CN115029668A - Method for preparing high-performance tantalum sputtering target material through pack rolling - Google Patents
Method for preparing high-performance tantalum sputtering target material through pack rolling Download PDFInfo
- Publication number
- CN115029668A CN115029668A CN202210621833.4A CN202210621833A CN115029668A CN 115029668 A CN115029668 A CN 115029668A CN 202210621833 A CN202210621833 A CN 202210621833A CN 115029668 A CN115029668 A CN 115029668A
- Authority
- CN
- China
- Prior art keywords
- rolling
- sputtering target
- target material
- target
- tantalum sputtering
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000005096 rolling process Methods 0.000 title claims abstract description 92
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 47
- 238000005477 sputtering target Methods 0.000 title claims abstract description 36
- 239000013077 target material Substances 0.000 title claims abstract description 33
- 238000003466 welding Methods 0.000 claims abstract description 30
- 238000004544 sputter deposition Methods 0.000 claims abstract description 22
- 238000010274 multidirectional forging Methods 0.000 claims abstract description 16
- 238000000137 annealing Methods 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000005242 forging Methods 0.000 claims description 11
- 239000013078 crystal Substances 0.000 claims description 9
- 238000003754 machining Methods 0.000 claims description 9
- 238000007789 sealing Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 4
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 238000009826 distribution Methods 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 12
- 238000001953 recrystallisation Methods 0.000 description 9
- 238000010894 electron beam technology Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
Images
Classifications
-
- 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
- B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
- B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
- B21J5/002—Hybrid process, e.g. forging following casting
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a method for preparing a high-performance tantalum sputtering target by pack rolling, belonging to the technical field of sputtering target preparation. The method comprises the following steps: carrying out multidirectional cross rolling on the high-purity tantalum cast ingot subjected to multidirectional forging to obtain an intermediate target blank, then stacking and fixing the two intermediate target blanks, carrying out accumulative cross stack rolling, and welding the target blank and a back plate to obtain a tantalum sputtering target material; the microstructure of the high-purity tantalum sputtering target obtained by the method is fine and uniform, the content of (111) on the sputtering surface is uniformly distributed, the content of (111) in the whole thickness direction is less than or equal to 50%, the microstructure of the prepared high-purity tantalum target is high in uniformity, and the requirement of large-size wafer semiconductor sputtering coating can be met.
Description
Technical Field
The invention belongs to the technical field of sputtering target preparation, and particularly relates to a method for preparing a high-performance tantalum sputtering target by pack rolling.
Background
The high-purity Ta sputtering target is widely applied to the integrated circuit Cu interconnection line manufacturing process and is used as a barrier layer to prevent Cu from diffusing to Si. The Ta target microstructure, and in particular the grain orientation, affects the thickness uniformity and electrical property uniformity of the sputtered film. Research shows that Ta crystal grains (110) are sputtered the fastest and (111) are the slowest. Therefore, the grain orientation distribution is a key influence factor for preparing the high-performance Ta target, and the structural uniformity of the large-size Ta target has a remarkable influence on the performance of a sputtering film. Because Ta belongs to high-layer fault energy metal, the most easily started sliding system is {110} <111> in the conventional cold plastic deformation process, and therefore (111) texture is easily formed. The conventional forging-rolling-heat treatment process is easy to cause the structure of the surface layer and the core of the tantalum ingot to have obvious difference, and the grain orientation gradient is generated. The longitudinal center of the Ta target is subjected to plane strain in the rolling process, so that a strong (111) texture can be formed. As shown in fig. 2, when the Ta target is excessively (111) generated toward the center, the target may suffer from non-uniformity of the sputtered film when sputtered to an intermediate position of the thickness, resulting in insufficient target life. In order to improve the uniformity of the grain orientation distribution in the tantalum target, in patent US8250895B2, the target blank rolling adopts an inclined rolling method, so as to control the strain state of the target blank, reduce the content of the core part (111), and reduce the grain orientation gradient in the thickness direction. In patent US2014/0242401a1, tantalum ingots are forged and heat-treated a plurality of times, then cold-rolled by a large-diameter rolling mill, and the content of (100) and (111) in the sputtering surface direction is controlled by vacuum annealing, so that the orientation distribution is uniform. Both of these methods require special equipment to implement. The patent US20030089429 adopts a powder metallurgy method, high-purity tantalum powder is formed in a hot pressing mode, and the orientation of the tantalum target prepared by the method is randomly distributed and uniformly distributed. However, this method may have problems that the target material cannot be completely densified and the oxygen content is high. In order to improve the uniformity of the structure in the Ta target, a method capable of effectively controlling the grain size and the orientation uniformity of the large-size high-purity tantalum target material is needed to be provided.
Disclosure of Invention
In order to solve the problems, the invention provides a method for preparing a high-performance tantalum sputtering target material by pack rolling, which comprises the following steps: carrying out multidirectional cross rolling on the high-purity tantalum cast ingot subjected to multidirectional forging to obtain an intermediate target blank, then stacking and fixing the two intermediate target blanks, carrying out accumulative cross stack rolling, and welding the target blank and a back plate to obtain a tantalum sputtering target material;
the method comprises the following specific steps:
1) carrying out multidirectional forging on the high-purity tantalum cast ingot, and refining the structure by matching intermediate annealing in the forging process;
2) performing multidirectional cross rolling and vacuum heat treatment on the forged cast ingot to prepare an intermediate target blank; the diameter phi of the intermediate target blank is 200-350mm, and the thickness is 20-30 mm;
3) stacking and fixing the two intermediate target blanks, and performing accumulated rolling to obtain a rolled target blank with the diameter of more than or equal to phi 450mm and the thickness of 6-9mm of a single target blank;
the rolling direction is multidirectional cross rolling, the total rolling deformation is 60-80%, and the pass deformation is 10-20%;
4) separating the target blank by machining, carrying out vacuum heat treatment, and controlling the grain size and orientation;
5) welding the target blank and the back plate to obtain a tantalum sputtering target material; the crystal grain orientation of the tantalum sputtering target material is uniformly distributed, the (111) of a sputtering surface is less than 50%, and the size of the crystal grain is less than or equal to 100 mu m.
Preferably, the total rolling deformation of the step 3) is 60%, and the pass deformation is 20%;
the deformation is 70%, and the pass deformation is 15%;
the deformation is 80%, and the pass deformation is 10%.
The step 1) of multidirectional forging comprises axial and radial die forging, wherein radial drawing is firstly carried out, and then axial upsetting and reciprocating deformation are carried out.
The rolling direction is turned to 90 degrees for each pass for 1 to 4 times and is turned to 90 degrees for each pass for 5 to 8 times,
the step 3) is to stack the two target blanks, the edges are fixed together, the fixing method adopts a welding or riveting mode,
further, the fixing method in the step 3) comprises a sheath sealing and welding mode.
And 5) taking the surface contacted with the target blank during stacking as a welding surface, and welding the target blank with the back plate to obtain a finished product.
The purity of the high-purity tantalum cast ingot in the step 1) is more than or equal to 99.995%.
The intermediate annealing temperature in the step 1) is 1100 ℃.
The temperature of the vacuum heat treatment in the step 2) is 1100 ℃.
The invention has the beneficial effects that:
1. the high-purity tantalum target material prepared by the method has high microstructure uniformity, and can meet the requirement of large-size wafer semiconductor sputtering coating.
2. The invention adopts the method of accumulating two target blanks and reducing the occurrence of grain orientation through multi-directional cross rolling, so that the grain orientation distribution of the target material film is more uniform, the (111) of the sputtering surface is less than 50 percent, and the grain size is less than or equal to 100 mu m.
Drawings
FIG. 1 is a flow chart of a process for preparing a high-purity tantalum target material according to the present invention;
FIG. 2 is a longitudinal sectional orientation distribution diagram of a tantalum sputtering target in comparative example 1 of the present invention;
FIG. 3 is a longitudinal section orientation distribution diagram of a tantalum sputtering target in example 1 of the present invention;
FIG. 4 shows the distribution of the orientation of tantalum sputtering targets in example 1 and comparative example 1;
FIG. 5 is a schematic view showing the rolling direction of the target in the examples and comparative examples of the present invention.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific examples:
a method for preparing a high-performance tantalum sputtering target material by stack rolling is disclosed, and the flow of the method is shown in figure 1: carrying out multidirectional cross rolling on the high-purity tantalum cast ingot subjected to multidirectional forging to obtain an intermediate target blank, then stacking and fixing the two intermediate target blanks, carrying out accumulative cross stack rolling, and welding the target blanks and a back plate to obtain a tantalum sputtering target material;
the method comprises the following specific steps:
1) carrying out multidirectional forging on a high-purity tantalum ingot with the purity of more than or equal to 99.995%, carrying out intermediate annealing at 1100 ℃ in the forging process, and refining the structure through multidirectional forging and vacuum heat treatment; the multidirectional forging comprises axial and radial die forging, wherein radial drawing is firstly carried out, and then axial upsetting and reciprocating deformation are carried out;
2) performing multidirectional cross rolling on the forged cast ingot, wherein the rolling direction is in a double-cross mode, namely, the cast ingot turns 90 degrees every time in 1-4 passes; after the first four times of rolling is finished, turning to 45 degrees, carrying out 5 th-8 th rolling, turning to 90 degrees each time, wherein the rolling directions of 1-4 times and the rolling directions of 5 th-8 times are respectively crossed by 45 degrees. Carrying out vacuum heat treatment to prepare an intermediate target blank; the diameter phi of the intermediate target blank is 200-350mm, and the thickness is 20-30 mm;
3) stacking the two intermediate target blanks, fixing the edges together, and performing accumulated stack rolling to obtain a stack-rolled target blank with the diameter of more than or equal to phi 450mm and the thickness of 6-9mm of a single target blank; the fixing method adopts a welding or riveting mode, and specifically comprises a sheathing seal welding mode.
As shown in fig. 5, the rolling direction is multidirectional cross rolling, and the rolling direction is in a double cross manner, i.e. the rolling direction is turned to 90 degrees every time in 1-4 passes; after the first four times of rolling is finished, turning to 45 degrees, carrying out 5 th-8 th rolling, turning to 90 degrees each time, wherein the rolling directions of 1-4 times and the rolling directions of 5 th-8 times are respectively crossed by 45 degrees. The total rolling deformation is 60-80%, and the pass deformation is 10-20%;
4) separating the target blank by machining, carrying out vacuum heat treatment, and controlling the grain size and orientation;
5) taking the surface contacted with the target blank during stacking as a welding surface, and welding the welding surface with a back plate to obtain a tantalum sputtering target material; the crystal grain orientation of the tantalum sputtering target material is uniformly distributed, the (111) of a sputtering surface is less than 50%, and the size of the crystal grain is less than or equal to 100 mu m.
In order to verify the effectiveness of the method, the electron beam melting is selected to obtain the high-purity tantalum metal ingot, the preparation method is carried out, the purity is more than or equal to 99.995%, and the size of the high-purity tantalum metal ingot is phi 150 x 100 mm.
Example 1
1) And carrying out axial and radial die forging on the high-purity tantalum metal cast ingot to finish multidirectional forging. The intermediate annealing temperature of the ingot is 1100 ℃.
2) And performing multi-directional cross rolling to obtain an intermediate target blank with the diameter of phi 335mm and the thickness of 20 mm. And (3) carrying out recrystallization heat treatment on the intermediate target blank, wherein the heat treatment temperature is 1100 ℃.
3) Stacking the two target blanks processed in the step 2), fixing the two target blanks by adopting an electron beam welding mode at the edge, and performing accumulative rolling, wherein the rolling direction is multidirectional cross rolling, and the rolling direction is a multidirectional cross rolling mode, namely the rolling direction is in a double cross mode, namely the rolling direction is turned by 90 degrees every time in 1-4 times, as shown in figure 5; after the first four times of rolling is finished, turning to 45 degrees, carrying out 5 th-8 th pass rolling, turning to 90 degrees each time, and enabling the rolling directions of the 1 st-4 passes and the rolling directions of the 5 th-8 passes to be crossed at 45 degrees respectively. The deformation is 60%, and the pass deformation is 20%. The size diameter of the laminated rolling target blank is more than or equal to phi 450mm, and the thickness of a single target blank is 8 mm.
4) Separating the target blank by machining, wherein the machining diameter is phi 450mm, and the thickness is kept unchanged; leveling the separated target blank, and carrying out vacuum recrystallization annealing at the annealing temperature of 1100 ℃ for 2h to obtain a uniform and refined recrystallized microstructure.
5) And (3) taking the surface contacted with the target blank when the target blank is stacked as a welding surface, and welding the welding surface with a back plate to obtain the finished tantalum sputtering target material.
The results obtained are shown in Table 1 and it is seen that a significant refinement in grain size is obtained, the average grain size is 68.3 μm and the size distribution is uniform. The content of the sputtering surface (111) was projected from the longitudinal section, and the maximum content was 38.15%.
Example 2
1) And carrying out axial and radial die forging on the high-purity tantalum metal cast ingot to finish multidirectional forging. The intermediate annealing temperature of the ingot is 1100 ℃.
2) And (3) performing multidirectional cross rolling to obtain an intermediate target blank with the diameter of 300mm and the thickness of 25 mm. And (3) carrying out recrystallization heat treatment on the intermediate target blank, wherein the heat treatment temperature is 1100 ℃.
3) And (3) stacking the two target blanks processed in the step 2), fixing the two target blanks at the edges by adopting an electron beam welding mode for accumulative stack rolling, wherein the rolling direction is multidirectional cross rolling, the deformation is 70%, and the pass deformation is 15%. The size diameter of the laminated rolling target blank is more than or equal to phi 450mm, and the thickness of a single target blank is 7.5 mm.
4) Separating the target blank by machining, wherein the machining diameter is phi 450mm, and the thickness is kept unchanged; leveling the separated target blank, and carrying out vacuum recrystallization annealing at the annealing temperature of 1100 ℃ for 2h to obtain a uniform and refined recrystallized microstructure.
5) And (3) taking the surface contacted with the target blank during stacking as a welding surface, and welding the welding surface with a back plate to obtain the finished product of the tantalum sputtering target material.
The results obtained are shown in Table 1, and it can be seen that a significant refinement in grain size is obtained, the average grain size is 72.6 μm, and the size distribution is uniform. The content of the sputtering surface (111) projected from the longitudinal section was 37.21% at the maximum.
Example 3
1) And carrying out axial and radial die forging on the high-purity tantalum metal cast ingot to finish multidirectional forging. The intermediate annealing temperature of the ingot is 1100 ℃.
2) And performing multi-directional cross rolling to obtain an intermediate target blank with the diameter of phi 273.8mm and the thickness of 30 mm. And (3) carrying out recrystallization heat treatment on the intermediate target blank, wherein the heat treatment temperature is 1100 ℃.
3) And (3) stacking the two target blanks after the treatment in the step (2), fixing the two target blanks by adopting an electron beam welding mode at the edge, and performing accumulative rolling, wherein the rolling direction is multidirectional cross rolling, the deformation is 80%, and the pass deformation is 10%. The size diameter of the laminated rolling target blank is more than or equal to phi 450mm, and the thickness of a single target blank is 6 mm.
4) Separating the target blank by machining, wherein the machining diameter is phi 450mm, and the thickness is kept unchanged; leveling the separated target blank, and carrying out vacuum recrystallization annealing at the annealing temperature of 1100 ℃ for 2h to obtain a uniform and refined recrystallized microstructure.
5) And (3) taking the surface contacted with the target blank during stacking as a welding surface, and welding the welding surface with a back plate to obtain the finished product of the tantalum sputtering target material.
The results obtained are shown in Table 1 and it can be seen that a significant refinement in grain size is obtained, the average grain size is 75.8 μm and the size distribution is uniform. The content of the sputtering surface (111) projected from the longitudinal section was 40.53% at the maximum.
In order to verify the effectiveness of the method of the invention, a conventional thermomechanical processing process was used to prepare a tantalum target, which was compared to the target of the invention. The material is still selected to be electron beam smelted into high-purity tantalum metal ingot with the purity more than or equal to 99.995 percent and the ingot size phi of 150 multiplied by 100 mm. The method comprises the following specific steps:
comparative example 1
1. And carrying out axial and radial die forging on the cast ingot to finish multidirectional forging. The intermediate annealing temperature of the ingot is 1100 ℃, and the annealing time is 2 h. The diameter of the target blank is 223mm, and the thickness is 45 mm.
2. And (3) performing multidirectional cross rolling, wherein the deformation is 80%, the pass deformation is 15%, and the purpose is to further refine grains by using the deformation process. The size diameter of the target blank is more than or equal to phi 450mm, and the thickness of the target blank is 9 mm.
3. Vacuum recrystallization annealing is carried out, the annealing temperature is 1100 ℃, and the annealing time is 2 hours.
4. And processing the prepared plate blank into a target finished product.
The results obtained are shown in Table 1, and it can be seen that the average grain size is 85.5 μm and the core grain size is large. The content of the sputtering surface (111) projected from the longitudinal section was 83.54%.
Comparative example 2
1. And carrying out axial and radial die forging on the cast ingot to finish multidirectional forging. The intermediate annealing temperature of the ingot is 1100 ℃, and the annealing time is 2 h.
2. And (4) performing multidirectional cross rolling to obtain a target blank with the diameter phi of 300mm and the thickness of 25 mm. And (4) carrying out recrystallization heat treatment on the target blank. The heat treatment temperature is 1100 ℃.
3. And (3) performing multidirectional cross rolling, wherein the deformation is 70%, the pass deformation is 20%, and the purpose is to further refine grains by using the deformation process. The size diameter of the target blank is more than or equal to phi 450mm, and the thickness of the target blank is 7.5 mm.
4. Vacuum recrystallization annealing is carried out, the annealing temperature is 1100 ℃, and the annealing time is 2 hours.
5. And processing the prepared plate blank into a target finished product.
The results obtained are shown in Table 1, and it can be seen that the average grain size is 82.3. mu.m. The content of the sputtering surface (111) projected from the longitudinal section was 85.32% at the maximum.
Comparing the results of the examples with those of the comparative examples, it is seen that the crystal grain sizes in the examples are finer and the average crystal grain size is not more than 100 μm. The (111) content of the sputtering surface was less than 50% as a whole. FIG. 2 is a microstructure of a longitudinal section of example 1, from which it is apparent that the grain size distribution is uniform and the content distribution of the sputtering surface at the central portion (111) is uniform. FIG. 3 is a microstructure of a longitudinal section of comparative example 1, from which it can be seen that the grain size is excessively large in the center and the content of the sputtering surface is remarkably increased at the center position (111). FIG. 4 is a graph showing the content distribution of the sputtering surface of the target in example 1 and comparative example 1 over the entire longitudinal section (111), and shows that the content of the sputtering surface of the target in the comparative example rapidly increases at the center position (111), the orientation gradient is large over the thickness direction, and the uniformity of the film is deteriorated when the sputtering surface is sputtered to the thickness center. The target prepared by the method of the invention has more uniform orientation distribution and better sputtering stability of the high-purity tantalum target, and can meet the use requirement of high-end semiconductor integrated circuits.
Table 1 comparison table of target material preparation results of inventive example and comparative example
| Grain size | Maximum value of sputtering surface (111) | |
| Example 1 | 75.8μm | 38.15％ |
| Example 2 | 72.6μm | 37.21％ |
| Example 3 | 68.3μm | 40.53％ |
| Comparative example 1 | 85.5μm | 83.54％ |
| Comparative example 2 | 82.3μm | 85.32％ |
Claims (10)
1. A method for preparing a high-performance tantalum sputtering target material by pack rolling is characterized by comprising the following steps: carrying out multidirectional cross rolling on the high-purity tantalum cast ingot subjected to multidirectional forging to obtain an intermediate target blank, then stacking and fixing the two intermediate target blanks, carrying out accumulative cross stack rolling, and welding the target blank and a back plate to obtain a tantalum sputtering target material;
the method comprises the following specific steps:
1) carrying out multidirectional forging on the high-purity tantalum ingot, wherein the forging process is matched with intermediate annealing operation;
2) performing multidirectional cross rolling and vacuum heat treatment on the forged cast ingot to prepare an intermediate target blank; the diameter phi of the intermediate target blank is 200-350mm, and the thickness is 20-30 mm;
3) stacking and fixing the two intermediate target blanks, and performing accumulated rolling to obtain a rolled target blank with the diameter of more than or equal to phi 450mm and the thickness of 6-9mm of a single target blank;
the rolling direction is multidirectional cross rolling, the total rolling deformation is 60-80%, and the pass deformation is 10-20%;
4) separating the target blank by machining, carrying out vacuum heat treatment, and controlling the size and orientation of grains;
5) welding the target blank and the back plate to obtain a tantalum sputtering target material; the crystal grain orientation of the tantalum sputtering target material is uniformly distributed, the (111) of a sputtering surface is less than 50%, and the size of the crystal grain is less than or equal to 100 mu m.
2. The method for preparing the high-performance tantalum sputtering target material through pack rolling according to claim 1, wherein the total rolling deformation in the step 3) is 60%, and the pass deformation is 20%.
3. The method for preparing the high-performance tantalum sputtering target material through pack rolling according to claim 1, wherein the deformation in the step 3) is 70%, and the pass deformation is 15%.
4. The method for preparing the high-performance tantalum sputtering target material through pack rolling according to claim 1, wherein the deformation in the step 3) is 80%, and the pass deformation is 10%.
5. The method for preparing the high-performance tantalum sputtering target material through pack rolling according to claim 1, wherein the step 1) of multidirectional forging comprises axial and radial die forging.
6. The method for preparing the high-performance tantalum sputtering target material through pack rolling according to claim 1, wherein the multi-direction cross rolling is performed, and the rolling direction is in a double cross manner, namely the rolling direction is turned to 90 degrees every time in 1-4 passes; after the first four times of rolling is finished, turning to 45 degrees, carrying out 5 th-8 th pass rolling, turning to 90 degrees each time, and enabling the rolling directions of the 1 st-4 passes and the rolling directions of the 5 th-8 passes to be crossed at 45 degrees respectively.
7. The method for preparing the high-performance tantalum sputtering target material through pack rolling according to claim 1, wherein in the step 3), two target blanks are stacked and fixed together at the edges, and the fixing method adopts a welding or riveting mode; further, the fixing method comprises a sheathing sealing and welding mode.
8. The method for preparing the high-performance tantalum sputtering target material through pack rolling according to claim 1, wherein the surface of the target blank in the step 5) is used as a welding surface when being stacked, and is welded with a back plate to form a finished product.
9. The method for preparing the high-performance tantalum sputtering target material through pack rolling according to claim 1, wherein the purity of the high-purity tantalum ingot in the step 1) is more than or equal to 99.995%.
10. The method for preparing the high-performance tantalum sputtering target material through pack rolling according to claim 1, wherein the annealing temperature in the step 1) is 1100 ℃, and the vacuum heat treatment temperature in the step 2) is 1100 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210621833.4A CN115029668B (en) | 2022-06-02 | 2022-06-02 | Method for preparing high-performance tantalum sputtering target material by means of pad rolling |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210621833.4A CN115029668B (en) | 2022-06-02 | 2022-06-02 | Method for preparing high-performance tantalum sputtering target material by means of pad rolling |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115029668A true CN115029668A (en) | 2022-09-09 |
| CN115029668B CN115029668B (en) | 2024-05-17 |
Family
ID=83122643
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210621833.4A Active CN115029668B (en) | 2022-06-02 | 2022-06-02 | Method for preparing high-performance tantalum sputtering target material by means of pad rolling |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115029668B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1659305A (en) * | 2002-09-20 | 2005-08-24 | 株式会社日矿材料 | Tantalum sputtering target and method for preparation thereof |
| CN105525263A (en) * | 2015-12-23 | 2016-04-27 | 有研亿金新材料有限公司 | Preparation method for high-performance tantalum sputtering target |
| CN106399954A (en) * | 2016-08-30 | 2017-02-15 | 有研亿金新材料有限公司 | Processing method of long-service-life copper manganese alloy target material |
-
2022
- 2022-06-02 CN CN202210621833.4A patent/CN115029668B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1659305A (en) * | 2002-09-20 | 2005-08-24 | 株式会社日矿材料 | Tantalum sputtering target and method for preparation thereof |
| CN105525263A (en) * | 2015-12-23 | 2016-04-27 | 有研亿金新材料有限公司 | Preparation method for high-performance tantalum sputtering target |
| CN106399954A (en) * | 2016-08-30 | 2017-02-15 | 有研亿金新材料有限公司 | Processing method of long-service-life copper manganese alloy target material |
Non-Patent Citations (1)
| Title |
|---|
| 潘文高等: "钽材轧制和再结晶织构演变研究进展", 材料导报, vol. 30, no. 11, pages 150 - 156 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115029668B (en) | 2024-05-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US6193821B1 (en) | Fine grain tantalum sputtering target and fabrication process | |
| JP5578496B2 (en) | Tantalum sputtering target | |
| JP4976013B2 (en) | Copper sputtering target and method of forming copper sputtering target | |
| JP4974362B2 (en) | Ta sputtering target and manufacturing method thereof | |
| JP2004526863A (en) | Refractory metal plate having uniform texture and method for producing the plate | |
| CN103827348B (en) | Tantalum sputtering target and manufacture method thereof | |
| JP2002518593A (en) | Metal product having fine and uniform structure and texture and method for manufacturing the same | |
| TWI623638B (en) | Sputtering target and manufacturing method thereof | |
| JP2004513228A (en) | Physical vapor deposition target and method for producing metal material | |
| US9890452B2 (en) | Tantalum sputtering target, method for manufacturing same, and barrier film for semiconductor wiring formed by using target | |
| CN104419901B (en) | A kind of manufacture method of tantalum target | |
| CN113046705B (en) | Copper target material and preparation method and application thereof | |
| CN105431565B (en) | Tantalum spattering target and its manufacturing method | |
| JP5325096B2 (en) | Copper target | |
| CN104755651B (en) | Tantalum sputtering target and method for producing same | |
| KR102365363B1 (en) | Titanium target for sputtering, manufacturing method thereof, and manufacturing method of titanium-containing thin film | |
| CN112410699B (en) | Method for optimizing grain size and uniformity of tantalum plate | |
| US20190055629A1 (en) | Method of making a tantalum sputtering target with increased deposition rate | |
| CN115029668B (en) | Method for preparing high-performance tantalum sputtering target material by means of pad rolling | |
| CN113718110B (en) | Preparation method of high-quality niobium plate adopting accumulated energy to control plate structure | |
| CN111155060A (en) | Method for manufacturing cobalt target blank | |
| CN114000073A (en) | Process method for improving internal structure of high-purity nickel target material | |
| CN113617840A (en) | Preparation method of multi-metal multilayer gradient composite material | |
| CN115044876A (en) | Preparation method of small-size high-performance tantalum target blank | |
| CN115948718A (en) | High-purity magnesium sputtering target material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |