy strip for catering utensils, and belongs to the field of titanium alloy strip preparation. The preparation method comprises the following steps: mixing titanium sponge and molybdenum powder according to the mass ratio of 97:3, performing warm isostatic pressing to form a consumable electrode, and then performing vacuum consumable arc melting to form a titanium alloy cast ingot; forging a titanium alloy ingot into a titanium alloy plate blank, hot-rolling the titanium alloy plate blank into a hot-rolled titanium alloy strip with the thickness of 4mm, sequentially annealing and pickling the semi-finished product of the hot-rolled titanium alloy strip to obtain a titanium alloy semi-finished product titanium strip, cold-rolling the titanium alloy semi-finished product titanium strip into a cold-rolled titanium alloy strip with the thickness of 2mm, and sequentially performing oil removal cleaning, finished product annealing and leveling treatment to obtain the high-strength titanium alloy strip for catering utensils. The preparation method provided by the invention not only solves the problem of excessive precipitation of molybdenum element in the existing titanium-molybdenum alloy, but also improves the comprehensive mechanical property of the titanium-molybdenum alloy while improving the processing plasticity of the titanium alloy, and is suitable for manufacturing high-pressure catering utensils.
Description
Technical Field
The invention relates to the technical field of titanium alloy strip preparation, in particular to a preparation method of a high-strength titanium alloy strip for catering utensils.
Background
The pure titanium metal has the advantages of small density, high specific strength, good corrosion resistance, excellent biocompatibility, no heavy metal precipitation and the like, and is suitable for manufacturing various catering utensils. Titanium catering utensils have been widely introduced into the market, such as titanium thermos cups, frying pans, soup pots, milk pots, etc., but in high altitude areas, air is thin, atmospheric pressure is reduced, and the boiling point of water is reduced, so that food cannot be completely cooked, and high pressure catering utensils are required to be used for increasing the boiling point.
At present, the common high-pressure tableware on the market is mainly made of stainless steel, aluminum alloy and other materials, the problem that the precipitation of elements such as nickel, chromium, cadmium, aluminum and the like is excessive and the human health is damaged exists, and the problem of the precipitation of the metal elements can be avoided by utilizing titanium and titanium alloy to produce the high-pressure tableware. However, pure titanium has low tensile strength at room temperature, low hardness and poor scratch and abrasion resistance, so that catering utensils made of pure titanium cannot meet the pressure requirement of 500KPa, and needs to be alloyed to improve mechanical properties and technological properties.
However, many alloy additives (aluminum, nickel, zirconium, niobium) have significant metal precipitation properties, which limits the use of the alloy material in the manufacture of eating utensils. The molybdenum element is a isomorphous beta stabilizing element, and the addition of the molybdenum element is beneficial to refining alloy grains and improving plasticity, can effectively improve the room temperature performance and the high temperature strength, and enhances the machinability of the alloy. Although molybdenum is a trace element required by human body and is beneficial to development and metabolism of human body when being taken in a proper amount, the existing titanium-molybdenum alloy has higher molybdenum content (omega) Mo Not less than 10%), very easyThe excessive intake of molybdenum is easy to cause harm to human health; with a molybdenum content (omega) Mo Less than or equal to 3.0 percent), the titanium-molybdenum alloy has poor comprehensive mechanical property and can not meet the pressure requirement of catering appliances in high altitude areas.
Disclosure of Invention
The purpose of the invention is: the preparation method of the high-strength titanium alloy strip for the catering utensils is provided for solving the technical problems that the high molybdenum content in the existing titanium-molybdenum alloy is harmful to human health, and the molding and mechanical properties of the catering utensils are influenced due to the low molybdenum content.
In order to achieve the purpose, the invention provides the technical scheme that:
a preparation method of a high-strength titanium alloy strip for catering utensils comprises the following steps:
mixing titanium sponge and molybdenum powder with the Fisher's average particle size of 4-5 mu m according to the mass ratio of 97:3 in an inert gas atmosphere to obtain a mixture;
carrying out warm isostatic pressing on the mixture to form a consumable electrode, and carrying out vacuum consumable arc melting by using the consumable electrode to obtain a titanium alloy ingot;
forging the titanium alloy ingot into a titanium alloy plate blank;
hot rolling the titanium alloy plate blank into a hot-rolled titanium alloy strip with the thickness of 4mm, and sequentially annealing and pickling a semi-finished product to obtain a titanium alloy semi-finished product titanium strip;
and cold-rolling the titanium alloy semi-finished product titanium strip into a cold-rolled titanium alloy strip with the thickness of 2mm, and sequentially performing oil removal cleaning, finished product annealing and flattening treatment on the cold-rolled titanium alloy strip to obtain the high-strength titanium alloy strip for catering utensils.
As a further improved technical scheme of the invention, the tensile strength at room temperature of the high-strength titanium alloy strip for the catering utensils is more than or equal to 550MPa, the yield strength is more than or equal to 480MPa, and the elongation is more than or equal to 35%.
As a further improved technical scheme of the invention, the titanium sponge is grade 0 titanium sponge or grade 1 titanium sponge.
As a further improved technical scheme of the invention, the times of the vacuum consumable arc melting are three times, wherein the current of the first melting is 15kA, and the voltage is 28V; the current of the second smelting is 20kA, and the voltage is 30V; the current of the third smelting is 25kA, and the voltage is 35V.
As a further improved technical scheme of the invention, the hot rolling of the titanium alloy slab into the hot rolled titanium alloy strip with the thickness of 2mm comprises the following steps:
hot rolling the titanium alloy plate blank into a rough rolled strip with the thickness of 30mm, wherein the hot rolling temperature is 820-850 ℃, the heat preservation time is 5-6h, and the deformation is 85%;
and (3) hot rolling the rough rolled strip coil into a hot rolled titanium alloy strip with the thickness of 4mm, wherein the hot rolling temperature of the coil is 780-800 ℃, the heat preservation time is 30-40min, and the deformation is 86.7%.
As a further improved technical scheme of the invention, the annealing temperature of the hot-rolled titanium alloy strip semi-finished product is 720-750 ℃, and the time is 40-60 min.
As a further improved technical scheme of the invention, the annealing temperature of the finished cold-rolled titanium alloy strip is 670-700 ℃, and the time is 40-60 min.
As a further improved technical scheme of the invention, the pass deformation of the cold rolling is 5-15%.
As a further improved technical scheme of the invention, the forging times are two;
the temperature of each forging is 1000-1100 ℃, the heat preservation time of the first forging is 5-9h, and the heat preservation time of the second forging is 2 h.
As a further improved technical scheme of the invention, the rotation speed of mixing the titanium sponge and the molybdenum powder with the Fisher average particle size of 4-5 mu m according to the mass ratio of 97:3 is 150-225 r/min.
Compared with the prior art, the invention has the advantages or beneficial effects that at least:
the invention provides a preparation method of a high-strength titanium alloy strip for catering utensils, which comprises the steps of mixing titanium sponge and molybdenum powder according to the mass ratio of 97:3, performing warm isostatic pressing to form a consumable electrode, performing vacuum consumable arc melting, forging to form a titanium alloy plate blank, sequentially performing forging, hot rolling, semi-finished product annealing, acid washing, cold rolling, oil removal cleaning, finished product annealing and leveling treatment, and strictly controlling technological parameters of hot rolling, cold rolling, annealing and the like, thereby preparing the high-strength titanium alloy strip for the catering utensils. The preparation method provided by the invention not only ensures that the molybdenum element precipitation amount of the catering utensil made of the titanium-molybdenum alloy is extremely low by controlling the mass ratio of the titanium sponge to the molybdenum powder to be 97:3, effectively solves the problem that the excessive precipitation of the molybdenum element is harmful to the health of a human body, but also enables the molybdenum powder to be refined and filled in the tissue gaps of the titanium sponge by controlling the granularity of the titanium sponge and the molybdenum powder and the technological parameters of hot rolling, cold rolling, annealing and the like, effectively prevents the adhesion and segregation phenomena of the titanium sponge and the molybdenum powder, is beneficial to refining the grain size of an alloy tissue and improving the processing plasticity, thereby enhancing the comprehensive mechanical property while improving the elongation of the titanium alloy, and enabling the catering utensil manufactured by the preparation method to meet the pressure requirement of a high altitude area.
Drawings
In order to more clearly illustrate the technical solution of the present invention, the drawings used in the description of the embodiments will be briefly described 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 graph showing the variation of the comprehensive mechanical properties of a high-strength titanium alloy strip for catering utensils, which is manufactured according to an embodiment of the invention, with the molybdenum content;
FIG. 2 is a cross-sectional metallographic view of a high-strength titanium alloy strip for tableware, which is manufactured by the method;
FIG. 3 is a longitudinal structure metallographic picture of a high-strength titanium alloy strip for tableware, which is manufactured by the invention.
Detailed Description
The technical solution of the present invention will be clearly and completely described below in conjunction with the present invention. It should be apparent that the embodiments described below are only a part 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 invention.
It will be appreciated by those skilled in the art that the titanium sponge and molybdenum powders in the examples below are commercially available or obtained by routine experimentation.
The preparation method of the high-strength titanium alloy strip for the catering utensils comprises the steps of S101-S105.
S101-mixing: in an inert gas atmosphere, mixing titanium sponge and molybdenum powder with the Fisher's average particle size of 4-5 mu m according to a mass ratio of 97:3 to obtain a mixture. Wherein, the inert gas is high-purity argon with the mass purity of not less than 99.99 percent.
It should be noted that, titanium sponge and molybdenum powder generate heat easily in the mixing process to generate oxide impurities, which has a certain influence on the alloying process, and this embodiment mixes materials in the inert gas atmosphere, so that the titanium sponge and/or molybdenum powder can be prevented from being oxidized by heat. In addition, the heating degree of the inert gas atmosphere with high vacuum degree and the mixing at high rotation speed can be increased, and the uneven mixing and/or the mixing time can be increased due to the excessively low rotation speed, and the embodiment performs a single-factor variable experiment to determine that the vacuum degree of the inert gas atmosphere is not more than 0.1Pa, the mixing rotation speed is 150-. Meanwhile, when the titanium sponge and the molybdenum powder are mixed, the molybdenum powder is unevenly distributed in the titanium sponge due to the overlarge particle size of the molybdenum powder, and the raw materials are adhered to each other due to the overlarge particle size of the molybdenum powder, so that the material mixing is uneven, and the segregation phenomenon is easily caused. Therefore, in the embodiment, high-purity titanium sponge and molybdenum powder with the Fisher's average particle size of 4-5 μm are selected as raw materials during material mixing, and the material mixing rotation speed is controlled to be 150-225r/min and the material mixing time is controlled to be 3-5h in the inert gas atmosphere with the vacuum degree of not more than 0.1Pa, so that the material mixing uniformity is improved.
As will be understood by those skilled in the art, the titanium alloy strip for catering utensils should maintain good strength and safety at both room temperature and high temperature, wherein the addition amount of molybdenum element should be reduced based on safety considerations, but too low addition amount of molybdenum element may result in that the compressive strength, yield strength and elongation of the alloy may not meet the corresponding requirements, and may not even play a role in improving the alloy structure grains, and the comprehensive mechanical properties (compressive strength, yield strength and elongation) of the titanium-molybdenum alloy at molybdenum contents of 2%, 3% and 4% respectively are studied by tensile experiments in this example, and the results are shown in FIG. 1.
As can be seen from FIG. 1, as the content of molybdenum element increases, the compressive strength of the titanium-molybdenum alloy increases from 541MPa to 645MPa, the yield strength increases from 494MPa to 588MPa, and the elongation decreases from 38% to 30%. Therefore, based on the requirements of forming, stretching and processing plasticity of the tableware, the titanium belt for the tableware with the molybdenum content of 3% has better mechanical property, can completely meet the pressure requirement of the tableware in a high altitude area, has extremely low molybdenum element precipitation rate, and meets the safety requirement of heavy metal precipitation.
Meanwhile, the purity of the titanium sponge in the embodiment is more than or equal to 99.5 percent so as to reduce the segregation phenomenon and improve the quality of the titanium belt for the catering utensils. The titanium sponge is a common titanium alloy raw material, and the purity of the 0-grade titanium sponge and the 1-grade titanium sponge is very high, so that the purity requirement of the titanium sponge can be met, and therefore the 0-grade titanium sponge and the 1-grade titanium sponge are preferably used as the titanium sponge raw material in the embodiment.
S102-smelting: and carrying out warm isostatic pressing on the mixture to form a consumable electrode, and carrying out vacuum consumable arc melting by using the consumable electrode to obtain a titanium alloy ingot.
It should be noted that the vacuum consumable electrode melting is a process of melting metal by using arc energy in a vacuum chamber of the vacuum consumable electrode melting furnace, and in this embodiment, the consumable electrode ingot is subjected to vacuum consumable electrode melting to form a titanium alloy ingot, so that not only can a titanium alloy ingot with uniform structure, no shrinkage cavity and compactness be obtained, but also nonmetallic inclusions in titanium and molybdenum raw materials can be removed, and thus the cold and hot processing performance, plasticity and mechanical performance of the titanium alloy ingot are obviously improved. The vacuum consumable arc melting in the embodiment is multiple melting in which current and voltage are sequentially increased, and the multiple melting in which current and voltage are sequentially increased can improve not only the surface compactness of the titanium alloy ingot but also the uniformity of the grain structure of the titanium alloy ingot, and the preferred vacuum consumable arc melting in the embodiment includes: smelting for the first time, wherein the current of the smelting for the first time is 15kA, and the voltage is 28V; smelting for the second time, wherein the current of the smelting for the second time is 20kA, and the voltage is 30V; and carrying out third melting, wherein the current of the third melting is 25kA, and the voltage is 35V, and researches prove that the titanium alloy ingot formed by carrying out the third vacuum consumable arc melting in the embodiment has better performance, and particularly the uniformity of the grain structure and the surface compactness of the titanium alloy ingot can be obviously improved.
As will be understood by those skilled in the art, the consumable electrode is easy to generate hot crack defects when vacuum arc melting is carried out, and the vacuum arc melting effect is influenced. In the embodiment, the consumable electrode is formed by adopting a warm isostatic pressing technology, so that the firmness of the consumable electrode is obviously improved, the occurrence of the hot crack defect of the consumable electrode is further reduced, and the vacuum consumable electric arc melting effect is improved, so that the cold and hot processing performance, the plasticity and the mechanical property of the titanium alloy cast ingot are further improved.
S103-forging: and forging the titanium alloy ingot into a titanium alloy plate blank.
In the present embodiment, after the titanium alloy ingot is formed by vacuum consumable arc melting, the titanium alloy ingot is forged into a titanium alloy slab, so as to improve the properties of the titanium alloy slab, such as grain structure, processing plasticity, compressive strength, yield strength, and the like. Moreover, as will be understood by those skilled in the art, reasonable process parameters can be used to improve the texture and properties of the titanium alloy slab during the forging process.
In this embodiment, the influence of temperature on the structure and performance of the titanium alloy slab is studied by using a tensile test, and the result shows that: when the forging forming temperature is 1000-1100 ℃, the structure and the performance of the titanium alloy slab can be improved to a certain degree. Meanwhile, the present embodiment also studies the influence of the time parameter on the structure and performance of the titanium alloy slab, and the result shows that: forging and forming a titanium alloy ingot twice, wherein the heat preservation time of the first forging and forming is 5-9 h; when the heat preservation time of the second forging forming is 2 hours, the improvement effect of the forging on the structure and the performance of the titanium alloy plate blank is obviously enhanced. Therefore, in the embodiment, the titanium alloy ingot is forged and formed twice at the temperature of 1000-1100 ℃, and the heat preservation time of the first forging and forming is 5-9 h; the holding time of the second forging forming is 2 hours.
S104-hot rolling: and hot rolling the titanium alloy plate blank into a hot-rolled titanium alloy strip with the thickness of 4mm, and sequentially annealing and pickling the semi-finished product of the hot-rolled titanium alloy strip to obtain the titanium alloy semi-finished product titanium strip.
It should be noted that the grain structure and mechanical properties of the alloy during hot rolling are reasonably controlled by controlling the hot rolling process parameters (hot rolling temperature, holding time, deformation, etc.), and the grain structure and mechanical properties of the alloy at different hot rolling temperatures and deformations are studied in this example. The results show that: the grain structure of the alloy can be obviously improved through two hot rolling forming processes. In addition, when the titanium alloy slab is hot-rolled twice into a hot-rolled titanium alloy strip with a thickness of 4mm, the hot-rolling forming is preferably performed by the following steps: under the conditions that the temperature is 820-.
It will be appreciated by those skilled in the art that the present example sequentially performs the semi-finished annealing and the pickling of the hot rolled titanium alloy strip, wherein the pickling removes the oxide skin from the surface of the hot rolled titanium alloy strip. Of course, the pickling time and temperature can be determined according to the pickling condition, and this embodiment is not limited. The annealing parameters of the semi-finished product have significant influence on the formation and growth of the grain structure, and the influence of temperature and time on the grain structure of the alloy is researched in the embodiment, and the result shows that: the annealing temperature of the hot-rolled titanium alloy strip is controlled to be 720-750 ℃, and when the annealing time is 40-60min, the structure grains of the obtained titanium alloy semi-finished product titanium strip are more uniform, so that the processing plasticity of the alloy is effectively improved.
S105-cold rolling: and cold-rolling the titanium alloy semi-finished product titanium strip into a cold-rolled titanium alloy strip with the thickness of 2mm, and sequentially carrying out oil removal cleaning, finished product annealing and leveling treatment on the cold-rolled titanium alloy strip to obtain the high-strength titanium alloy strip for the catering utensils.
It should be noted that cold rolling can significantly increase the yield strength and elongation of the alloy, but the cold rolling process parameters (rolling temperature and deformation) have a certain influence on the mechanical properties of the alloy. In the study of the embodiment, the influence of the rolling deformation on the yield strength and the elongation of the formed strip is relatively obvious, so that the embodiment improves the yield strength and the elongation by controlling the pass deformation of the cold rolling forming to be 5-15%. Meanwhile, the annealing temperature and the annealing time of the finished product both have obvious influence on the grain structure and the processing plasticity of the alloy, and the influence of the annealing temperature and the annealing time (speed) on the grain structure of the alloy is researched by a single-factor variable method in the embodiment, and the result shows that: in the embodiment, the annealing temperature of the cold-rolled titanium alloy strip is controlled to 670-700 ℃, and the annealing time is 40-60min, so that the grain structure of the alloy is obviously improved and is more uniform.
In this example, the finished titanium strip of the titanium alloy after being flattened is observed by X500-fold metallographic microscope, and the results are shown in fig. 2 to 3. FIG. 2 shows a metallographic photograph of a transverse structure of a high-strength titanium alloy strip for tableware, which is manufactured according to the embodiment; fig. 2 shows a longitudinal structure metallographic picture of the high-strength titanium alloy strip for tableware made by the embodiment.
As can be seen from the figures 2 and 3, the reasonable control of the grain size of the alloy structure is realized by the two-rolling-process hot rolling and the multi-pass small-deformation process mode and the final product annealing, so that the grain size of the alloy structure is favorably refined, the average grain size is smaller than 10 mu m, the grain size of the alloy structure is more uniform, and the mechanical property of the high-strength titanium alloy strip for catering appliances is enhanced.
As can be seen from the above description, the preparation method of the high-strength titanium alloy strip for catering utensils comprises the following steps: mixing titanium sponge and molybdenum powder with the Fisher's average particle size of 4-5 mu m according to the mass ratio of 97:3, performing vacuum consumable arc melting through a warm isostatic pressing forming consumable electrode, forging into a titanium alloy plate blank, performing hot rolling forming on the titanium alloy plate blank to obtain the titanium alloy plate blank with the thickness of 4mm, performing semi-finished product annealing and acid pickling, performing cold rolling forming on the required thickness, and performing oil removal cleaning, finished product annealing and leveling treatment in sequence to obtain the high-strength titanium alloy strip for catering utensils. Based on the fact, the high-strength titanium alloy strip for tableware manufactured by the embodiment has very low molybdenum content (omega) Mo 3.0 percent), effectively solves the problem that excessive molybdenum element is separated out to harm human health, thins and fills the molybdenum powder in the tissue gaps of the titanium sponge by controlling the granularity of the molybdenum powder and mixing the molybdenum powder under the protection of inert gas, effectively prevents the adhesion and segregation phenomena, thereby realizing the grain refinement of the alloy tissue and the improvement of processing plasticity, and also leads the grain structure and the granularity of the alloy to be changed to be more uniform and smaller micrometers by controlling the technological parameters of hot rolling, semi-finished product annealing, cold rolling, finished product annealing and the like, thereby improving the comprehensive mechanical property of the alloy while improving the processing plasticity of the alloy, leading the tensile strength at room temperature to be more than or equal to 550MPa, the yield strength to be more than or equal to 480MPa and the elongation to be more than or equal to 35 percent, and being suitable for manufacturing dining and drinking appliances in high altitude areas.
Embodiments of the present application are described in further detail below with reference to specific examples.
Example 1
The preparation method of the high-strength titanium alloy strip for catering utensils, provided by the embodiment 1, comprises the following steps:
step one, mixing materials: putting molybdenum powder with the Fisher's average particle size of 4 mu m and sponge titanium with the purity of more than or equal to 99.5% in batches according to the mass ratio of 3:97 into a planetary mixer, and mixing materials for 4 hours at the rotating speed of the planetary mixer of 180r/min in the gas protection atmosphere of high-purity argon with the mass purity of not less than 99.99%. Wherein the vacuum degree of the gas protection atmosphere is not more than 0.1 Pa.
Step two, smelting: and (3) after the mixture is subjected to warm isostatic pressing to form the consumable electrode, performing three times of vacuum consumable arc melting by using the consumable electrode to obtain a titanium alloy ingot with phi of 720 mm. Wherein the current for the first smelting is 15kA, and the voltage is 28V; the current of the second smelting is 20kA, and the voltage is 32V; the current of the third smelting is 25kA, and the voltage is 35V.
Step three, forging: and forging the titanium alloy ingot at the temperature of 1100 ℃ for two times to obtain a titanium alloy plate blank with the thickness of 200mm, wherein the heat preservation time of the first heat forging is 6 hours, and the heat preservation time of the second heat forging is 2 hours.
Step four, hot rolling: carrying out four-roller hot rolling on the titanium alloy plate blank to obtain a titanium alloy plate blank with the thickness of 30mm, wherein the rolling temperature is 850 ℃, the heat preservation time is 5 hours, and the deformation is 85%; and then performing furnace-coiling four-roller hot rolling to obtain a hot-rolled titanium alloy strip with the thickness of 4mm, wherein the rolling temperature is 800 ℃, the heat preservation time is 30min, and the deformation is 86.7%. And finally, annealing the semi-finished product of the hot-rolled titanium alloy strip for 45min at the temperature of 750 ℃, and removing the oxide skin on the surface of the hot-rolled titanium alloy strip by shot blasting and acid washing for later use.
Step five, cold rolling: and (3) carrying out cold rolling on the titanium alloy semi-finished product titanium strip in a 20-roller reversing mill at a reduction rate of 50% to obtain a cold-rolled titanium alloy strip with the thickness of 2mm, and then sequentially carrying out oil removal cleaning, finished product annealing and leveling treatment on the cold-rolled titanium alloy strip to obtain the high-strength titanium alloy strip for catering utensils. Wherein the annealing temperature of the finished product is 680 ℃, and the time is 50 min.
The titanium alloy strip for the catering utensils, which is prepared in the embodiment 1, is subjected to tensile test detection, and the result shows that the tensile strength of the titanium alloy strip at room temperature is 608MPa, the yield strength is 572MPa, and the elongation rate is 37%, so that the catering utensils prepared from the titanium alloy strip can meet the required pressure requirement of 500Kpa, and the catering utensils are suitable for high-altitude areas.
Example 2
As a comparative example to example 1, this example 2 provides a method of producing a titanium alloy strip, comprising the steps of:
step one, mixing materials: putting molybdenum powder with the Fisher's average particle size of 4 mu m and sponge titanium with the purity of more than or equal to 99.5% in batches according to the mass ratio of 2:98 into a planetary mixer, mixing materials at the rotating speed of 180r/min of the planetary mixer in the gas protection atmosphere of high-purity argon with the mass purity of not less than 99.99%, wherein the mixing time is 4 hours, and thus obtaining the mixture. Wherein the vacuum degree of the gas protection atmosphere is not more than 0.1 Pa.
Step two, smelting: and (3) after the mixture is subjected to warm isostatic pressing to form the consumable electrode, performing three times of vacuum consumable arc melting by using the consumable electrode to obtain a titanium alloy ingot with phi of 720 mm. Wherein the current for the first smelting is 14kA, and the voltage is 28V; the current of the second smelting is 20kA, and the voltage is 30V; the current of the third smelting is 25kA, and the voltage is 35V.
Step three, forging: and forging the titanium alloy ingot at the temperature of 1100 ℃ for two times to obtain a titanium alloy plate blank with the thickness of 200mm, wherein the heat preservation time of the first heat forging is 9 hours, and the heat preservation time of the second heat forging is 2 hours.
Step four, hot rolling: carrying out four-roller hot rolling on the titanium alloy plate blank to obtain a titanium alloy plate blank with the thickness of 30mm, wherein the rolling temperature is 820 ℃, the heat preservation time is 6 hours, and the deformation is 85%; and then performing furnace-winding four-roller hot rolling to obtain a hot-rolled titanium alloy strip with the thickness of 4mm, wherein the rolling temperature is 780 ℃, the heat preservation time is 60min, and the deformation is 86.7%. And finally, annealing the semi-finished product of the hot-rolled titanium alloy strip for 50min at the temperature of 730 ℃, and removing the oxide skin on the surface of the hot-rolled titanium alloy strip by shot blasting and acid washing for later use.
Step five, cold rolling: and (3) carrying out cold rolling on the titanium alloy semi-finished product titanium strip in a 20-roller reversing mill at a reduction rate of 50% to obtain a cold-rolled titanium alloy strip with the thickness of 2mm, and then sequentially carrying out oil removal cleaning, finished product annealing and leveling treatment on the cold-rolled titanium alloy strip to obtain the high-strength titanium alloy strip for catering utensils. Wherein the annealing temperature of the finished product is 680 ℃.
The tensile test of the high-strength titanium alloy strip for catering utensils, which is prepared in example 2, shows that the tensile strength of the titanium alloy strip at room temperature is 541MPa, the yield strength is 494MPa, the elongation is 38%, and catering utensils prepared from the titanium alloy strip cannot meet the required pressure requirement of 500Kpa, and have a crack phenomenon.
Example 3
As another comparative example to example 1, example 3 provides a method of producing a titanium alloy strip, comprising the steps of:
step one, mixing materials: putting molybdenum powder with the Fisher's average particle size of 4 mu m and sponge titanium with the purity of more than or equal to 99.5% in batches according to the mass ratio of 4:96 into a planetary mixer, and mixing materials for 4 hours at the rotating speed of the planetary mixer of 180r/min in the gas protection atmosphere of high-purity argon with the mass purity of not less than 99.99%. Wherein the vacuum degree of the gas protection atmosphere is not more than 0.1 Pa.
Step two, smelting: and (3) after the mixture is subjected to warm isostatic pressing to form the consumable electrode, performing three times of vacuum consumable arc melting by using the consumable electrode to obtain a titanium alloy ingot with phi of 720 mm. Wherein the current for the first smelting is 15kA, and the voltage is 28V; the current of the second smelting is 20kA, and the voltage is 32V; the current of the third smelting is 25kA, and the voltage is 35V.
Step three, forging: and forging the titanium alloy ingot at the temperature of 1100 ℃ for two times to obtain a titanium alloy plate blank with the thickness of 200mm, wherein the heat preservation time of the first heat forging is 6 hours, and the heat preservation time of the second heat forging is 2 hours.
Step four, hot rolling: carrying out four-roller hot rolling on the titanium alloy plate blank to obtain a titanium alloy plate blank with the thickness of 30mm, wherein the rolling temperature is 850 ℃, the heat preservation time is 5 hours, and the deformation is 85%; and then performing furnace winding four-roller hot rolling to obtain a hot-rolled titanium alloy strip with the thickness of 4mm, wherein the rolling temperature is 800 ℃, the heat preservation time is 30min, and the deformation is 86.7%. And finally, annealing the semi-finished product of the hot-rolled titanium alloy strip for 45min at the temperature of 750 ℃, and removing the oxide skin on the surface of the hot-rolled titanium alloy strip by shot blasting and acid washing for later use.
Step five, cold rolling: and (3) carrying out cold rolling on the titanium alloy semi-finished product titanium strip in a 20-roller reversing mill at a reduction rate of 50% to obtain a cold-rolled titanium alloy strip with the thickness of 2mm, and then sequentially carrying out oil removal cleaning, finished product annealing and leveling treatment on the cold-rolled titanium alloy strip to obtain the high-strength titanium alloy strip for catering utensils. Wherein the annealing temperature of the finished product is 680 ℃, and the time is 50 min.
The tensile test of the high-strength titanium alloy strip for catering appliances, which is prepared in the example 1, shows that the tensile strength of the titanium alloy strip at room temperature is 645MPa, the yield strength is 588MPa and the elongation is 30 percent.
It will be evident 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 (8)
1. A preparation method of a high-strength titanium alloy strip for catering appliances is characterized by comprising the following steps:
mixing titanium sponge and molybdenum powder with the Fisher's average particle size of 4-5 mu m according to the mass ratio of 97:3 in an inert gas atmosphere to obtain a mixture;
carrying out warm isostatic pressing on the mixture to form a consumable electrode, and carrying out vacuum consumable arc melting by using the consumable electrode to obtain a titanium alloy ingot;
forging the titanium alloy ingot into a titanium alloy plate blank;
the method comprises the following steps of hot rolling the titanium alloy plate blank into a hot-rolled titanium alloy strip with the thickness of 4mm, and sequentially annealing and pickling a semi-finished product on the hot-rolled titanium alloy strip to obtain the titanium alloy semi-finished product titanium strip, wherein the hot rolling of the titanium alloy plate blank into the hot-rolled titanium alloy strip with the thickness of 4mm comprises the following steps: hot rolling the titanium alloy plate blank into a rough rolled strip with the thickness of 30mm, wherein the hot rolling temperature is 820-850 ℃, the heat preservation time is 5-6h, and the deformation is 85%; and hot rolling the rough rolled strip coil into a hot rolled titanium alloy strip with the thickness of 4mm, wherein the hot rolling temperature of the coil is 780-800 ℃, the heat preservation time is 30-40min, and the deformation is 86.7%;
and cold-rolling the titanium alloy semi-finished product titanium strip into a cold-rolled titanium alloy strip with the thickness of 2mm, and sequentially performing oil removal cleaning, finished product annealing and flattening treatment on the cold-rolled titanium alloy strip to obtain the high-strength titanium alloy strip for catering utensils, wherein the room-temperature tensile strength of the high-strength titanium alloy strip for catering utensils is more than or equal to 550MPa, the yield strength of the high-strength titanium alloy strip is more than or equal to 480MP a, and the elongation of the high-strength titanium alloy strip is more than or equal to 35%.
2. The method for preparing a high-strength titanium alloy strip for tableware according to claim 1, wherein the titanium sponge is grade 0 titanium sponge or grade 1 titanium sponge.
3. The method for preparing the high-strength titanium alloy strip for the catering utensils as claimed in claim 1, wherein the number of times of vacuum consumable arc melting is three, wherein the current for the first melting is 15kA, and the voltage is 28V; the current of the second smelting is 20kA, and the voltage is 30V; the current of the third smelting is 25kA, and the voltage is 35V.
4. The preparation method of the high-strength titanium alloy strip for tableware according to claim 1, wherein the annealing temperature of the semi-finished hot-rolled titanium alloy strip is 720-750 ℃ and the annealing time is 40-60 min.
5. The method for preparing the high-strength titanium alloy strip for tableware according to claim 4, wherein the annealing temperature of the finished cold-rolled titanium alloy strip is 670-700 ℃ and the annealing time is 40-60 min.
6. A method for preparing a high-strength titanium alloy strip for tableware according to claim 5, wherein the pass deformation of the cold rolling is 5-15%.
7. The method for preparing a high-strength titanium alloy strip for tableware according to claim 1, wherein the forging is performed twice; the temperature of each forging is 1000-.
8. The preparation method of the high-strength titanium alloy strip for tableware according to claim 1, wherein the titanium sponge and the molybdenum powder with the Fisher average particle size of 4-5 μm are mixed according to a mass ratio of 97:3, and the rotating speed is 150-225 r/min.
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