CN112795798A - Preparation method of titanium alloy plate - Google Patents
Preparation method of titanium alloy plate Download PDFInfo
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- CN112795798A CN112795798A CN201911108305.3A CN201911108305A CN112795798A CN 112795798 A CN112795798 A CN 112795798A CN 201911108305 A CN201911108305 A CN 201911108305A CN 112795798 A CN112795798 A CN 112795798A
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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Abstract
The invention discloses a preparation method of a titanium alloy plate. Preparing a TC4 casting blank by adopting a plasma-vacuum consumable arc combined process; the first fire finish forging is carried out at 880 ℃, and the deformation is 60-75%; performing secondary fire finish forging at 850 ℃ and the deformation of 25-65%; and the third fire finish forging is carried out at 800 ℃, and the deformation is 45-75%. Rolling a 20mm finished plate, wherein the pass deformation is 4-6mm, and reversing rolling is performed when the deformation is 50%; when rolling a 2-10mm plate strip, hot rolling and then warm rolling are carried out, wherein the first-fire rolling temperature is 960 ℃ minus 1050 ℃, the second-fire rolling temperature is 950 ℃ minus 1000 ℃, and the third-fire and fourth-fire adopt warm rolling processes. The annealing temperature is 600-650 ℃, and the heat preservation time is 5-10 h. The invention removes impurities by high-temperature melting, dissolving, flotation and sedimentation, removes gas by using a partial pressure principle, reduces the burning loss of low-melting-point alloy element aluminum, omits an electrode preparation process, simplifies the production process, can directly use titanium residue, reduces the ingot casting cost, has uniform fine grain structure, and has the advantages of wide processing temperature range, good plate strength, plasticity and fracture toughness matching property and the like.
Description
Technical Field
The invention relates to titanium and titanium alloy processing, belongs to the technical field of non-ferrous metal pressure processing, and particularly relates to a preparation method of a titanium alloy plate.
Background
Ti-6Al-4V is the first two-phase (alpha + beta) titanium alloy to be developed and used most widely, and because the melting temperature of the titanium alloy exceeds 1800 ℃, and at high temperature, the titanium is easy to react with oxygen, hydrogen, water vapor, carbon dioxide and metal oxygen in the environmentCompound Fe2O3、 SiO2The alloy is caused to absorb oxygen, increase hydrogen, increase iron and silicon. The content of impurities such as iron, oxygen, hydrogen and the like in the titanium alloy is high under the influence of the high-temperature metallurgical property of the titanium alloy, and the upper limit of the allowable iron, oxygen and hydrogen of the alloy is as follows according to the national standard requirement: fe: 0.3% max; o: 0.2% max; h: 0.015% max. Because part of iron and oxygen exist in the titanium alloy matrix in the form of coarse metal compounds, and part of hydrogen exists in the titanium alloy matrix in the form of fine dispersed bubbles, the metallurgical defects of the alloy matrix are increased.
At present, the Ti-6Al-4V alloy is smelted by mainly adopting a consumable electrode smelting process for 2-4 times, the smelting process has two influences on the smelting process of the Ti-6Al-4V alloy and the quality of cast ingots, firstly, the titanium alloy liquid is smelted and purified by electric arc smelting at the high temperature of 5000 ℃ and the high vacuum of 0.001-0.01Pa, the volatilization loss of the metal aluminum with low melting point is extremely large in the smelting process of the alloy, the production cost is increased, and the control of the alloy components is extremely difficult. Secondly, the consumable electrode smelting process has shallow metal melting bath and extremely short time for keeping the alloy in a liquid state, and high-density and low-density impurities existing in the alloy can not be effectively removed, are sources of alloy crack initiation and crack propagation, are important reasons for causing the failure of aircraft structural parts, reduce the plasticity and the processing performance of the alloy and shorten the service life of the alloy.
The TC4 alloy adopts near-beta forging and near-beta heat treatment process, can improve damage tolerance performance, and the processing technology is characterized in that the temperature control requirement in the processing process is very strict due to the close relationship between the beta process and the deformation process of the alloy. The titanium alloy has poor heat conductivity, deformation generated in the hot working process can not be easily and effectively led out, and is influenced by deformation heat effect, the local area of the workpiece is extremely easy to have overhigh temperature in the working process, so that the local area of the alloy is overheated, overburning and thick in structure, and the performance and quality of the alloy are unstable due to uneven structure.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the preparation method of the high-quality titanium alloy plate, which is convenient to operate and controllable in process, improves the fracture toughness of the alloy and improves the processing performance and the use performance of the alloy.
The technology adopts a plasma cold hearth furnace to carry out TC4 alloy one-time smelting, high-density and low-density impurities in the TC4 alloy are melted and dissolved through high temperature generated by plasma, the impurities which can not be removed are solidified in a skull of the cold hearth through the mechanisms of flotation and sedimentation, and are removed from titanium alloy liquid, pure titanium alloy liquid with uniform temperature and components is obtained, and the titanium alloy liquid is cast into a primary ingot. The TC4 alloy is twice smelted by vacuum self-consuming arc smelting process, and the harmful gas impurities in the alloy are removed by high temperature and high vacuum generated during vacuum smelting.
The method adopts the plasma cold hearth furnace to carry out the primary smelting of the TC4 alloy, omits the electrode preparation process, simplifies the production process, can directly utilize titanium residue and reduces the production cost of cast ingots.
When the plasma cold bed smelting-vacuum consumable arc combined smelting process is adopted, the furnace pressure is increased by introducing pure argon or helium protective atmosphere into a furnace chamber, so that the burning loss of low-melting-point alloy element aluminum is reduced, and gas impurities and low-melting-point impurities in the alloy are removed by improving the purity of protective gas and utilizing the partial pressure principle. Before the titanium alloy is smelted by adopting the process, the furnace burden is subjected to alkali washing, acid washing and vacuum drying to remove grease and water in the raw materials, so that gas, oxide and nitride inclusions brought by the furnace burden can be effectively reduced.
The method utilizes the advantages of smaller deformation resistance and better plasticity of the TC4 alloy during rolling in the beta phase region, adopts rolling in the beta phase region, simultaneously ensures that the deformation of the alloy in the alpha + beta phase region reaches 30-40 percent, avoids reserving coarse grains in metal when the beta phase region is finished processing, reduces the mechanical property of the plate, and can obtain uniform fine-grained structure and higher mechanical property.
The method comprises the steps of forging and cogging TC4 alloy cast ingots before rolling, selecting cogging temperature of 1100 ℃, and completing cogging in three firing times. The cogging adopts a two-stage ingot heating process of slow heating at low temperature and fast heating at high temperature, so that the temperature difference stress of the ingot can be reduced, the retention time of the ingot at high temperature can be shortened, the pollution of gas to the ingot is reduced, and the total heat preservation time is 6 hours.
The process of the third forging comprises the following steps:
first hot forging, wherein the heating temperature is 1050-1100 ℃, and the finish forging temperature is as follows: 880 ℃, deflection: 60 to 75 percent.
Second fire forging, wherein the heating temperature is 1000-1080 ℃, and the finish forging temperature is as follows: 850 ℃, deformation: 25 to 65 percent.
And third hot forging, wherein the heating temperature is 900-1000 ℃, and the finish forging temperature is as follows: 800 ℃, deformation: 45 to 75 percent.
The method uses pure titanium to coat the rolling plate blank, improves the process plasticity of the TC4 alloy and improves the pass processing rate. In order to prevent the titanium blank from being oxidized and air-absorbed at high temperature, before rolling, the surface of the titanium blank is coated with an anti-oxidation coating, and the coating comprises the following components: SiO 22:37％、 B2O3:8.0％；Na2O：30％；TiO2:25％。
The plate is rolled in a four-roller reversible hot rolling mill, and the hot rolled plate with the finished product of more than 10mm adopts a hot rolling process. For example, a 20mm rolled sheet is used, and a 200mm thick sheet blank is heated by induction heating. The rolling temperature is 50-80 ℃ lower than the forging temperature, the first fire rolling temperature is 960-1050 ℃, the pass processing rate is not more than 15%, the final rolling temperature is 880 ℃, and the plate blank is rolled to the thickness of 50mm by one fire. Second hot rolling temperature: 950 ℃ and 1000 ℃, preserving the heat for 45 minutes, controlling the pass deformation at 4-6mm, controlling the final rolling temperature at 860 ℃, and rolling the plate blank to the thickness of 20mm of the finished product by using two fires. When the rolling deformation reaches 50%, reversing rolling is needed to prevent the groove-shaped defects caused by uneven deformation on the surface of the finished plate.
When the method is adopted to roll the plate and strip with the thickness of 2-10mm, the process of hot rolling and warm rolling is adopted, so that the deformation and the total deformation degree of the plate and strip blank can be ensured, the harm of high-temperature hot rolling harmful gas to the surface of the plate is reduced, and the intermediate annealing process of cold rolling is avoided. Taking a rolled finished product as a plate with the thickness of 3.2mm as an example, a plate blank with the thickness of 150mm is firstly hot rolled and then warm rolled, an induction heating process is adopted, the first fire rolling temperature is 960-. Second hot rolling temperature: 950 ℃ and 1000 ℃, the finishing temperature is 860 ℃, and the plate blank is rolled to the thickness of 10mm by two times of fire. The warm rolling process is adopted for the three and four fires. The warm rolling adopts induction heating, the heating time is 18-26 minutes, the blank heating temperature is 720-740 ℃, the plate blank is rolled to the thickness of 5mm by three fire, and the plate blank is rolled to the size of 3.2mm by four fire.
The method is characterized in that the plate after warm rolling is subjected to vacuum annealing, the plate and strip are degreased and cleaned, then the plate and strip are vacuumized and replaced by helium, and a sectional heating mode is adopted. When the temperature is raised to 500 ℃, the circulating fan is started to strengthen the heat exchange process, and the annealing furnace is kept in an exhaust state, so that the titanium coil is ensured to obtain a clean surface. The annealing temperature is 600-650 ℃, and the heat preservation time is 5-10 h.
The above purpose is realized by the following scheme:
the preparation method of the titanium alloy plate is characterized by comprising the following preparation steps:
1. casting a titanium alloy ingot: the alloy casting comprises the following steps
The high-quality 0-grade sponge titanium with impurity content not more than 0.3% and titanium content not less than 99.7%, double 0-grade electrolytic aluminum ingots and Al-80V intermediate alloy are selected as raw materials. As the granularity of the raw materials is too large, alloy components are easy to segregate and mix, before the raw materials are processed, an electrolytic aluminum ingot needs to be sheared into lump materials with the granularity of 8-12.7mm for later use, and the Al-80V intermediate alloy needs to be crushed and sieved to the granularity of 3-12.7mm for later use.
The prepared electrolytic aluminum, the aluminum-vanadium intermediate alloy and the titanium sponge are sent into a drying furnace for drying, the drying of all the raw materials adopts a vacuum drying method, and the drying and drying conditions are as follows: the vacuum degree is 5Pa, the drying temperature is 120-180 ℃, and the temperature is kept for 4-6 h. The drying and drying aims to remove the adsorbed moisture in the raw materials, and the raw materials are directly discharged from the furnace after the drying and drying are finished.
And thirdly, the ingredients are a key process for obtaining high-quality ingots with qualified impurities and components and uniformly distributed components. The sponge titanium, the electrolytic aluminum lump material and the Al-V intermediate alloy are mixed according to the proportion required by the alloy process, and the influence of the burning loss and segregation of alloy elements on the structure and components of the cast ingot is considered during the material mixing. The prepared furnace burden is used as a raw material, the plasma cold hearth furnace smelting is carried out in a 3200kw plasma beam cold hearth furnace, the furnace pressure is controlled within the range of 25-120kPa during smelting, and the smelting loss of the metallic aluminum is reduced. Melting a primary titanium alloy ingot by using a 900kw high-energy plasma gun as a heat source, refining the molten titanium alloy liquid twice by using two 800kw plasma guns as the heat source, solidifying the impurities which cannot be removed in a skull of a cooling furnace bed through the mechanisms of flotation and sedimentation by melting and dissolving high-density and low-density impurities in the alloy at high temperature, removing the impurities from the titanium alloy liquid to obtain the pure titanium alloy liquid with uniform temperature and components, transferring the purified titanium alloy liquid to a water-cooled crystallizer, introducing water into the crystallizer for cooling to obtain the primary titanium alloy ingot, cooling the ingot to below 400 ℃, and discharging the ingot.
Fourthly, carrying out secondary smelting on the alloy by using a 2000kw consumable electrode arc furnace, using the alloy residual material with the same mark as an electrode bottom pad, loading an arc striking material on the bottom pad, vacuumizing to 0.001-0.01Pa in advance after the charging is finished, and welding the consumable electrode and the auxiliary electrode together. The no-load voltage of the electric arc furnace is adjusted to 70V, and arc discharge is generated by means of instant contact between the electrode and the arc-striking agent, so that the electric arc burns stably and a metal molten pool is formed quickly. And then, closing the vacuum valve, and filling 18-20kPa argon or helium into the furnace chamber to carry out protective atmosphere smelting, thereby reducing the smelting loss of aluminum. By improving the purity of the protective gas and utilizing the partial pressure principle, the volatile gas and low-melting-point impurities of the alloy in a high-temperature state are removed. The smelting voltage is adjusted to 35-40V, and the smelting current is adjusted to 9300A-9600A. In order to reduce shrinkage cavities and loosening areas at the head of the ingot and improve the yield of the ingot, the ingot needs to be capped in the later stage of smelting, the current in the capping stage is gradually reduced from 3500A to about 900A, and the capping time accounts for one third of the whole smelting stage. And after the capping is finished, cooling the cast ingot to below 400 ℃ and discharging. By adopting a plasma cold bed smelting-vacuum consumable arc smelting combined smelting process, the high-quality ingot with low gas and low melting point inclusion and high-density and low-density inclusion effectively removed is obtained.
2. Forging and cogging: the TC4 alloy cast ingot has a coarse structure and low deformability, is easy to crack when being directly rolled, and is required to be forged and cogging before rolling, wherein the cogging temperature is generally 150 ℃ above the beta transition temperature and 250 ℃, and the cogging temperature is 1100 ℃ selected in the process. The ingot is heated under the condition of micro-oxidation atmosphere by using coal gas, natural gas, butane and the like as fuels. The cogging is completed by three times of heating.
The surface of the cast ingot is coated with an anti-oxidation coating, after the cast ingot is charged at 900 ℃ and heated to 1100 ℃, because the TC4 alloy has low heat conductivity coefficient at low temperature and high heat conductivity coefficient at high temperature, and is easily polluted by N2, O2, H2 and the like at high temperature, in order to prevent the cracking of the cast ingot caused by the core surface temperature difference stress in the heating process and reduce the pollution of high-temperature harmful gas to the cast ingot, the process adopts a two-section cast ingot heating process, adopts slow heating at low temperature and quick heating at high temperature, can reduce the temperature difference stress of the cast ingot, can shorten the retention time of the cast ingot at high temperature and reduce the pollution of gas to the cast ingot, and the total heat preservation time is 6H, and then the cast ingot is taken out of the.
The forging cogging adopts a free forging process, cogging is carried out on a 2500-ton hydraulic press, tapping and quick-beating are carried out when forging is started, and the contact time of a casting blank and a lower anvil is reduced as much as possible so as to reduce the occurrence of cold edges and surface cracks of the casting blank. The deformation degree of each forging is not more than 5% -8%, the primary coarse grain structure of casting is initially broken, and the plasticity is improved. Then the hammering force is gradually increased to increase the deformation degree, and the forging deformation degree is controlled within the range of 20-30%. The extension forging is repeated to refine the coarse structure at the center of the ingot, and the temperature of the forging stock should be 950-1000 ℃ after the structure grains are refined. During forging, local temperature rise caused by deformation heat effect is noticed, and the phenomenon that the local temperature of the cast ingot rises to cause the cast ingot to generate uneven microstructure is avoided. And finishing the first hot forging after three times of upsetting. Performing secondary fire forging, keeping the temperature at 1000 ℃ for 4 hours, and performing unidirectional drawing forging; and performing third-time forging, keeping the temperature at 950 ℃ for 3 hours, and performing unidirectional drawing.
The process of the third forging comprises the following steps:
first hot forging, wherein the heating temperature is 1050-1100 ℃, and the finish forging temperature is as follows: 880 ℃, deflection: 60 to 75 percent.
Second fire forging, wherein the heating temperature is 1000-1080 ℃, and the finish forging temperature is as follows: 850 ℃, deformation: 25 to 65 percent.
And third hot forging, wherein the heating temperature is 900-1000 ℃, and the finish forging temperature is as follows: 800 ℃, deformation: 45 to 75 percent.
3. Plate blank preparation: the cogging forged blank is cut into square plate blanks, and the square plate blanks are freely forged on an air hammer. In order to improve the process plasticity of the TC4 alloy and increase the pass processing rate, a layer of pure titanium can be coated on the forged plate blank before rolling. In order to prevent the titanium blank from being oxidized and air-absorbed at high temperature, before rolling, the surface of the titanium blank is coated with an anti-oxidation coating, and the coating comprises the following components: SiO 22:37％、 B2O3:8.0％；Na2O：30％；TiO2:25％。
4. Plate preparation: the slab is hot rolled in a phi 600 mm/phi 1350 x 1200 four-roller reversible hot rolling mill, and when the finished product is a hot rolled thick plate with the thickness of 20mm, the slab with the thickness of 200mm is used and is heated by induction. The rolling temperature is 50-80 ℃ lower than the forging temperature, and the first firing rolling temperature is 960-1050 ℃. When rolling is started, the pass deformation is controlled to be 3-4mm, the pass processing rate is not more than 15%, the final rolling temperature is 880 ℃, and the plate blank is rolled to be 50mm thick by one fire. Second hot rolling temperature: 950 ℃ and 1000 ℃, preserving the heat for 45 minutes, controlling the pass deformation at 4-6mm, controlling the finish rolling temperature at 860 ℃, and rolling the plate blank to the thickness of 20mm by using two fires. And (4) processing the plate by a surface planing and milling machine, inspecting, packaging and warehousing. When the TC4 alloy thick plate is rolled, when the unidirectional rolling deformation reaches 50%, reversing rolling is needed to prevent the groove-shaped defect caused by uneven deformation on the surface of the finished plate.
When the rolled finished product is a plate with the thickness of 3.2mm, a plate blank with the thickness of 150mm is firstly hot rolled and then warm rolled. An induction heating process is adopted, the first-time rolling temperature is 960-1050 ℃, the pass deformation is controlled to be 3-4mm when rolling is started, the final rolling temperature is 880 ℃, and the plate blank is rolled to be 30mm thick by one time. Second hot rolling temperature: 950 ℃ and 1000 ℃, preserving the heat for 45 minutes, controlling the pass deformation at 4-6mm, controlling the final rolling temperature at 860 ℃, and rolling the plate blank to the thickness of 10mm by using two fires.
The warm rolling process is adopted by the third fire and the fourth fire, so that the deformation and the total deformation degree of the plate and strip blank can be ensured, the damage of high-temperature hot rolling harmful gas to the surface of the plate is reduced, and the intermediate annealing process of cold rolling is avoided. The warm rolling adopts induction heating, the heating time is 18-26 minutes, the blank heating temperature is 720-740 ℃, the plate blank is rolled to the thickness of 5mm by three fire, and the plate blank is rolled to the size of 3.2mm by four fire. Annealing the warm-rolled plate in vacuum, and washing rolling oil on the surface of the plate in alkali liquor before annealing. After vacuumizing, helium is used for replacement, and then a sectional heating mode is adopted to relieve the temperature difference between the inner part and the surface of the coil. When the temperature rises, a circulating fan of the annealing furnace needs to be started, and the heat exchange process is strengthened through convective heat transfer. Before 500 ℃, the annealing furnace is kept in a gas-exhausting state to ensure that the titanium coil obtains a clean surface. The annealing temperature is 600-650 ℃, and the heat preservation time is 5-10 h. And (4) carrying out alkali washing, acid washing, surface defect coping, inspection, packaging and warehousing on the annealed strip coil.
The invention has the characteristics that: the method adopts a plasma cold bed smelting-vacuum consumable electric arc combined smelting process, high-density and low-density impurities in TC4 alloy are melted and dissolved through high temperature generated by plasma, the impurities which can not be removed are solidified in a solidified shell of a cold bed through flotation and sedimentation mechanisms, and harmful gas impurities in the alloy are removed through high temperature and high vacuum generated during vacuum consumable electric arc smelting. The preparation process of the electrode is omitted, the production process is simplified, the titanium residue can be directly utilized, and the production cost of the cast ingot is reduced. The furnace pressure is improved by introducing pure argon or helium protective atmosphere into the furnace chamber, the burning loss of the low-melting-point alloy element aluminum is reduced, and gas impurities and low-melting-point impurities in the alloy are removed by improving the purity of the protective gas and utilizing the partial pressure principle. By utilizing the advantages of smaller deformation resistance and better plasticity of the TC4 alloy during rolling in the beta phase region, the rolling in the beta phase region is adopted, and meanwhile, the deformation of the alloy in the alpha + beta phase region is ensured to reach 30-40%, so that coarse grains are prevented from being reserved in metal when the beta phase region is finished, the mechanical property of the plate is reduced, and uniform fine grain structure and higher mechanical property can be obtained. The hot rolled plate with the thickness of more than 10mm adopts forging cogging and hot rolling processes, the plate strip with the thickness of 2-10mm adopts forging cogging and hot rolling initial rolling, and then the warm rolling process is carried out.
The method has the advantages of wide processing temperature range, uniform and controllable plate structure, capability of fully exerting the performance advantages of the dual-phase titanium alloy, better matching of strength, plasticity and fracture toughness of the processed plate and improvement of performance stability of different batches of plates.
Detailed Description
Example the production process of TC4 plate with thickness of 20mm and thickness of 3.2mm is as follows:
the above purpose is realized by the following scheme:
1. casting a titanium alloy ingot: the alloy casting comprises the following steps
The high-quality 0-grade sponge titanium with impurity content not more than 0.3% and titanium content not less than 99.7%, double 0-grade electrolytic aluminum ingots and Al-80V intermediate alloy are selected as raw materials. As the granularity of the raw materials is too large, alloy components are easy to segregate and mix, before the raw materials are processed, an electrolytic aluminum ingot needs to be sheared into lump materials with the granularity of 8-12.7mm for later use, and the Al-80V intermediate alloy needs to be crushed and sieved to the granularity of 3-12.7mm for later use.
The prepared electrolytic aluminum, the aluminum-vanadium intermediate alloy and the titanium sponge are sent into a drying furnace for drying, the drying of all the raw materials adopts a vacuum drying method, and the drying and drying conditions are as follows: the vacuum degree is 5Pa, the drying temperature is 120-180 ℃, and the temperature is kept for 4-6 h. The drying and drying aims to remove the adsorbed moisture in the raw materials, and the raw materials are directly discharged from the furnace after the drying and drying are finished.
And thirdly, the ingredients are a key process for obtaining high-quality ingots with qualified impurities and components and uniformly distributed components. The sponge titanium, the electrolytic aluminum lump material and the Al-V intermediate alloy are mixed according to the proportion required by the alloy process, and the influence of the burning loss and segregation of alloy elements on the structure and components of the cast ingot is considered during the material mixing. The prepared furnace burden is used as a raw material, the plasma cold hearth furnace smelting is carried out in a 3200kw plasma beam cold hearth furnace, the furnace pressure is controlled within the range of 25-120kPa during smelting, and the smelting loss of the metallic aluminum is reduced. Melting a primary titanium alloy ingot by using a 900kw high-energy plasma gun as a heat source, refining the molten titanium alloy liquid twice by using two 800kw plasma guns as the heat source, solidifying the impurities which cannot be removed in a skull of a cooling furnace bed through the mechanisms of flotation and sedimentation by melting and dissolving high-density and low-density impurities in the alloy at high temperature, removing the impurities from the titanium alloy liquid to obtain the pure titanium alloy liquid with uniform temperature and components, transferring the purified titanium alloy liquid to a water-cooled crystallizer, introducing water into the crystallizer for cooling to obtain the primary titanium alloy ingot, cooling the ingot to below 400 ℃, and discharging the ingot.
Fourthly, carrying out secondary smelting on the alloy by using a 2000kw consumable electrode arc furnace, using the alloy residual material with the same mark as an electrode bottom pad, loading an arc striking material on the bottom pad, vacuumizing to 0.001-0.01Pa in advance after the charging is finished, and welding the consumable electrode and the auxiliary electrode together. The no-load voltage of the electric arc furnace is adjusted to 70V, and arc discharge is generated by means of instant contact between the electrode and the arc-striking agent, so that the electric arc burns stably and a metal molten pool is formed quickly. And then, closing the vacuum valve, and filling 18-20kPa argon or helium into the furnace chamber to carry out protective atmosphere smelting, thereby reducing the smelting loss of aluminum. By improving the purity of the protective gas and utilizing the partial pressure principle, the volatile gas and low-melting-point impurities of the alloy in a high-temperature state are removed. The smelting voltage is adjusted to 35-40V, and the smelting current is adjusted to 9300A-9600A. In order to reduce shrinkage cavities and loosening areas at the head of the ingot and improve the yield of the ingot, the ingot needs to be capped in the later stage of smelting, the current in the capping stage is gradually reduced from 3500A to about 900A, and the capping time accounts for one third of the whole smelting stage. And after the capping is finished, cooling the cast ingot to below 400 ℃ and discharging. By adopting a plasma cold bed smelting-vacuum consumable arc smelting combined smelting process, the high-quality ingot with low gas and low melting point inclusion and high-density and low-density inclusion effectively removed is obtained. The size of the No. 1 cast ingot is as follows: and phi 630mm, and the chemical components are (in percentage by mass of elements): al: 6.29 percent; v: 4.03 percent; fe: 0.16 percent; c: 0.033%; n: 0.022%; o: 0.054%; h: 0.011 percent.
The size of the 2# ingot is as follows: phi 500mm, and the chemical components are (in percentage by mass of elements): al: 5.93 percent; v: 3.96 percent; fe: 0.19 percent; c: 0.039%; n: 0.017 percent; o: 0.058%; h: 0.01 percent.
2. Forging and cogging: the TC4 alloy cast ingot has a coarse structure and low deformability, is easy to crack when being directly rolled, and is required to be forged and cogging before rolling, wherein the cogging temperature is generally 150 ℃ above the beta transition temperature and 250 ℃, and the cogging temperature is 1100 ℃ selected in the process. The ingot is heated under the condition of micro-oxidation atmosphere by using coal gas, natural gas, butane and the like as fuels. The cogging is completed by three times of heating, and before each heating, an anti-oxidation coating is coated on the surface of the cast ingot or the blank.
1# and 2# ingot castings are sawed, the sawed short ingots are charged at 900 ℃ and heated to 1100 ℃, because the TC4 alloy has low thermal conductivity at low temperature and high thermal conductivity at high temperature, and the short ingots are easily polluted by N2, O2, H2 and the like at high temperature, the temperature difference stress of the ingots can be reduced for preventing the temperature difference stress of a core surface in the heating process from causing the cracking of the ingots, and the pollution of high-temperature harmful gas to the ingots is reduced.
The forging cogging adopts a free forging process, cogging is carried out on a 2500-ton hydraulic press, tapping and quick-beating are carried out when forging is started, and the contact time of a casting blank and a lower anvil is reduced as much as possible so as to reduce the occurrence of cold edges and surface cracks of the casting blank. The deformation degree of each forging is not more than 5% -8%, the primary coarse grain structure of casting is initially broken, and the plasticity is improved. Then the hammering force is gradually increased to increase the deformation degree, and the forging deformation degree is controlled within the range of 20-30%. The extension forging is repeated to refine the coarse structure at the center of the ingot, and the temperature of the forging stock should be 950-1000 ℃ after the structure grains are refined. During forging, local temperature rise caused by deformation heat effect is noticed, and the phenomenon that the local temperature of the cast ingot rises to cause the cast ingot to generate uneven microstructure is avoided. And finishing the first hot forging after three times of upsetting. Performing secondary fire forging, keeping the temperature at 1000 ℃ for 4 hours, and performing unidirectional drawing forging; and the third heat forging is carried out for 3h at 950 ℃, the forging stock of the 1# cast ingot is unidirectionally drawn to 200mm x 2000mm, and the forging stock of the 2# cast ingot is unidirectionally drawn to 150mm x 1600 mm.
The process of the third forging comprises the following steps:
first hot forging, wherein the heating temperature is 1050-1100 ℃, and the finish forging temperature is as follows: 880 ℃, deflection: 60 to 75 percent.
Second fire forging, wherein the heating temperature is 1000-1080 ℃, and the finish forging temperature is as follows: 850 ℃, deformation: 25 to 65 percent.
And third hot forging, wherein the heating temperature is 900-1000 ℃, and the finish forging temperature is as follows: 800 ℃, deformation: 45 to 75 percent.
3. Plate blank preparation: the forged blank after cogging was cut into square slabs of 200mm 380mm and 150mm 280mm, and freely forged on an air hammer. In order to improve the process plasticity of the TC4 alloy and increase the pass processing rate, a layer of pure titanium can be coated on the forged plate blank before rolling. In order to prevent the titanium blank from being oxidized and air-absorbed at high temperature, before rolling, the surface of the titanium blank is coated with an anti-oxidation coating, and the coating comprises the following components: SiO 22:37％、B2O3:8.0％；Na2O：30％；TiO2:25％。
4. Rolling the plate: the slab is hot rolled in a phi 600 mm/phi 1350 x 1200 four-roller reversible hot rolling mill, and when the finished product is a hot rolled thick plate with the thickness of 20mm, the slab with the thickness of 200mm is used and is heated by induction. The rolling temperature is 50-80 ℃ lower than the forging temperature, and the first firing rolling temperature is 960-1050 ℃. When rolling is started, the pass deformation is controlled to be 3-4mm, the pass processing rate is not more than 15%, the final rolling temperature is 880 ℃, and the plate blank is rolled to be 50mm thick by one fire. Second hot rolling temperature: 950 ℃ and 1000 ℃, preserving the heat for 45 minutes, controlling the pass deformation at 4-6mm, controlling the finish rolling temperature at 860 ℃, and rolling the plate blank to the thickness of 20mm by using two fires. And (4) processing the plate by a surface planing and milling machine, inspecting, packaging and warehousing. When the TC4 alloy thick plate is rolled, when the unidirectional rolling deformation reaches 50%, reversing rolling is needed to prevent the groove-shaped defect caused by uneven deformation on the surface of the finished plate.
When the rolled finished product is a plate with the thickness of 3.2mm, a plate blank with the thickness of 150mm is firstly hot rolled and then warm rolled. An induction heating process is adopted, the first-time rolling temperature is 960-1050 ℃, the pass deformation is controlled to be 3-4mm when rolling is started, the final rolling temperature is 880 ℃, and the plate blank is rolled to be 30mm thick by one time. Second hot rolling temperature: 950 ℃ and 1000 ℃, preserving the heat for 45 minutes, controlling the pass deformation at 4-6mm, controlling the final rolling temperature at 860 ℃, and rolling the plate blank to the thickness of 10mm by using two fires.
The warm rolling process is adopted by the third fire and the fourth fire, so that the deformation and the total deformation degree of the plate and strip blank can be ensured, the damage of high-temperature hot rolling harmful gas to the surface of the plate is reduced, and the intermediate annealing process of cold rolling is avoided. The warm rolling adopts induction heating, the heating time is 18-26 minutes, the blank heating temperature is 720-740 ℃, the plate blank is rolled to the thickness of 5mm by three fire, and the plate blank is rolled to the size of 3.2mm by four fire. Annealing the warm-rolled plate in vacuum, and washing rolling oil on the surface of the plate in alkali liquor before annealing. After vacuumizing, helium is used for replacement, and then a sectional heating mode is adopted to relieve the temperature difference between the inner part and the surface of the coil. When the temperature rises, a circulating fan of the annealing furnace needs to be started, and the heat exchange process is strengthened through convective heat transfer. Before 500 ℃, the annealing furnace is kept in a gas-exhausting state to ensure that the titanium coil obtains a clean surface. The annealing temperature is 600-650 ℃, and the heat preservation time is 5-10 h. And (4) carrying out alkali washing, acid washing, surface defect coping, inspection, packaging and warehousing on the annealed strip coil.
The mechanical properties of the treated plate are shown in table 1, the strength-plasticity-fracture toughness of the plate produced by the process are well matched, the strength reaches more than 923MPa, and the fracture toughness reaches 92MPa/m0.5
TABLE 1 mechanical properties of TC4 alloy sheet
The TC4 alloy plates with the serial numbers of 1 and 2 have the thickness of 20 mm;
the TC4 alloy plates with the serial numbers of 3 and 4 have the thickness of 3.2 mm;
the invention has the characteristics that: the method adopts a plasma cold bed smelting-vacuum consumable electric arc combined smelting process, high-density and low-density impurities in TC4 alloy are melted and dissolved through high temperature generated by plasma, the impurities which can not be removed are solidified in a solidified shell of a cold bed through flotation and sedimentation mechanisms, and harmful gas impurities in the alloy are removed through high temperature and high vacuum generated during vacuum consumable electric arc smelting. The preparation process of the electrode is omitted, the production process is simplified, the titanium residue can be directly utilized, and the production cost of the cast ingot is reduced. The furnace pressure is improved by introducing pure argon or helium protective atmosphere into the furnace chamber, the burning loss of the low-melting-point alloy element aluminum is reduced, and gas impurities and low-melting-point impurities in the alloy are removed by improving the purity of the protective gas and utilizing the partial pressure principle. By utilizing the advantages of smaller deformation resistance and better plasticity of the TC4 alloy during rolling in the beta phase region, the rolling in the beta phase region is adopted, and meanwhile, the deformation of the alloy in the alpha + beta phase region is ensured to reach 30-40%, so that coarse grains are prevented from being reserved in metal when the beta phase region is finished, the mechanical property of the plate is reduced, and uniform fine grain structure and higher mechanical property can be obtained. The hot rolled plate with the thickness of more than 10mm adopts forging cogging and hot rolling processes, the plate strip with the thickness of 2-10mm adopts forging cogging and hot rolling initial rolling, and then the warm rolling process is carried out.
The method has the advantages of wide processing temperature range, uniform and controllable plate structure, capability of fully exerting the performance advantages of the dual-phase titanium alloy, better matching of the properties such as strength, plasticity, fracture toughness and the like of the processed plate, and improvement of the performance stability of different batches of plates.
The processing process flow of the titanium alloy plate is shown in figure 1, and figure 1 shows a TC4 alloy plate production process.
Claims (6)
1. The invention discloses a preparation method of a titanium alloy plate, which adopts a plasma cold hearth furnace to carry out TC4 primary smelting, carries out secondary smelting by a vacuum self-consuming electric arc process, carries out forging cogging on a TC4 alloy cast ingot before rolling, selects the cogging temperature of 1100 ℃, and completes cogging in three fire times; the cogging adopts a two-stage ingot heating process of slow heating at low temperature and fast heating at high temperature, so that the temperature difference stress of the ingot can be reduced, the retention time of the ingot at high temperature can be shortened, the pollution of gas to the ingot is reduced, and the total heat preservation time is 6 hours.
2. According to claim 1, three forging processes are used:
first hot forging, wherein the heating temperature is 1050-1130 ℃, and the finish forging temperature is as follows: 880 ℃, deflection: 60% -75%;
second fire forging, wherein the heating temperature is 1000-1080 ℃, and the finish forging temperature is as follows: 850 ℃, deformation: 25% -65%;
and third hot forging, wherein the heating temperature is 900-1000 ℃, and the finish forging temperature is as follows: 800 ℃, deformation: 45% -75%;
the pure titanium is adopted to coat the rolled plate blank, so that the alloy process plasticity is improved, and the pass processing rate is increased; before rolling, an anti-oxidation coating is coated on the surface of a titanium blank, and the coating comprises the following components: SiO 22:37%、B2O3:8.0%；Na2O：30%；TiO2:25%。
3. According to the claims 1-2, the finished hot rolled plate with the thickness of more than 10mm adopts a hot rolling process; taking rolling a 20mm finished plate as an example, a 200mm thick plate blank is heated by induction; the rolling temperature is 50-80 ℃ lower than the forging temperature, the first fire rolling temperature is 960-1050 ℃, the pass processing rate is not more than 15%, the final rolling temperature is 880 ℃, and the plate blank is rolled to the thickness of 50mm by one fire; second hot rolling temperature: 950 ℃ and 1000 ℃, preserving the heat for 45 minutes, controlling the pass deformation at 4-6mm, controlling the final rolling temperature at 860 ℃, and rolling the plate blank to the thickness of 20mm of the finished product by using two fire; when the rolling deformation reaches 50%, reversing rolling is needed to prevent the groove-shaped defects caused by uneven deformation on the surface of the finished plate.
4. According to the claims 2-3, when the method is adopted to roll the plate and strip with the thickness of 2-10mm, the process of hot rolling firstly and warm rolling secondly is adopted, the harm of the high-temperature hot rolling harmful gas to the surface of the plate is reduced, and the cold rolling intermediate annealing process is avoided; taking a rolled finished product as a plate with the thickness of 3.2mm as an example, hot rolling and then warm rolling are carried out on a plate blank with the thickness of 150mm, an induction heating process is adopted, the first fire rolling temperature is 960-; second hot rolling temperature: 950 ℃ and 1000 ℃, the finishing temperature is 860 ℃, and the plate blank is rolled to the thickness of 10mm by two fires; warm rolling technology is adopted for the three and four fires; the warm rolling adopts induction heating, the heating time is 18-26 minutes, the blank heating temperature is 720-740 ℃, the plate blank is rolled to the thickness of 5mm by three fire, and the plate blank is rolled to the size of 3.2mm by four fire.
5. According to the claims 1-4, the plate after warm rolling is vacuum annealed, the plate and strip are degreased and cleaned, then vacuumized, replaced by helium, and heated in a sectional heating mode; when the temperature is raised to 500 ℃, starting a circulating fan to strengthen the heat exchange process, and keeping the annealing furnace in an exhaust state to ensure that the titanium coil obtains a clean surface; the annealing temperature is 600-650 ℃, and the heat preservation time is 5-10 h.
6. A method for producing a titanium alloy sheet according to claims 1 to 5, comprising the steps of:
(1) the casting of the titanium alloy ingot comprises the following steps:
the surface of the cast ingot is coated with the anti-oxidation coating, after the cast ingot is charged in a furnace at 900 ℃ and the temperature is raised to 1100 ℃, because the TC4 alloy has low thermal conductivity at low temperature and high thermal conductivity at high temperature, and is easy to be N at high temperature2、O2、H2The process adopts a two-section ingot casting heating process, adopts slow heating at low temperature and quick heating at high temperature, can reduce the temperature difference stress of the ingot casting, shorten the retention time of the ingot casting at high temperature, reduce the pollution of gas to the ingot casting, has the total heat preservation time of 6 hours, and then is discharged and forged;
adopting a free forging process, cogging on a 2500-ton hydraulic press, starting forging, tapping and quickly hitting, and reducing the contact time of a casting blank and a lower anvil to the greatest extent so as to reduce the occurrence of cold edges and surface cracks of the casting blank; the deformation degree of each forging is not more than 5% -8%, the primary coarse grain structure of casting is initially broken, and the plasticity is improved; then gradually increasing the hammering force to increase the deformation degree, and controlling the forging deformation degree within the range of 20-30%; repeatedly performing extension forging to refine the coarse structure at the central part of the ingot, wherein after the structure grains are refined, the temperature of the forging stock is preferably 950-1000 ℃; during forging, local temperature rise caused by deformation heat effect is required to be noticed, so that the local temperature rise of the cast ingot is prevented, and the cast ingot is prevented from generating uneven microstructure; finishing the first hot forging after three times of upsetting; performing secondary fire forging, keeping the temperature at 1000 ℃ for 4 hours, and performing unidirectional drawing forging; performing third-time forging, keeping the temperature at 950 ℃ for 3 hours, and performing unidirectional drawing;
the process of the third forging comprises the following steps:
first hot forging, wherein the heating temperature is 1050-1100 ℃, and the finish forging temperature is as follows: 880 ℃, deflection: 60% -75%;
second fire forging, wherein the heating temperature is 1000-1080 ℃, and the finish forging temperature is as follows: 850 ℃, deformation: 25% -65%;
and third hot forging, wherein the heating temperature is 900-1000 ℃, and the finish forging temperature is as follows: 800 ℃, deformation: 45% -75%;
(3) plate blank preparation: cutting the cogging forged blank into a square plate blank, and freely forging on an air hammer; in order to improve the process plasticity of the TC4 alloy and increase the pass processing rate, a layer of pure titanium can be coated on the forged plate blank before rolling; in order to prevent the titanium blank from being oxidized and air-absorbed at high temperature, before rolling, the surface of the titanium blank is coated with an anti-oxidation coating, and the coating comprises the following components: SiO 22:37%、B2O3:8.0%；Na2O：30%；TiO2:25%；
(4) Plate preparation: the slab is hot rolled in a phi 600 mm/phi 1350 x 1200 four-roller reversible hot rolling mill, and when the finished product is a hot rolled thick plate with the thickness of 20mm, the slab with the thickness of 200mm is used for induction heating; the rolling temperature is 50-80 ℃ lower than the forging temperature, and the first fire rolling temperature is 960-1050 ℃; when rolling is started, the pass deformation is controlled to be 3-4mm, the pass processing rate is not more than 15%, the final rolling temperature is 880 ℃, and the plate blank is rolled to be 50mm thick by one fire; second hot rolling temperature: 950 ℃ and 1000 ℃, preserving the heat for 45 minutes, controlling the pass deformation at 4-6mm, controlling the final rolling temperature at 860 ℃, and rolling the plate blank to the thickness of 20mm by using two fire; after the plate is processed by a surface planing and milling machine, the plate is inspected, packaged and put in storage; when the TC4 alloy thick plate is rolled, when the unidirectional rolling deformation reaches 50%, reverse rolling is needed, and the groove-shaped defect caused by uneven deformation on the surface of the finished plate is prevented;
when the rolled finished product is a plate with the thickness of 3.2mm, a plate blank with the thickness of 150mm is firstly hot rolled and then warm rolled; an induction heating process is adopted, the first-time rolling temperature is 960-1050 ℃, the pass deformation is controlled to be 3-4mm when rolling is started, the final rolling temperature is 880 ℃, and the plate blank is rolled to be 30mm thick by one time; second hot rolling temperature: 950 ℃ and 1000 ℃, preserving the heat for 45 minutes, controlling the pass deformation at 4-6mm, controlling the final rolling temperature at 860 ℃, and rolling the plate blank to the thickness of 10mm by using two fire;
the warm rolling process is adopted for the third fire and the fourth fire, so that the deformation and the total deformation degree of the plate and strip blank can be ensured, the damage of high-temperature hot rolling harmful gas to the surface of the plate is reduced, and the intermediate annealing process of cold rolling is avoided; induction heating is adopted for warm rolling, the heating time is 18-26 minutes, the blank heating temperature is 720-; annealing the warm-rolled plate in vacuum, and washing rolling oil on the surface of the plate in alkali liquor before annealing; after vacuumizing, replacing with helium, and then adopting a sectional heating mode to relieve the temperature difference between the interior and the surface of the strip coil; when the temperature is raised, a circulating fan of the annealing furnace is started, and the heat exchange process is strengthened through convective heat exchange; before 500 ℃, the annealing furnace needs to keep an exhaust state to ensure that the titanium coil obtains a clean surface; the annealing temperature is 600-; carrying out alkali washing, acid washing, surface defect coping, inspection, packaging and warehousing on the annealed strip coil;
the invention adopts a plasma cold bed smelting-vacuum consumable arc combined smelting process to melt, dissolve, float and settle impurities; removing alloy gas and low-melting-point impurities by using a partial pressure principle, and reducing the burning loss of a low-melting-point alloy element aluminum; the electrode preparation process is omitted, the production process is simplified, the titanium residue can be directly utilized, and the ingot casting production cost is reduced; the rolling process can ensure that the product obtains uniform fine grain structure and higher mechanical property, and has the advantages of wide processing temperature range, uniform and controllable plate structure, better matching of strength, plasticity and fracture toughness of processed plates, and improved performance stability of different batches of plates.
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