CN109518106B - Treatment method for removing impurity elements in vanadium alloy through titanium-vanadium connection - Google Patents
Treatment method for removing impurity elements in vanadium alloy through titanium-vanadium connection Download PDFInfo
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- 229910052744 lithium Inorganic materials 0.000 description 1
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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
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- Crystallography & Structural Chemistry (AREA)
- Engineering & Computer Science (AREA)
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- Mechanical Engineering (AREA)
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Abstract
A treatment method for removing impurity elements in vanadium alloy by titanium-vanadium connection belongs to the field of metal materials. The invention improves the purity of the vanadium alloy by utilizing the solid state diffusion connection of the pure titanium metal and the vanadium alloy or plating a layer of pure titanium metal on the surface of the vanadium alloy and enabling the pure titanium to continuously absorb impurity elements in the vanadium alloy at a certain temperature in an isothermal way. By utilizing a titanium-vanadium diffusion bonding layer formed in the forged and heat-treated pure titanium sealing sheath, according to the stronger affinity of pure titanium metal to impurity elements (C, N, O), the impurity elements in the vanadium alloy are adsorbed to form Ti- (CNO) precipitates in the pure titanium metal, so that the impurity elements in the vanadium alloy are reduced, and the performance degradation of the vanadium alloy in the service process is prevented.
Description
Technical Field
The invention relates to a solid phase purification treatment method for reducing impurity elements (C, N, O) in vanadium alloy, which is characterized in that the impurity elements in the vanadium alloy are absorbed by utilizing stronger bonding capacity of titanium and C, N, O elements, so that the mechanical property degradation of the vanadium alloy under service conditions is avoided.
Background
The vanadium alloy is one of the main candidates of future nuclear fusion reactor cladding structure materials and fast reactor fuel cladding due to good compatibility with liquid lithium, non-magnetism, good radiation resistance and high-temperature mechanical property. But vanadium is chemically active and tends to absorb impurity elements (C, N, O). These interstitial impurity atoms C, N, O have strong binding ability with lattice atoms in the matrix, and are likely to form a precipitate phase. Particularly, under the conditions of high temperature and high irradiation flux of the reactor, a large amount of precipitated phases can cause material embrittlement, thereby endangering the safe operation of the reactor.
At present, there are three main measures for preventing vanadium alloy from adsorbing impurity elements: firstly, vacuum smelting is adopted, so that the opportunity that the vanadium alloy adsorbs nitrogen and oxygen in the air is reduced; but a stainless steel sealing sheath is adopted in the rolling process; thirdly, yttrium, silicon, aluminum and other elements are added to be combined with oxygen and nitrogen in the vanadium alloy to remove the elements. However, these measures cannot completely solve the problem of impurity absorption of vanadium alloy, for example, in vacuum smelting, impurity elements are absorbed even though the gas pressure is low; however, by adding other alloying elements, the formed precipitated phases are often left in the vanadium alloy in large particles, and the precipitated phases are also brittle and can harm the toughness of the vanadium alloy.
Along with the transformation and upgrading of economic structures in China, the adjustment and transformation of energy structures are at the forefront, and the development of nuclear energy, particularly nuclear fusion, fourth-generation high-temperature air-cooled and solid-cooled reactors is imperative. The vanadium alloy is used as a candidate structural material of a nuclear fusion reactor and a fuel cladding layer of a fourth-generation high-temperature gas and solid-cooled reactor, and the improvement of the mechanical property of the vanadium alloy at high temperature has important influence on safe service.
Disclosure of Invention
The invention aims to provide a method capable of absorbing interstitial impurity elements in a vanadium alloy, which can effectively reduce the content of the impurity elements in the vanadium alloy and ensure that the vanadium alloy keeps excellent mechanical properties in a high-temperature service process.
A treatment method for removing impurity elements in vanadium alloy by vanadium-titanium connection is characterized by comprising the following specific treatment steps:
step 1, polishing a pure titanium metal plate by using sand paper, washing the pure titanium metal by using alcohol after polishing, and cleaning the surface of the cut vanadium alloy by using alcohol;
step 2, processing the pure titanium metal plate into a cuboid sealing sheath with a proper size by using electron beam welding, plugging the vanadium alloy, and performing vacuum electron beam sealing welding again;
step 3, performing hot-pressure processing on the welded titanium clad sleeve by using forging equipment to extrude a connecting gap between the two metals; the selected pressure processing temperature is higher than 882.5 ℃, the proper forging temperature is 950-1150 ℃, and sand burying and cooling are selected after forging;
step 4, aging the obtained titanium and vanadium of the V-Ti binary diffusion coupling system at a temperature higher than 882.5 ℃ by a vacuum heat treatment furnace to further promote the diffusion of elements to reduce the content of impurity elements in the vanadium alloy matrix, and continuously reduce the generation of precipitated phases in the vanadium alloy under the actual service condition to ensure the safety of the reactor in service under the high-temperature condition; when the titanium coating needs to be stripped, the mechanical stripping is adopted to clean the bonding surface by using a grinding wheel.
And (3) carrying out isothermal treatment on the titanium-coated vanadium component after forging at a certain temperature in a vacuum heat treatment furnace to further purify the vanadium alloy. The high-temperature service component can be directly used, and the coated titanium is used for absorbing impurity elements in the vanadium alloy for a long time under the service condition. If the titanium layer needs to be removed, mechanical stripping combined with grinding wheel cleaning can be adopted.
Further, the vacuum degree used by the vacuum heat treatment furnace is 10-3Pa, and the heat treatment temperature is between 1000 and 1150 ℃.
Further, for the components in high-temperature service, direct service is selected, and the coated titanium is used for absorbing impurity elements in the vanadium alloy for a long time under the service condition.
Furthermore, in step 2, a layer of pure titanium may be plated on the surface of the electropolished vanadium alloy by using a plating method, and the plating time may be controlled according to the required thickness. Furthermore, the pure titanium coating can be promoted to absorb impurity elements in the vanadium alloy under the condition of vacuum heat treatment according to requirements.
Further, the treatment method for removing the impurity elements in the vanadium alloy through vanadium-titanium connection comprises the following specific steps:
1) and processing a pure titanium plate with the thickness of 0.5cm by utilizing linear cutting, and processing the pure titanium metal plate into a cuboid shell by utilizing electron beam welding. Processing the vanadium alloy into a size matched with the shell, and sealing the vanadium alloy in the pure titanium sheath by using electron beam welding again. After each linear cutting, the cutting surface of the wire is polished by diamond abrasive paper to reduce the roughness of the surfaces of two metals, reduce the defects of an interface area after connection and clean by using alcohol; cutting vanadium alloy wire into 4 x 9cm3The size of the cuboid is just matched with the size of the inner space of the pure titanium sheath;
2) the processed pure titanium sheath is forged at high temperature to reduce the contact gap between the two metals, the forged surface is selected as the front surface of the cuboid, and the reduction amount is not easy to be too large (10-30%). The heating temperature is required to be in a body-centered cubic phase interval of two metals, the diffusion rate and equipment heating temperature limitation are combined, the heating temperature is required to be 950-1100 ℃, and the gap between the two metals is easily eliminated because the thermal expansion coefficient of the vanadium alloy is slightly larger than that of pure titanium. The reduction is recommended to be between 0.5 and 1.5cm due to the difference in strength of the two metals at high temperature, and the higher the temperature, the smaller the reduction is recommended. After forging, sand is buried and cooled to reduce residual stress and crack defects caused by martensite phase transformation near the interface.
3) And (3) carrying out isothermal treatment on the titanium-coated vanadium component after forging at a certain temperature in a vacuum heat treatment furnace to further purify the vanadium alloy. The high-temperature service component can be directly used, and the coated titanium is used for absorbing impurity elements in the vanadium alloy for a long time under the service condition. The vacuum degree of the vacuum heat treatment furnace is 10-3Pa, and the heat treatment temperature is between 1000 and 1150 ℃. If the titanium layer needs to be removed, mechanical stripping combined with grinding wheel cleaning can be adopted.
The heat-treated sample was polished and subjected to 95% acetic acid+ 5% perchloric acid electropolishing (60V,10-20s), etching (HF + HNO)3+3Glycerinum) it can be observed that the metal on one side of pure titanium has a needle-like or strip-like precipitated phase distribution, indicating that the impurity elements are continuously absorbed by the pure titanium metal and solidified in the precipitated phase mode. And due to the Kendall effect, vanadium atoms can be diffused into metal titanium, while titanium atoms are difficult to diffuse into the vanadium alloy, so that the vanadium alloy matrix is protected from being influenced by diffusion.
According to the invention, a high-purity titanium metal plate (99.9%) is processed into a cuboid sealing sheath by using vacuum electron beam welding, vanadium alloy matched with the high-purity titanium metal plate is subjected to vacuum sealing by using electron beam welding again, the processed titanium alloy sheath is subjected to pressure processing at high temperature, a connecting gap between two metals is extruded, and isothermal heat treatment is carried out for a certain time to form a Ti-V approximate binary system diffusion coupler. At the temperature higher than 882.5 ℃, pure titanium and vanadium alloy have similar lattice parameters in a body-centered cubic structure, V and Ti can be infinitely solid-dissolved in the phase interval, and the alloy elements have relatively higher diffusion rate in the body-centered cubic structure. By utilizing the influence of the concentration chemical potential of impurity elements in metals on two sides and the higher affinity of Ti atoms to C, N, O elements in the aging process at high temperature (>882.5 ℃) for a certain time, the pure titanium metal absorbs the impurity elements (C, N, O) in the vanadium alloy and forms needle-shaped or strip-shaped precipitated phase Ti- (CNO) in the pure titanium, thereby reducing the content of the impurity elements in the vanadium alloy. Meanwhile, the diffusion rate of the substitution type element (V, Ti) is low in the body-centered cubic system relative to the diffusion rate of the interstitial type impurity element (C, N, O), and the substitution type element and the interstitial type impurity element mutually diffuse only in a local region of the interface to form a V-Ti diffusion connection joint. And due to the kirkendall effect, only a small part of Ti atoms in the pure titanium can diffuse into the vanadium alloy. Therefore, after subsequent heat treatment and in the service process, the vanadium alloy base metal can be ensured not to be greatly influenced. The solubility of the impurity element (C, N, O) in alpha-Ti is higher than that in beta-Ti, and in the subsequent cooling process, the phase transition point of beta → alpha of the pure titanium region far away from the interface region is higher than that of the pure titanium near the interface region (relatively more V content and beta stabilizing element exist), so when the phase transition point enters the alpha phase interval far away from the interface region, the phase transition point still stays in the beta phase region near the interface region, the impurity element is more easily diffused into the alpha phase interval, and a great amount of Ti- (CNO) precipitates are formed.
The method has the advantages that the pure titanium sheath can be used for protecting the vanadium alloy from being influenced by impurity elements in the air in the mechanical hot processing process, impurities in the vanadium alloy can be continuously removed through subsequent heat treatment, harmful phases are not formed in the vanadium alloy, and the method does not influence the performance of a vanadium alloy matrix. The adsorption process of the titanium-vanadium connection interface system can be carried out under special heat treatment conditions, and can also be continuously carried out under high-temperature service conditions.
The invention can adsorb impurity elements in certain alloys by diffusion of the impurity interstitial elements in a solid state, namely, for certain alloys which are possibly greatly influenced by the impurity interstitial elements, the purity of the certain alloys can be hardly ensured by using a traditional method in the smelting and hot working processes. And selecting a pure metal with stronger affinity with the impurity elements to form a diffusion connection interface, and utilizing the stronger affinity of the metal to adsorb the impurity elements (C, N, O) in the target alloy to form a precipitated phase or an intermetallic compound in the pure metal in subsequent heat treatment or under high-temperature service conditions so as to continuously purify the target alloy.
Drawings
FIG. 1 is an optical microstructure of a sample of example 1 of a diffusion bonding interface composite layer of the present invention in a forged state,
FIG. 2 shows the scanning microstructure and corresponding energy spectrum distribution of the sample of example 1 of the diffusion bonding interface composite layer of the present invention after being subjected to a heat treatment of 1000 deg.C/4 h after forging,
fig. 3 is a schematic diagram illustrating the concept of removing impurity elements from an alloy by solid state diffusion bonding according to the present invention.
Detailed Description
According to the specific embodiment of the invention, an Olympus BX51 metallographic microscope (OM) and a ZEISS ULTRA-55 Scanning Electron Microscope (SEM) are adopted to observe the tissue morphology of the diffusion joint, and the distribution of the components of the diffusion joint is characterized by combining an energy spectrum (EDS).
Example 1
In the example, the vanadium alloy comprises V-3.08Cr-2.58Ti-0.32Y, the impurity element contents are respectively C-0.018%, N-0.014% and O-0.0093%, the purity of the pure titanium metal plate is 99.9%, and the thickness of the pure titanium metal plate is 0.5 cm. The pure titanium metal plate was wire cut to produce two 5 × 5cm square plate-like test specimens and four 5 × 10cm rectangular plate-like test specimens. The vanadium alloy wire was cut into 4 × 9cm rectangular parallelepiped, all the raw materials were cleaned with alcohol, and all the raw materials were electropolished with 95% acetic acid + 5% perchloric acid solution at 60V for 15 s. A sealed capsule of pure titanium of size 5 x 10cm was machined using vacuum electron beam welding and the vanadium alloy was sealed therein. Forging and pressing are carried out at a high temperature of 1150-950 ℃ so as to eliminate a gap between the two metals by extrusion and ensure that the connecting joint has no defects. After forging, sand burying cooling is selected to reduce the cooling speed, so that the defects of overlarge residual stress, cracks caused by martensite transformation of an interface region and the like are prevented. A plurality of pure titanium sealing sheaths are processed by the process for subsequent heat treatment at different temperatures and different times. The subsequent heat treatment is carried out by wrapping one of the pure titanium sheaths in a vacuum heat treatment furnace, the heat preservation temperature is 1000 ℃, the time is 4 hours, and the air pressure in the vacuum furnace is less than 10-3Pa. The forged and heat-treated ti-rice composite diffusion layer was wire-cut into a 1 × 1cm small sample, and the side surface thereof was polished, and etched using a hydrofluoric acid + nitric acid + glycerol solution (volume ratio 1:1:3), and the microstructure obtained was as shown in fig. 1 and 2, respectively. It can be observed that a large amount of acicular precipitated phases are distributed on the substrate on the side of pure titanium far from the interface, while no such precipitated phases appear on the side of pure titanium near the interface, and the energy spectrum of fig. 2 illustrates that the titanium element in pure titanium diffuses less into the vanadium alloy substrate, thereby ensuring that the vanadium alloy substrate is not substantially affected by the diffusion conditions. The core idea to be explained in the invention is shown in fig. 3, namely, the impurity elements in some alloys can be adsorbed by diffusion of impurity interstitial elements in a solid state, namely, the impurities possibly suffered from the impurities are interstitially adsorbedCertain alloys with great influence of elements can be difficult to ensure the purity of the alloy by using the traditional method in smelting and hot working processes. And selecting a pure metal with stronger affinity with the impurity elements to form a diffusion connection interface, and utilizing the stronger affinity of the metal to adsorb the impurity elements (C, N, O) in the target alloy to form a precipitated phase or an intermetallic compound in the pure metal in subsequent heat treatment or under high-temperature service conditions so as to continuously purify the target alloy.
Claims (4)
1. A processing method for removing impurity elements in vanadium alloy by vanadium-titanium connection is characterized by comprising the following processing steps:
step 1, polishing a pure titanium metal plate by using sand paper, washing the pure titanium metal by using alcohol after polishing, and cleaning the surface of the cut vanadium alloy by using alcohol;
step 2, processing the pure titanium metal plate into a cuboid sealing sheath with a proper size by using electron beam welding, plugging the vanadium alloy, and performing vacuum electron beam sealing welding again;
step 3, performing hot-pressure processing on the welded titanium clad sleeve by using forging equipment to extrude a connecting gap between the two metals; the selected pressure processing temperature is higher than 882.5 ℃, and after forging, sand burying and cooling are selected;
step 4, aging the obtained titanium and vanadium of the V-Ti binary diffusion coupling system at a temperature higher than 882.5 ℃ by a vacuum heat treatment furnace to further promote the diffusion of elements to reduce the content of impurity elements in the vanadium alloy matrix, and continuously reduce the generation of precipitated phases in the vanadium alloy under the actual service condition to ensure the safety of the reactor in service under the high-temperature condition; when the titanium coating needs to be removed, mechanically stripping and cleaning a grinding wheel on the bonding surface;
carrying out isothermal treatment on the titanium-coated vanadium component after forging at a certain temperature in a vacuum heat treatment furnace to further purify the vanadium alloy; the components in high-temperature service can be directly used, and the coated titanium is used for absorbing impurity elements in the vanadium alloy for a long time under the service condition; if the titanium layer needs to be removed, mechanical stripping is adopted to be combined with a grinding wheel for cleaning;
the vacuum degree of the vacuum heat treatment furnace is 10-3Pa, and the heat treatment temperature is between 1000 and 1150 ℃.
2. The method for removing impurity elements in vanadium-titanium alloy according to claim 1, wherein the high-temperature service component is directly serviced, and the coated titanium is used to absorb the impurity elements in the vanadium alloy for a long time under the service condition.
3. The method as claimed in claim 1, wherein step 2 is to plate a layer of pure titanium on the surface of the vanadium alloy after electropolishing by plating, and the plating time is controlled according to the required thickness; and simultaneously, the pure titanium coating is promoted to absorb impurity elements in the vanadium alloy under the vacuum heat treatment condition according to requirements.
4. The treatment method for removing impurity elements in vanadium alloy through vanadium-titanium connection as claimed in claim 1, characterized by comprising the following steps:
(1) processing a pure titanium plate with the thickness of 0.5cm by utilizing linear cutting, and processing the pure titanium metal plate into a cuboid shell by utilizing electron beam welding; processing the vanadium alloy into a size matched with the shell, and sealing the vanadium alloy in the pure titanium sheath by using electron beam welding again; after each linear cutting, the cutting surface of the wire is polished by diamond abrasive paper to reduce the roughness of the surfaces of two metals, reduce the defects of an interface area after connection and clean by using alcohol; cutting vanadium alloy wire into 4 x 9cm3The size of the cuboid is just matched with the size of the inner space of the pure titanium sheath;
(2) forging the processed pure titanium sheath at high temperature to reduce the contact gap between the two metals, wherein the forged surface is the front surface of a cuboid, and the reduction is 10-30%; the heating temperature is required to be in a body-centered cubic phase temperature range of two metals, and is limited by combining the diffusion rate and the equipment heating temperature, the heating temperature is required to be 950-1100 ℃, and the reduction is 0.5-1.5 cm; after forging and pressing are finished, sand is selected to be embedded and cooled;
(3) carrying out isothermal treatment on the titanium-coated vanadium component after forging in a vacuum heat treatment furnace to further purify the vanadium alloy; the vacuum degree of the vacuum heat treatment furnace is 10-3Pa, and the heat treatment temperature is between 1000 and 1150 ℃.
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| US3802939A (en) * | 1971-03-22 | 1974-04-09 | Kobe Steel Ltd | Surface-hardened titanium or zirconium and their alloys and method of processing same |
| US4610720A (en) * | 1984-05-16 | 1986-09-09 | The United States Of America As Represented By The Department Of Energy | Method for preparing high purity vanadium |
| CN103667746B (en) * | 2013-11-04 | 2014-10-22 | 宝鸡市嘉诚稀有金属材料有限公司 | Preparation method of pure vanadium ingot |
| CN106756375B (en) * | 2017-01-03 | 2018-05-18 | 北京科技大学 | A kind of vanadium alloy composite material and preparation method thereof |
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2018
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