CN112251692A - High-purity tantalum plate and heat treatment method thereof - Google Patents
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Abstract
The invention discloses a high-purity tantalum plate and a heat treatment method thereof, relating to the technical field of heat treatment, wherein the average grain size is less than 30 mu m, the standard deviation of the average grain size is less than 3 mu m, and the method comprises the following steps: placing the high-purity tantalum plate subjected to plastic deformation in a heat treatment furnace, heating to 500-700 ℃, and carrying out constant-temperature heat treatment for 80-120 min; reducing or increasing the heat treatment temperature by 100-200 ℃, and continuously carrying out constant-temperature heat treatment on the high-purity tantalum plate for 70-100 min; raising the heat treatment temperature to 1030-1130 ℃, and continuing to perform constant-temperature heat treatment on the high-purity tantalum plate for 60-90 min; and opening the furnace door and cooling to room temperature when the high-purity tantalum plate is cooled to 90-150 ℃. The method has the beneficial effects that by carrying out multi-stage annealing treatment on the high-purity tantalum plate, the tantalum crystal grains can be refined and the uniformity of the tantalum crystal grains can be improved on the premise of not increasing the deformation degree of the tantalum plate, and the method has the advantages of simplicity in operation, low cost, easiness in implementation and the like.
Description
Technical Field
The invention relates to the technical field of heat treatment, in particular to a high-purity tantalum plate and a heat treatment method thereof.
Background
The tantalum has the advantages of high melting point, good conductivity, high thermal stability, stable chemical property, good room temperature toughness and the like, and is widely applied to the fields of electronics, electrics, energy chemical industry, aerospace and the like. In recent years, tantalum and tantalum-based films become key materials for preparing diffusion barrier layers between copper wires and silicon substrates in integrated circuits, copper can be prevented from diffusing into the silicon substrates to form copper-silicon alloys, and therefore the service life of equipment is greatly prolonged. Magnetron sputtering is a main method for preparing tantalum films, and a tantalum target material for sputtering is a key consumable material in the process. Therefore, the preparation of the tantalum target with excellent performance is crucial to the manufacture of modern integrated circuits.
The performance of tantalum targets (lifetime, deposition rate, film formation uniformity, etc.) depends on chemical purity, grain size, grain orientation, and grain uniformity. Research shows that the deposition of impurity particles can short circuit the film; as the grain size increases, the target surface erosion rate decreases, so the film deposition rate decreases; as the uniformity of the grains decreases, the uniformity of the thickness of the deposited film decreases; the increased orientation ratios of the (100) crystal plane and the (111) crystal plane on the sputtering plane are beneficial to improving the film deposition rate and the film uniformity. Therefore, high purity tantalum targets with fine (typically below 100 μm) and uniform grains generally have excellent properties.
The common method for preparing the high-purity tantalum target material comprises the steps of firstly preparing a high-purity tantalum ingot by adopting electron beam melting, and then carrying out plastic processing such as forging, rolling and the like and heat treatment on the high-purity tantalum ingot to fully crush and homogenize coarse grains in the as-cast tantalum ingot. The grain size of the high-purity tantalum ingot reaches the centimeter level, and large plastic deformation is usually needed for grain refinement. However, tantalum has a large cold deformation resistance and a high work hardening rate, and cracks are easily generated when large plastic deformation occurs; and the high-temperature oxidation resistance of the tantalum is poor, so the temperature deformation and thermal deformation process is complex and the cost is high. The average grain size of the high-purity tantalum for the target is generally 35-150 mu m at present, and the difficulty in further refining grains is high. Meanwhile, the deformation uniformity of the tantalum cast ingot is poor, a band-shaped structure is easy to generate, and the target material structure is subjected to grain layering, so that fine and uniform grains are difficult to form after deformation. At present, no mature preparation technology can solve the problems.
Disclosure of Invention
The invention aims to solve at least one of the technical problems in the prior art, and provides a high-purity tantalum plate and a heat treatment method thereof, which can refine tantalum crystal grains and improve the uniformity of the tantalum crystal grains on the premise of not increasing the deformation degree of the tantalum plate, have the advantages of simple operation, low cost, easy realization and the like, and are suitable for popularization.
The technical solution of the invention is as follows:
a high purity tantalum plate having an average grain size of less than 30 μm and a standard deviation of the average grain size of less than 3 μm.
A heat treatment method of a high-purity tantalum plate comprises the following steps:
step 1, placing the high-purity tantalum plate subjected to plastic deformation in a heat treatment furnace, heating the high-purity tantalum plate to 500-700 ℃, and carrying out constant-temperature heat treatment for 80-120 min;
step 2, reducing or increasing the heat treatment temperature in the step 1 by 100-200 ℃, and continuously carrying out constant-temperature heat treatment on the high-purity tantalum plate for 70-100 min;
step 3, raising the heat treatment temperature in the step 2 to 1030-1130 ℃, and continuing to perform constant-temperature heat treatment on the high-purity tantalum plate for 60-90 min; and opening the furnace door and cooling to room temperature when the high-purity tantalum plate is cooled to 90-150 ℃ in the heat treatment furnace.
Preferably, in the step 1, the purity of the high-purity tantalum plate is not less than 99.9%.
As a preferred technical scheme, in the step 1, the plastic deformation process of the high-purity tantalum plate comprises the steps of forging the electron beam melting tantalum ingot for one time or multiple times, carrying out annealing treatment after each forging, wherein the sum of equivalent strains generated in the forging process is 3-4,
according to a preferable technical scheme, in the step 1, the plastic deformation process of the high-purity tantalum plate further comprises rolling the forged and annealed electron beam melting-state tantalum ingot, and the sum of equivalent strains generated in the rolling process is 1.5-3.
According to a preferable technical scheme, in the step 1-3, the heat treatment process of the high-purity tantalum plate is carried out under the protection of an argon atmosphere.
As a preferred technical scheme, the temperature rise rate of the heat treatment furnace in the steps 1-3 is 10 ℃/min.
As a preferred technical scheme, in the step 2, the constant-temperature heat treatment temperature is 350-800 DEG C
According to a preferable technical scheme, in the step 1, the constant-temperature heat treatment temperature is 550-650 ℃, and the constant-temperature heat treatment time is 90-150 min; in the step 2, the constant temperature heat treatment temperature is 450-550 ℃ or 650-750 ℃, and the constant temperature heat treatment time is 80-90 min; in the step 3, the constant temperature heat treatment temperature is 1050-1100 ℃, and the constant temperature heat treatment time is 70-80 min.
As a preferable technical scheme, in the step 1, the constant temperature heat treatment temperature is 600 ℃; in the step 2, the constant temperature heat treatment temperature is 500 ℃ or 700 ℃; in the step 3, the constant temperature heat treatment temperature is 1080 ℃.
As a preferable technical scheme, in the step 1, the constant temperature heat treatment temperature is 550 ℃; in the step 2, the constant temperature heat treatment temperature is 450 ℃ or 750 ℃; in the step 3, the constant temperature heat treatment temperature is 1050 ℃.
The invention has at least one of the following beneficial effects: the invention provides a multi-stage annealing process of a high-purity tantalum plate, which enables the deformed tantalum plate to firstly undergo a recovery process and then to be subjected to recrystallization annealing, so that crystal grains can be refined and homogenized more, the tantalum crystal grains can be refined and the uniformity of the tantalum crystal grains can be improved on the premise of not increasing the deformation degree of the tantalum plate, the multi-stage annealing process has the advantages of simple operation, low cost, easiness in realization and the like, is suitable for popularization, and provides a simple and effective method for refining and homogenizing the crystal grains of the high-purity tantalum plate for a target material. The high-purity tantalum plate prepared by the method disclosed by the invention is fine and uniform in crystal grain, the average crystal grain size is less than 30 microns, and the average crystal grain size is reduced by 26-35% compared with that of the tantalum plate prepared by a common heat treatment process under the same deformation degree; the standard deviation of the average grain size is less than 3 mu m, and is reduced by 33-49% compared with the common heat treatment process. Meanwhile, the (222) crystal face texture coefficient of the high-purity tantalum plate prepared by the method is increased by 24% compared with that of the common heat treatment process. The method has important practical value for preparing the high-purity tantalum sputtering target with excellent performance.
Drawings
FIG. 1 is a diagram of the gold phase of the Transverse (TD) -plate Normal (ND) plane of a high purity tantalum plate after treatment in examples and comparative examples, wherein (a) is the gold phase diagram of example 1, (b) is the gold phase diagram of example 2, (c) is the gold phase diagram of comparative example 1, and (d) is the gold phase diagram of comparative example 2;
FIG. 2 is a bar graph of the average grain size of the treated high purity tantalum plates of the examples and comparative examples;
FIG. 3 is an XRD spectrum of rolled surface of high purity tantalum plate after treatment in example 1 and comparative example 1.
Detailed Description
The invention provides a heat treatment method of a high-purity tantalum plate, which comprises the following steps:
step 1, forging a cylindrical tantalum ingot in an electron beam melting state at room temperature for one time or more, preferably, forging each time in an axial direction and four radial directions respectively, wherein the radial direction 1 and the radial direction 2 are perpendicular to each other, the radial direction 3 and the radial direction 4 are perpendicular to each other, and the radial direction 1 and the radial direction 3 form an included angle of 45 degrees; the sum of equivalent strains generated in the forging process is 3-4; annealing treatment is carried out after each forging; finally, performing unidirectional rolling on the forged and annealed blank at room temperature to obtain a high-purity tantalum plate, wherein the sum of equivalent strains generated in the rolling process is 1.5-3; the purity of the obtained high-purity tantalum plate is not less than 99.9%; placing the high-purity tantalum plate obtained after plastic deformation in a heat treatment furnace, filling argon into the heat treatment furnace, heating the high-purity tantalum plate to 500-700 ℃ under the protection of argon atmosphere, wherein the heating rate is 10 ℃/min, and then carrying out constant-temperature heat treatment at 500-700 ℃ for 80-120 min; preferably, the constant temperature heat treatment temperature is 550-650 ℃, or 600-700 ℃, or 500-600 ℃, or 520-560 ℃, or 580-620 ℃, or 630-670 ℃, and the like, and the constant temperature heat treatment time is 90-110 min; more preferably, the constant temperature heat treatment temperature is 500 ℃ or 520 ℃ or 550 ℃ or 570 ℃ or 600 ℃ or 630 ℃ or 650 ℃ or 670 ℃ or 690 ℃ or the like.
Step 2, reducing or increasing the heat treatment temperature in the step 1 by 100-200 ℃, wherein the heating rate is 10 ℃/min, the constant temperature heat treatment temperature is not lower than 350 ℃ and is not more than 800 ℃, and continuously carrying out constant temperature heat treatment on the high-purity tantalum plate for 70-100 min under the protection of argon atmosphere; preferably, the constant temperature heat treatment temperature is 400-450 ℃, or 450-550 ℃, or 650-700 ℃, or 700-800 ℃ and the like, and the constant temperature heat treatment time is 70-90 min; more preferably, the constant temperature heat treatment temperature is 400 ℃ or 450 ℃ or 500 ℃ or 530 ℃ or 550 ℃ or 650 ℃ or 750 ℃ or 780 ℃ or the like.
Step 3, raising the heat treatment temperature in the step 2 to 1030-1130 ℃, wherein the temperature raising rate is 10 ℃/min, and continuously carrying out constant-temperature heat treatment on the high-purity tantalum plate for 60-90 min under the protection of argon atmosphere; stopping heating, cooling the heat treatment furnace for 3-5 hours, opening a furnace door when the temperature of the high-purity tantalum plate is reduced to 90-150 ℃, preferably 100 ℃, and cooling the high-purity tantalum plate to room temperature. Preferably, the constant temperature heat treatment temperature is 1050-1100 ℃ or 1080-1120 ℃ or 1100-1130 ℃, and the constant temperature heat treatment time is 70-80 min; more preferably, the constant temperature heat treatment temperature is 1050 ℃ or 1060 ℃ or 1080 ℃ or 1090 ℃ or 1130 ℃ or the like.
The high-purity tantalum plate obtained by the heat treatment method has fine and uniform crystal grains, the average crystal grain size is less than 30 mu m, and the standard deviation of the average crystal grain size is less than 3 mu m.
The present invention will be described in further detail with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
(1) Plastic deformation of tantalum plate: forging the cylindrical tantalum ingot in an electron beam melting state for three times at room temperature, wherein each forging comprises forging along the axial direction and four radial directions respectively, wherein the radial direction 1 and the radial direction 2 are mutually vertical, the radial direction 3 and the radial direction 4 are mutually vertical, the radial direction 1 and the radial direction 3 form an included angle of 45 degrees, and the total equivalent strain generated in the forging process is 3.4; annealing at 1350 ℃ for 3 hours after the first forging, annealing at 1250 ℃ for 2 hours after the second forging, and annealing at 1150 ℃ for 1 hour after the third forging; finally, unidirectionally rolling the forged and annealed blank at room temperature to obtain a high-purity tantalum plate, wherein the sum of equivalent strains generated in the rolling process is 2.4; (2) third-stage annealing: placing the deformed tantalum plate into a heat treatment furnace, heating to 600 ℃ at a speed of 10 ℃/min, and keeping the temperature for 100 min; then cooling to 500 ℃ at a speed of 10 ℃/min, and preserving heat for 80 min; heating to 1050 deg.C at 10 deg.C/min, and maintaining for 80 min; and after the heat preservation is finished, cooling the tantalum plate along with the furnace for 4 hours, and opening the furnace door to obtain the high-purity tantalum plate.
Example 2
(1) Plastic deformation of tantalum plate: forging the cylindrical tantalum ingot in an electron beam melting state for three times at room temperature, wherein each forging comprises forging along the axial direction and four radial directions respectively, wherein the radial direction 1 and the radial direction 2 are mutually vertical, the radial direction 3 and the radial direction 4 are mutually vertical, the radial direction 1 and the radial direction 3 form an included angle of 45 degrees, and the total equivalent strain generated in the forging process is 3.4; annealing at 1350 ℃ for 3 hours after the first forging, annealing at 1250 ℃ for 2 hours after the second forging, and annealing at 1150 ℃ for 1 hour after the third forging; finally, unidirectionally rolling the forged and annealed blank at room temperature to obtain a high-purity tantalum plate, wherein the sum of equivalent strains generated in the rolling process is 2.4; (2) third-stage annealing: placing the deformed tantalum plate into a heat treatment furnace, heating to 600 ℃ at a speed of 10 ℃/min, and keeping the temperature for 100 min; then heating to 800 ℃ at a speed of 10 ℃/min, and preserving heat for 80 min; heating to 1050 deg.C at 10 deg.C/min, and maintaining for 80 min; and after the heat preservation is finished, cooling the tantalum plate along with the furnace for 4 hours, and opening the furnace door to obtain the high-purity tantalum plate.
Comparative example 1
(1) Preparing a plastic deformation tantalum plate: forging the cylindrical tantalum ingot in an electron beam melting state for three times at room temperature, wherein each forging comprises forging along the axial direction and four radial directions respectively, wherein the radial direction 1 and the radial direction 2 are mutually vertical, the radial direction 3 and the radial direction 4 are mutually vertical, the radial direction 1 and the radial direction 3 form an included angle of 45 degrees, and the total equivalent strain generated in the forging process is 3.4; annealing at 1350 ℃ for 3 hours after the first forging, annealing at 1250 ℃ for 2 hours after the second forging, and annealing at 1150 ℃ for 1 hour after the third forging; finally, unidirectionally rolling the forged and annealed blank at room temperature to obtain a high-purity tantalum plate, wherein the sum of equivalent strains generated in the rolling process is 2.4; (2) primary annealing: placing the deformed tantalum plate into a heat treatment furnace, heating to 1050 ℃ at a speed of 10 ℃/min, and preserving heat for 80 min; and after the heat preservation is finished, cooling the tantalum plate along with the furnace for 4 hours, and opening the furnace door to obtain the high-purity tantalum plate.
Comparative example 2
(1) Preparing a plastic deformation tantalum plate: forging the cylindrical tantalum ingot in an electron beam melting state for three times at room temperature, wherein each forging comprises forging along the axial direction and four radial directions respectively, wherein the radial direction 1 and the radial direction 2 are mutually vertical, the radial direction 3 and the radial direction 4 are mutually vertical, the radial direction 1 and the radial direction 3 form an included angle of 45 degrees, and the total equivalent strain generated in the forging process is 3.4; annealing at 1350 ℃ for 3 hours after the first forging, annealing at 1250 ℃ for 2 hours after the second forging, and annealing at 1150 ℃ for 1 hour after the third forging; finally, unidirectionally rolling the forged and annealed blank at room temperature to obtain a high-purity tantalum plate, wherein the sum of equivalent strains generated in the rolling process is 2.4; (2) secondary annealing: placing the deformed tantalum plate into a heat treatment furnace, heating to 600 ℃ at a speed of 10 ℃/min, and keeping the temperature for 100 min; then heating to 1050 ℃ at a speed of 10 ℃/min, and preserving heat for 80 min; and after the heat preservation is finished, cooling the tantalum plate along with the furnace for 4 hours, and opening the furnace door to obtain the high-purity tantalum plate.
The grain size and uniformity of the tantalum sheets after the heat treatment of the comparative examples and comparative examples were measured according to the following methods and results:
1. the results of observing the Transverse Direction (TD) -Normal Direction (ND) plane microstructures of the tantalum plates after the heat treatment of examples 1-2 and comparative examples 1-2 with an optical microscope are shown in fig. 1, wherein (a) is the microstructure of example 1, (b) is the microstructure of example 2, (c) is the microstructure of comparative example 1, and (d) is the microstructure of comparative example 2;
2. the average grain sizes of the tantalum sheets after heat treatment in examples 1 to 2 and comparative examples 1 to 2 were counted according to the method for measuring average grain size of metals (GB/T6394-2017), and the results are shown in FIG. 2.
3. The change in the grain orientation of the tantalum plates after the heat treatment of example 1 and comparative example 1 was detected by X-ray diffraction analysis (XRD), and the result is shown in fig. 3.
As can be seen from FIG. 1, the grains in FIGS. 1a and 1b are the smallest, the second time in FIG. 1d and the largest in FIG. 1c, so that the grain size of the tantalum sheet treated in examples 1-2 is significantly smaller than that of comparative examples 1-2, and therefore, the grain size of the tantalum sheet in the examples is advantageously reduced by annealing the tantalum sheet three times.
The average grain size and standard deviation of tantalum plates for different annealing processes are counted in fig. 2. The average grain sizes of the tantalum plates treated in examples 1 and 2 were 25.4 μm and 28.2 μm, respectively, and the average grain size of the tantalum plate treated in comparative example 1 was 38.5 μm, respectively, and it can be seen that the average grain sizes of the tantalum plates treated in examples 1 and 2 were reduced by 34% and 26.8% relative to comparative example 1, respectively, when comparing examples 1-2 with comparative example 1. The standard deviation of the average grain size of the tantalum plates in examples 1 and 2 was 2.1 and 2.7 μm, respectively, and the standard deviation of the tantalum plates after treatment in comparative example 1 was 4.1 μm, respectively, and it can be seen that the standard deviation of the tantalum plates after treatment in examples 1 and 2 was reduced by 48.8% and 34.1% relative to comparative example 1, respectively, when comparing examples 1-2 with comparative example 1. Wherein. In comparative example 2, the average grain size of the tantalum plate is higher than 30 μm, and the standard deviation is 2.7 μm, and comparing examples 1-2 with comparative example 2, it can be seen that the average grain size of the tantalum plate after treatment in examples 1-2 is significantly smaller than that in comparative example 2. It can be seen that in examples 1-2, the grain size can be significantly reduced and the grain uniformity can be improved by performing the three-stage annealing on the plastically deformed tantalum sheet.
As can be seen from fig. 3, the intensity of the (222) crystal plane diffraction peak of the sample in example 1 is significantly increased as compared with that in comparative example 1. It was found by calculating the Texture Coefficient (TC) that the TC value of the crystal plane of the sample (222) in example 1 was increased by 24% as compared with that in comparative example 1, and the TC values of the crystal planes of both (200) were close. In summary, compared with the common first-stage annealing process, in the embodiment 1, the high-purity tantalum target material prepared by plastic deformation is subjected to heat treatment by using the three-stage annealing process, so that the grain size of the high-purity tantalum target material can be reduced, the grain uniformity and the orientation rate of the (222) crystal face can be improved, and the deposition rate and uniformity of the tantalum film in the magnetron sputtering process can be improved.
The above are merely characteristic embodiments of the present invention, and do not limit the scope of the present invention in any way. All technical solutions formed by equivalent exchanges or equivalent substitutions fall within the protection scope of the present invention.
Claims (10)
1. A high purity tantalum plate characterized by an average grain size of less than 30 μm and a standard deviation of the average grain size of less than 3 μm.
2. The heat treatment method of the high-purity tantalum plate is characterized by comprising the following steps:
step 1, placing the high-purity tantalum plate subjected to plastic deformation treatment in a heat treatment furnace, heating the high-purity tantalum plate to 500-700 ℃, and carrying out constant-temperature heat treatment for 80-120 min;
step 2, reducing or increasing the heat treatment temperature in the step 1 by 100-200 ℃, and continuously carrying out constant-temperature heat treatment on the high-purity tantalum plate for 70-100 min;
step 3, raising the heat treatment temperature in the step 2 to 1030-1130 ℃, and continuing to perform constant-temperature heat treatment on the high-purity tantalum plate for 60-90 min; and opening the furnace door and cooling to room temperature when the high-purity tantalum plate is cooled to 90-150 ℃ in the heat treatment furnace.
3. The method of claim 2, wherein the heat treatment of the high purity tantalum plate comprises: in the step 1, the purity of the high-purity tantalum plate is not less than 99.9%.
4. The method of claim 2, wherein the heat treatment of the high purity tantalum plate comprises: in the step 1, the plastic deformation treatment of the high-purity tantalum plate comprises the steps of forging the electron beam melting tantalum ingot for one time or multiple times, annealing after each forging, and the sum of equivalent strains generated in the forging process is 3-4.
5. The method of claim 4, wherein the heat treatment of the high purity tantalum plate comprises: in the step 1, the plastic deformation treatment of the high-purity tantalum plate further comprises rolling the forged and annealed electron beam smelted tantalum ingot, wherein the sum of equivalent strains generated in the rolling process is 1.5-3.
6. The method of claim 5, wherein the heat treatment of the high purity tantalum plate comprises: in the step 1-3, the heat treatment process of the high-purity tantalum plate is carried out under the protection of argon atmosphere, and the heating rate of the heat treatment furnace is 10 ℃/min.
7. The method of claim 2, wherein the heat treatment of the high purity tantalum plate comprises: in the step 2, the constant temperature heat treatment temperature is 350-800 ℃.
8. The method of claim 2, wherein the heat treatment of the high purity tantalum plate comprises: in the step 1, the constant temperature heat treatment temperature is 550-650 ℃, and the constant temperature heat treatment time is 90-150 min; in the step 2, the constant temperature heat treatment temperature is 450-550 ℃ or 650-750 ℃, and the constant temperature heat treatment time is 80-90 min; in the step 3, the constant temperature heat treatment temperature is 1050-1100 ℃, and the constant temperature heat treatment time is 70-80 min.
9. The method of claim 2, wherein the heat treatment of the high purity tantalum plate comprises: in the step 1, the constant temperature heat treatment temperature is 600 ℃; in the step 2, the constant temperature heat treatment temperature is 500 ℃ or 700 ℃; in the step 3, the constant temperature heat treatment temperature is 1080 ℃.
10. The method of claim 2, wherein the heat treatment of the high purity tantalum plate comprises: in the step 1, the constant temperature heat treatment temperature is 550 ℃; in the step 2, the constant temperature heat treatment temperature is 450 ℃ or 750 ℃; in the step 3, the constant temperature heat treatment temperature is 1050 ℃.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116288091A (en) * | 2023-03-28 | 2023-06-23 | 南昌大学 | Annealing process for preparing superfine grain tantalum sheet at low temperature |
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| CN112251692B (en) | 2021-08-27 |
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