CN111441020A - Method for preparing TC4 titanium alloy sputtering target material at low cost - Google Patents
Method for preparing TC4 titanium alloy sputtering target material at low cost Download PDFInfo
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 84
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000005477 sputtering target Methods 0.000 title claims abstract description 25
- 239000013077 target material Substances 0.000 title claims abstract description 17
- 238000005096 rolling process Methods 0.000 claims abstract description 106
- 238000010438 heat treatment Methods 0.000 claims description 46
- 238000000137 annealing Methods 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 8
- 238000003723 Smelting Methods 0.000 claims description 6
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 claims description 4
- 229910000851 Alloy steel Inorganic materials 0.000 claims 1
- 230000001186 cumulative effect Effects 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000007769 metal material Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 22
- 238000005098 hot rolling Methods 0.000 description 18
- 238000007599 discharging Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 238000005266 casting Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/38—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B37/00—Control devices or methods specially adapted for metal-rolling mills or the work produced thereby
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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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/38—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
- B21B2001/386—Plates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B2201/00—Special rolling modes
- B21B2201/06—Thermomechanical rolling
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Abstract
The invention discloses a method for preparing TC4 titanium alloy sputtering target material with low cost, belonging to the technical field of metal material processing. By a three-fire isothermal rolling method, TC4 titanium alloy ingots smelted by an EB furnace are rolled unidirectionally along the length direction, and the total reduction is 86-90%. The invention not only simplifies the traditional titanium alloy processing process flow and effectively reduces the production cost, but also has good density and uniform microstructure of the prepared TC4 titanium alloy target material, and the mechanical property of the titanium alloy target material meets the requirements of international standards.
Description
Technical Field
The invention belongs to the technical field of metal material processing, and particularly relates to a method for preparing a TC4 titanium alloy sputtering target material at low cost.
Background
The titanium alloy has excellent properties of light weight, high strength, heat resistance, corrosion resistance, ultralow temperature resistance, no magnetism and the like, and is widely applied to the fields of aviation, aerospace, biomedicine and the like. The titanium alloy target is a key material for preparing military top-end weapons and is an important material for improving the traditional civil industry and the technical innovation development. In the coating industry, titanium alloy targets and films are widely used in surface strengthening films for tools, decoration, corrosion resistance and the like, and high-end technology industries such as microelectronics, magnetic recording, semiconductors, thin film resistors and the like.
The quality of the target becomes a critical factor in order to ensure the quality of the deposited film and to improve the sputtering efficiency. Through a large number of domestic and foreign researches, the factors which have the greatest influence on the quality of the sputtering target are as follows: purity, density, dimensional accuracy, grain size, texture, etc. The sputtering target material is mainly prepared by smelting casting and powder metallurgy process. At present, most of the preparation methods of titanium alloy targets are powder metallurgy processes, however, the titanium alloy targets prepared by the method have the defects of high porosity, poor compactness, high cost and the like.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing TC4 titanium alloy sputtering target material with low cost, TC4 titanium alloy is smelted by using an EB furnace, and the titanium alloy sputtering target material prepared by the method has high density, uniform microstructure and low cost.
The technical scheme adopted by the invention is as follows: provides a method for preparing TC4 titanium alloy sputtering target material with low cost. The method is characterized by comprising the following steps:
a. heating TC4 titanium alloy cast slab ingot smelted by an EB furnace to 800-1000 ℃, preserving heat for 30min, and carrying out first heating treatment, wherein the TC4 titanium alloy cast ingot is 8-9 mm in thickness, 120-125 mm in length and 30-35 mm in width;
b. b, performing first hot rolling on the plate obtained in the step a along the length direction of a slab ingot under a two-roller hot rolling mill, wherein the rolling pass is 1 pass, and the rolling deformation is 50-75%;
c. b, heating the plate obtained in the step b in a high-temperature furnace to the same temperature as that in the step a, preserving heat for 30min, and carrying out secondary heating treatment;
d. c, performing second fire rolling on the plate obtained in the step c, wherein the rolling direction is the same as that in the step b, the rolling pass is 1 pass, and the rolling deformation is 17% -55%;
e. heating the plate obtained in the step d in a high-temperature furnace to the same temperature as that in the step c, preserving the heat for 30min, and carrying out third heating treatment;
f. c, performing third fire rolling on the plate obtained in the step e, wherein the rolling direction is the same as that in the step b, the rolling pass is 1 pass, and the rolling deformation is 17% -45%;
g. and f, finally annealing the plate obtained in the step f at 700 ℃ for 2 hours, and then discharging and air-cooling to obtain the final TC4 titanium alloy plate, wherein the thickness of the TC4 titanium alloy plate is 0.8-1.15 mm.
Further, in the method for preparing the TC4 titanium alloy sputtering target material at low cost, the steps b, d and f are rolled in a unidirectional longitudinal rolling mode, and the accumulated total deformation amount in the steps is 86% -90%.
Further, in the method for preparing the TC4 titanium alloy sputtering target material at low cost, the heating temperature and the heating time in the steps a, c and e are the same.
Further, according to the method for preparing the TC4 titanium alloy sputtering target material with low cost, in the step g, the annealing temperature is 700 ℃, and the heat preservation time is 120 min.
Further, in the method for preparing the TC4 titanium alloy sputtering target material at low cost, in the step g, the thickness of the TC4 titanium alloy thin plate is 0.8-1.15 mm.
The invention has the following advantages:
the TC4 titanium alloy adopted by the invention is prepared by an EB furnace smelting method, the purity is higher, high-low density impurities which cannot be removed by other smelting methods can be effectively removed, and meanwhile, the TC4 titanium alloy is prepared by the EB furnace smelting method, the traditional titanium alloy processing flow is obviously shortened, and the production cost is effectively reduced.
The TC4 titanium alloy is prepared by a three-fire hot rolling method, the total reduction is about 90%, the density of the interior of a rolled plate is high, no gas is mixed, and the quality of a subsequent coating film can be ensured.
The TC4 titanium alloy is prepared by a three-fire hot rolling method, the rolling temperature of each pass is the same, the first-fire reduction is larger, the second-fire reduction is gradually reduced, the microstructure of the obtained TC4 titanium alloy is uniform, and the mechanical property meets the technical requirements of national standards of titanium and titanium alloy plates.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is a metallographic structure diagram of a TC4 titanium alloy plate prepared in example 1 of the present invention.
FIG. 2 is a metallographic structure diagram of a TC4 titanium alloy plate prepared in example 2 of the present invention.
FIG. 3 is a metallographic structure diagram of a TC4 titanium alloy plate prepared in example 3 of the present invention.
FIG. 4 is a metallographic structure diagram of a TC4 titanium alloy plate prepared in comparative example 1 according to the present invention.
FIG. 5 is a metallographic structure diagram of a TC4 titanium alloy plate prepared in comparative example 2 according to the present invention.
FIG. 6 is a metallographic structure diagram of a TC4 titanium alloy plate prepared in comparative example 3 according to the present invention.
Detailed Description
In order to make the technical solution of the present invention more clearly understood by those skilled in the art, the following examples are given to illustrate the present invention specifically, and it should be noted that the following examples are only suitable for further illustration of the present invention. It will be clear that the described embodiments are only a part of the invention and should not be interpreted as limiting the scope of protection of the invention.
The EB furnace used in this example was: c-type electron beam cold bed furnace with total power of 3200KW
The first fire rolling of the invention refers to: after the first heating, the blank is immediately placed into a rolling mill for a rolling process.
The rolling pass of the invention refers to: the number of times a billet is rolled through a rolling mill, i.e. one pass is called a rolling pass.
The rolling deformation of the invention is as follows: the reduction of the height of the rolled piece after rolling is the thickness of the blank before rolling minus the thickness of the plate after rolling.
The invention relates to a unidirectional longitudinal rolling finger: in the rolling, the rolling is always performed along the length direction of the billet without changing the rolling direction.
The EB furnace of the invention is used for smelting TC4 titanium alloy ingots, and the high-temperature furnace is a common furnace for heating before rolling TC4 titanium alloy ingots.
Example 1
This embodiment 1 provides a TC4 titanium alloy sputtering target, which is prepared by the following steps:
a. heating TC4 titanium alloy cast flat ingot smelted by an EB furnace to 800 ℃, preserving heat for 30min, and carrying out first heating treatment;
b. b, performing first hot rolling on the plate obtained in the step a along the length direction of a slab ingot under a two-roller hot rolling mill, wherein the rolling pass is 1 pass, and the rolling deformation is 53.8%;
c. b, heating the plate obtained in the step b to 800 ℃ in a high-temperature furnace, preserving heat for 30min, and carrying out secondary heating treatment;
d. c, performing second fire rolling on the plate obtained in the step c, wherein the rolling direction is the same as that in the step b, the rolling pass is 1 pass, and the rolling deformation is 50.9%;
e. d, heating the plate obtained in the step d to 800 ℃ in a high-temperature furnace, preserving heat for 30min, and carrying out third heating treatment;
f. c, performing third-time hot rolling on the plate obtained in the step e, wherein the rolling direction is the same as that in the step b, the rolling pass is 1 pass, and the rolling deformation is 43.2%;
g. and f, finally annealing the plate obtained in the step f at 700 ℃ for 2 hours, and then discharging and air-cooling to obtain the final TC4 titanium alloy plate, wherein the thickness of the TC4 titanium alloy plate is 1.1 mm.
The total deformation of the TC4 titanium alloy plate prepared in example 1 is 87.1%, the metallographic structure is a uniform and fine equiaxial structure, as shown in fig. 1, the aspect ratio of α phase is 2.8, the α phase content is 60%, the β phase content is 40%, the thickness of the plate after rolling is 1.1mm, the tensile strength is 1098.3MPa at room temperature, and the elongation after fracture is 10.3%, which satisfy the technical requirements of national standard of titanium and titanium alloy plates, thereby indicating that the TC4 titanium alloy plate prepared in this example has excellent mechanical properties.
Example 2
The embodiment provides a TC4 titanium alloy sputtering target material, and the preparation method comprises the following steps
a. Heating TC4 titanium alloy cast slab ingot smelted by an EB furnace to 900 ℃, preserving heat for 30min, and carrying out first heating treatment;
b. b, performing first hot rolling on the plate obtained in the step a along the length direction of a slab ingot under a two-roller hot rolling mill, wherein the rolling pass is 1 pass, and the rolling deformation is 52.9%;
c. b, heating the plate obtained in the step b to 900 ℃ in a high-temperature furnace, preserving heat for 30min, and carrying out secondary heating treatment;
d. c, performing second fire rolling on the plate obtained in the step c, wherein the rolling direction is the same as that in the step b, the rolling pass is 1 pass, and the rolling deformation is 51%;
e. d, heating the plate obtained in the step d to 900 ℃ in a high-temperature furnace, preserving heat for 30min, and carrying out third heating treatment;
f. c, performing third-time hot rolling on the plate obtained in the step e, wherein the rolling direction is the same as that in the step b, the rolling pass is 1 pass, and the rolling deformation is 41.3%;
g. and f, finally annealing the plate obtained in the step f at 700 ℃ for 2 hours, and then discharging and air-cooling to obtain the final TC4 titanium alloy plate, wherein the thickness of the TC4 titanium alloy plate is 1.15 mm.
The total deformation of the TC4 titanium alloy plate prepared in example 2 is 86.5%, the metallographic structure is a uniform and fine equiaxial structure, as shown in fig. 2, the aspect ratio of α phase is 3, the α phase content is 65%, the β phase content is 35%, the thickness of the plate after rolling is 1.15mm, the tensile strength is 1003.8MPa at room temperature, and the elongation after fracture is 10.4%, which satisfy the technical requirements of national standard of titanium and titanium alloy plates, thereby demonstrating that the TC4 titanium alloy plate prepared in this example has excellent mechanical properties.
Example 3
This embodiment 3 provides a TC4 titanium alloy sputtering target, which is prepared by the following steps:
a. heating TC4 titanium alloy cast flat ingot smelted by an EB furnace to 1000 ℃, preserving heat for 30min, and carrying out first heating treatment;
b. b, performing first hot rolling on the plate obtained in the step a along the length direction of a slab ingot under a two-roller hot rolling mill, wherein the rolling pass is 1 pass, and the rolling deformation is 71.8%;
c. b, heating the plate obtained in the step b to 1000 ℃ in a high-temperature furnace, preserving heat for 30min, and carrying out secondary heating treatment;
d. c, performing second fire rolling on the plate obtained in the step c, wherein the rolling direction is the same as that in the step b, the rolling pass is 1 pass, and the rolling deformation is 17.7%;
e. d, heating the plate obtained in the step d to 1000 ℃ in a high-temperature furnace, preserving heat for 30min, and carrying out third heating treatment;
f. c, performing third-time rolling on the plate obtained in the step e, wherein the rolling direction is the same as that in the step b, the rolling pass is 1 pass, and the rolling deformation is 42%;
g. and f, finally annealing the plate obtained in the step f at 700 ℃ for 2 hours, and then discharging and air-cooling to obtain the final TC4 titanium alloy plate, wherein the thickness of the TC4 titanium alloy plate is 1.13 mm.
The total deformation of the TC4 titanium alloy plate prepared in example 3 was 86.5%, the metallographic structure was a sheet layer α phase, as shown in fig. 3, the aspect ratio of α phase was 4.3, the content of α phase was 61%, the content of β phase was 39%, the thickness of the plate after rolling was 1.13mm, the tensile strength was 1095.4MPa at room temperature, and the elongation after fracture was 11.7%, which satisfied the technical requirements of "national standard for titanium and titanium alloy plates", thereby demonstrating that the TC4 titanium alloy plate prepared in this example has excellent mechanical properties.
Comparative example 1
The comparative example provides a TC4 titanium alloy sputtering target, and the preparation method comprises the following steps:
a. heating TC4 titanium alloy cast flat ingot smelted by an EB furnace to 800 ℃, preserving heat for 30min, and carrying out first heating treatment;
b. b, performing first hot rolling on the plate obtained in the step a along the length direction of a slab ingot under a two-roller hot rolling mill, wherein the rolling pass is 1 pass, and the rolling deformation is 12.14%;
c. b, heating the plate obtained in the step b to 800 ℃ in a high-temperature furnace, preserving heat for 30min, and carrying out secondary heating treatment;
d. c, performing second fire rolling on the plate obtained in the step c, wherein the rolling direction is the same as that in the step b, the rolling pass is 1 pass, and the rolling deformation is 19.74%;
e. and d, finally annealing the plate obtained in the step d at the annealing temperature of 700 ℃ for 2 hours, and then discharging and air-cooling to obtain the final TC4 titanium alloy plate, wherein the thickness of the TC4 titanium alloy plate is 6.10 mm.
Comparative example 1 a method for preparing a TC4 titanium alloy sputtering target, which is different from example 1 in that the total rolling deformation of example 1 is 87.1%, the rolling passes are three times, and the rolling deformation of each pass is gradually reduced, while the total rolling deformation of comparative example 1 is 29.5%, the rolling passes are two times, and the reduction of each pass is uniform, results show that example 1 is rolled under multiple passes with large deformation, so that the target has high compactness, uniform microstructure, small α phase size, α phase aspect ratio of 2.8, good room temperature mechanical property, tensile strength of 1098.3MPa, and elongation after breakage is 10.3%, which meet the performance requirements of the sputtering target, while comparative example 1 is rolled under small deformation, so that the original structure is not completely broken, the compactness is low, the microstructure is not uniform, the metallographic structure is α phase, as shown in fig. 4, α phase size, coarse α phase aspect ratio of 8.2, room temperature tensile property of 769.31MPa, poor tensile strength of 769.31, and elongation after breakage is lower than that of the microstructure of comparative example 1, and the comparative example 1 is processed under 800 ℃.
Comparative example 2
The comparative example provides a TC4 titanium alloy sputtering target, and the preparation method comprises the following steps:
a. heating TC4 titanium alloy cast slab ingot smelted by an EB furnace to 900 ℃, preserving heat for 30min, and carrying out first heating treatment;
b. b, performing first hot rolling on the plate obtained in the step a along the length direction of a slab ingot under a two-roller hot rolling mill, wherein the rolling pass is 1 pass, and the rolling deformation is 28.56%;
c. b, heating the plate obtained in the step b to 900 ℃ in a high-temperature furnace, preserving heat for 30min, and carrying out secondary heating treatment;
d. c, performing second fire rolling on the plate obtained in the step c, wherein the rolling direction is the same as that in the step b, the rolling pass is 1 pass, and the rolling deformation is 5.30%;
e. and d, finally annealing the plate obtained in the step d at the annealing temperature of 700 ℃ for 2 hours, and then discharging and air-cooling to obtain the final TC4 titanium alloy plate, wherein the thickness of the TC4 titanium alloy plate is 5.9 mm.
The method for preparing the TC4 titanium alloy plate in the comparative example 2 is different from the method for preparing the TC4 titanium alloy plate in the example 2, in that the total rolling deformation of the example 2 is 86.5 percent, the rolling passes are three times, the rolling deformation of each pass is nearly more than 40 percent, the total rolling deformation of the comparative example 2 is 32.3 percent, the rolling passes are two times, the reduction of the first pass is more than 20 percent, and the reduction of the second pass is less than 10 percent, so that the target prepared in the example 2 is good in compactness, uniform in microstructure, small in α phase size, good in α phase aspect ratio, good in room-temperature mechanical property, 1003.8MPa in tensile strength and 10.4 percent of elongation after breakage, the target prepared in the comparative example 2 is poor in compactness and non-uniform in microstructure, a metallographic structure is composed of a thin piece layer α phase and a small amount of β phase, as shown in a graph 5, a α phase size is large, a α phase aspect ratio is 6.8, poor in room-temperature mechanical property, the strength is 836.827MPa, the elongation after breakage is 7.073 percent, and the mechanical property of the rolling process is lower than that of the comparative example 2 and the mechanical property is processed under the 900 ℃.
Comparative example 3
The comparative example provides a TC4 titanium alloy sputtering target, which is prepared by the steps of:
a. heating TC4 titanium alloy cast flat ingot smelted by an EB furnace to 1000 ℃, preserving heat for 30min, and carrying out first heating treatment;
b. b, performing first hot rolling on the plate obtained in the step a along the length direction of a slab ingot under a two-roller hot rolling mill, wherein the rolling pass is 1 pass, and the rolling deformation is 30.39%;
c. b, heating the plate obtained in the step b to 1000 ℃ in a high-temperature furnace, preserving heat for 30min, and carrying out secondary heating treatment;
d. c, performing second fire rolling on the plate obtained in the step c, wherein the rolling direction is the same as that in the step b, the rolling pass is 1 pass, and the rolling deformation is 5.26%;
e. and d, finally annealing the plate obtained in the step d at the annealing temperature of 700 ℃ for 2 hours, and then discharging and air-cooling to obtain the final TC4 titanium alloy plate, wherein the thickness of the TC4 titanium alloy plate is 5.60 mm.
Comparative example 3 a method for manufacturing a TC4 titanium alloy plate, except that the total rolling deformation of example 3 was 86.5% at 1000 ℃, the rolling passes were three times, and the difference between the rolling deformation of the first pass was large, while the total rolling deformation of comparative example 3 was 34%, the rolling passes were two times, and the reduction of the first pass was large and the reduction of the second pass was small, resulting in that the original structure of example 3 was completely crushed, the compactness was good, the microstructure was uniform, the metallographic structure consisted of lamellar secondary α phase, the mechanical properties at room temperature were good, the tensile strength was 1095.4MPa, and the elongation after fracture was 11.7%, and the mechanical properties met the national standards, whereas the microstructure of comparative example 3 was non-uniform, the metallographic structure consisted of fine acicular α phase and coarse β phase, as shown in fig. 6, and the mechanical properties at room temperature was poor, the tensile strength was 976.065MPa, and the elongation after fracture was 7.353%, to summarize the rolling properties at 1000 ℃ and the uniformity of the grain boundary mechanical properties of comparative example 3 and the microstructure processing method were lower than the present processing method.
Claims (6)
1. A method for preparing TC4 titanium alloy sputtering target material with low cost is characterized by comprising the following steps:
a. smelting a TC4 titanium alloy ingot by using an EB furnace, heating, preserving heat, and carrying out primary heating treatment;
b. b, performing first fire rolling on the plate obtained in the step a along the length direction of the plate, wherein the rolling pass is 1 pass, and the rolling deformation is 50-75%;
c. b, heating the plate obtained in the step b to the same temperature as that in the step a, preserving heat, and carrying out secondary heating treatment;
d. c, performing second fire rolling on the plate obtained in the step c, wherein the rolling direction is the same as that in the step b, the rolling pass is 1 pass, and the rolling deformation is 17% -55%;
e. heating the plate obtained in the step d to the same temperature as that in the step c, preserving heat, and carrying out third heating treatment;
f. c, performing third fire rolling on the plate obtained in the step e, wherein the rolling direction is the same as that in the step b, the rolling pass is 1 pass, and the rolling deformation is 17% -45%;
g. and f, annealing the plate obtained in the step f, and air-cooling to obtain the TC4 titanium alloy sputtering target.
2. The method for preparing the alloy steel according to claim 1, wherein the steps b, d and f are rolled in a unidirectional longitudinal rolling mode, and the cumulative total deformation of the steps b, d and f is 86-90%.
3. The method according to claim 1, wherein the holding time of steps a, c and e is the same, and the TC4 titanium alloy ingot in step a is heated to 800-1000 ℃ after being smelted by using an EB furnace.
4. The method according to claim 1, wherein the annealing temperature in step g is 700 ℃ and the annealing time is 120 min.
5. The method according to claim 1, wherein the thickness of the TC4 titanium alloy sputtering target in the step g is 0.8-1.15 mm.
6. The TC4 titanium alloy sputtering target material prepared by the preparation method of any one of the preceding claims, which has a thickness of 0.8-1.15 mm.
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| CN113231465A (en) * | 2021-05-13 | 2021-08-10 | 太原理工大学 | Large-size Ni-Ni3Preparation method of Al-NiAl laminated structure composite board |
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