CN114875369A - Low-oxygen tantalum target material and preparation method thereof - Google Patents
Low-oxygen tantalum target material and preparation method thereof Download PDFInfo
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- CN114875369A CN114875369A CN202210516810.7A CN202210516810A CN114875369A CN 114875369 A CN114875369 A CN 114875369A CN 202210516810 A CN202210516810 A CN 202210516810A CN 114875369 A CN114875369 A CN 114875369A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/023—Hydrogen absorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention provides a low-oxygen tantalum target material and a preparation method thereof, wherein the preparation method comprises the following steps: (1) placing the tantalum source in a hydrogenation device, vacuumizing, introducing hydrogen for heating, and stopping heating when the pressure in the hydrogenation device does not decrease any more to obtain a tantalum hydride source; (2) sequentially crushing and heat-treating the tantalum hydride source in the step (1) to obtain tantalum hydride powder; (3) and (3) sequentially carrying out cold isostatic pressing, vacuum sintering, degassing treatment and hot isostatic pressing on the dehydrotantalum powder in the step (2) to obtain the low-oxygen tantalum target material. According to the invention, the dehydro-tantalum powder is combined with cold isostatic pressing, vacuum sintering and hot isostatic pressing, so that the oxygen content of the tantalum target material is greatly reduced, the oxygen content of the tantalum target material is lower than 100ppm, the purity and the density of the tantalum target material are ensured, the density is as high as 99.9%, the purity is as high as 99.9999%, and the method has a good industrial application prospect.
Description
Technical Field
The invention belongs to the technical field of target preparation, and particularly relates to a low-oxygen tantalum target and a preparation method thereof.
Background
In the field of microelectronics, tantalum targets are commonly used for preparing thin film electrodes, interconnection lines and barrier layers of semiconductor devices, and the purity and gas content requirements of the tantalum targets are very high. With the rapid development of the semiconductor industry, the demand for the target material is increasing, and the target material becomes an indispensable key material for the development of the semiconductor industry. The quality of the target directly affects the quality of the wafer, and the grain size, internal structure and texture orientation of the target have great influence on the preparation and performance of the metal film of the integrated circuit.
At present, the sputtering tantalum target is mainly prepared into a tantalum ingot by a traditional smelting method, and then plastic deformation and annealing are carried out for many times. CN106521434B discloses a preparation method of a high-purity tantalum target material with preferred orientation, which comprises the following steps: (1) cogging tantalum ingots, then pickling, and annealing in a vacuum annealing furnace; (2) carrying out primary rolling and secondary rolling on the tantalum material subjected to annealing treatment, wherein the direction of the secondary rolling is vertical to the direction of the primary rolling; (3) pickling the rolled tantalum material, and then carrying out vacuum annealing treatment in a vacuum heat treatment furnace; (4) rolling for the third time, wherein the rolling direction is the same as the first rolling direction; (5) rolling for the fourth time, wherein the rolling direction is the same as the third rolling direction; (6) and (3) pickling the rolled tantalum material, and then annealing in a vacuum heat treatment furnace. The tantalum target blank with uniform grain size and internal texture is prepared by the preparation method, but the sputtering performance of the target is seriously influenced by the internal 'inherent texture belt'. Meanwhile, the preparation method has the disadvantages of complex process, long flow and low yield, and the cost for preparing the tantalum target material is high.
CN105177513A discloses a method for preparing a high-performance tantalum target material by a powder metallurgy method, which comprises the following steps: and (3) performing discharge plasma sintering on the tantalum powder, cooling to a temperature not higher than 160 ℃, demolding, and machining the obtained tantalum target blank to obtain the tantalum target. The method for preparing the tantalum target by adopting the powder metallurgy method is beneficial to obtaining the internal structure with uniform granularity and no texture, and simultaneously greatly improves the processing performance of the tantalum target. However, tantalum powder is easy to absorb oxygen, and oxygen is introduced in the powder preparation process, so that the oxygen content of the tantalum target prepared by the powder metallurgy method exceeds the standard. If the low-oxygen tantalum powder material is prepared, procedures such as oxygen reduction and acid washing are required, the oxygen reduction and acid washing procedures can cause the risk of increasing the content of metal impurities, carbon and the like, the oxygen reduction effect is very limited, and the oxygen content of the tantalum powder can be controlled to be less than or equal to 500ppm after the oxygen reduction.
In summary, how to provide a method for preparing a high-purity low-oxygen tantalum target material, which reduces the oxygen content and internal defects of the tantalum target material, improves the purity and yield of the tantalum target material, and reduces the process cost and energy consumption, becomes a problem to be solved by those skilled in the art.
Disclosure of Invention
In order to solve the technical problems, the invention provides the low-oxygen tantalum target material and the preparation method thereof, and the preparation method combines cold isostatic pressing, vacuum sintering and hot isostatic pressing of the dehydrotantalum powder, so that the oxygen content of the tantalum target material is greatly reduced, and the purity and the density of the tantalum target material are ensured.
In order to achieve the technical effect, the invention adopts the following technical scheme:
the invention provides a preparation method of a low-oxygen tantalum target material, which comprises the following steps:
(1) placing the tantalum source in a hydrogenation device, vacuumizing, introducing hydrogen for heating, and stopping heating when the pressure in the hydrogenation device does not decrease any more to obtain a tantalum hydride source;
(2) sequentially crushing and heat-treating the tantalum hydride source in the step (1) to obtain tantalum hydride powder;
(3) and (3) sequentially carrying out cold isostatic pressing, vacuum sintering, degassing treatment and hot isostatic pressing on the dehydrotantalum powder in the step (2) to obtain the low-oxygen tantalum target material.
According to the preparation method, the tantalum hydride source obtained by hydrogenating the tantalum source is crushed and thermally treated to obtain the dehydrotantalum powder, and the dehydrotantalum powder is sequentially subjected to a combined mode of cold isostatic pressing, vacuum sintering, degassing treatment and hot isostatic pressing, so that the oxygen content of the tantalum target is greatly reduced, the introduction of other metal impurities in the oxygen reduction and acid washing processes of the traditional low-oxygen tantalum powder is avoided, the purity and the density of the tantalum target are ensured, and the preparation method has a good industrial application prospect.
In a preferred embodiment of the present invention, the purity of the tantalum source in step (1) is > 99.99%, and may be, for example, 99.991%, 99.992%, 99.993%, 99.994%, 99.995%, 99.996%, 99.997%, 99.998%, or 99.999%, but the present invention is not limited to the above-mentioned values, and other values not listed in the numerical range may be similarly applied.
As a preferred embodiment of the present invention, the temperature of the hydrogenation heating in the step (1) is 600-700 ℃, for example, 600 ℃, 610 ℃, 620 ℃, 630 ℃, 640 ℃, 650 ℃, 660 ℃, 670 ℃, 680 ℃, 690 ℃, or 700 ℃, but is not limited to the recited values, and other values not recited in the numerical range are also applicable.
As a preferred embodiment of the present invention, the temperature of the heat treatment in the step (2) is 400-600 ℃, for example, 400 ℃, 420 ℃, 440 ℃, 460 ℃, 480 ℃, 500 ℃, 520 ℃, 540 ℃, 560 ℃, 580 ℃ or 600 ℃, but is not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the time of the heat treatment in step (2) is 100-140min, such as 100min, 105min, 110min, 115min, 120min, 125min, 130min, 135min or 140min, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
In the present invention, the crushing is performed by using a pair of rolls and a jet mill in this order, both of which are provided with a liner made of tantalum having a purity of 99.99% or more, for example, 99.991%, 99.993%, 99.995%, 99.997%, 99.999%, or the like, but not limited to the above-mentioned values, and other values not listed in the numerical range are also applicable.
Preferably, the heat treatment in step (2) is followed by a sieving treatment.
Preferably, the sieving treatment screens out the tantalum hydride powder with the particle size of 180-325 meshes, such as 180 meshes, 200 meshes, 220 meshes, 240 meshes, 260 meshes, 280 meshes, 300 meshes, 320 meshes or 325 meshes, but the sieving treatment is not limited to the enumerated values, and other unrecited values in the numerical range are also applicable.
In a preferred embodiment of the present invention, the cold isostatic pressing pressure in step (3) is 160-240Mpa, such as 160Mpa, 170Mpa, 180Mpa, 190Mpa, 200Mpa, 210Mpa, 220Mpa, 230Mpa, or 240Mpa, but the pressure is not limited to the above values, and other values not listed in the numerical range are also applicable.
Preferably, the cold isostatic pressing in step (3) has a dwell time of 10-20min, such as 10min, 12min, 14min, 16min, 18min or 20min, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, a cold pressed blank is obtained after said cold isostatic pressing of step (3).
In the present invention, the cold isostatic pressing is performed in a gum cover seal.
As a preferable technical scheme of the invention, the vacuum degree of the vacuum sintering in the step (3) is less than or equal to 5 multiplied by 10 -4 Pa, for example, may be 10 -6 Pa、10 -5 Pa、3×10 -5 Pa、5×10 -5 Pa、7×10 -5 Pa、9×10 -5 Pa or 5X 10 -4 Pa, etc., but are not limited to the recited values, and other values not recited within the numerical range are also applicable.
Preferably, the temperature of the vacuum sintering in step (3) is 2200-.
Preferably, the vacuum sintering in step (3) is carried out for 4-6h, such as 4h, 4.2h, 4.4h, 4.6h, 4.8h, 5h, 5.2h, 5.4h, 5.6h, 5.8h or 6h, but not limited to the recited values, and other values in the range of values are also applicable.
In the invention, the gas in the air holes is escaped in a vacuum sintering mode, so that the oxygen content in the tantalum target material is greatly reduced.
As a preferable technical scheme of the invention, before the degassing treatment in the step (3), the blank after vacuum sintering is placed in a sheath for welding.
In the invention, the sheath is made of stainless steel.
Preferably, the degassing treatment temperature in step (3) is 400-.
Preferably, the degassing treatment in step (3) is carried out for 6-9h, such as 6h, 6.5h, 7h, 7.5h, 8h, 8.5h or 9h, but not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the vacuum degree in the envelope in the step (3) is 1.0 × 10 -3 -1.0×10 -2 Pa, for example, may be 1.0X 10 -3 Pa、2.0×10 -3 Pa、3.0×10 -3 Pa、4.0×10 -3 Pa、5.0×10 -3 Pa、6.0×10 -3 Pa、7.0×10 -3 Pa、8.0×10 -3 Pa、9.0×10 -3 Pa or 1.0X 10 -2 Pa, etc., but are not limited to the recited values, and other values not recited within the numerical range are also applicable.
In a preferred embodiment of the present invention, the hot isostatic pressing temperature in step (3) is 1000-1250 ℃, and may be, for example, 1000 ℃, 1050 ℃, 1100 ℃, 1150 ℃, 1200 ℃ or 1250 ℃, but the present invention is not limited to the above-mentioned values, and other values not shown in the numerical range are also applicable.
Preferably, the hot isostatic pressing pressure in step (3) is 170-180Mpa, such as 170Mpa, 172Mpa, 174Mpa, 176Mpa, 178Mpa or 180Mpa, but not limited to the recited values, and other values in the range of values are also applicable.
Preferably, the dwell time of the hot isostatic pressing in step (3) is 3-6h, for example, 3h, 3.5h, 4h, 4.5h, 5h, 5.5h or 6h, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the tantalum target crude product is obtained after the hot isostatic pressing in the step (3).
Preferably, the tantalum target crude product is machined to obtain the low-oxygen tantalum target.
In the present invention, the post-hiping pack is machined.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) placing the tantalum source with the purity of more than 99.99 percent in a hydrogenation device, vacuumizing, introducing hydrogen, heating to 600-700 ℃, and stopping heating when the pressure in the hydrogenation device is not reduced any more to obtain the tantalum hydride source;
(2) crushing the tantalum hydride source in the step (1), performing heat treatment at the temperature of 400-;
(3) performing cold isostatic pressing on the dehydrogenation tantalum powder in the step (2) for 10-20min at the pressure of 160-240Mpa to obtain a cold-pressed blank, and then performing vacuum sintering at the temperature of 2200-2600 ℃ for 4-6h, wherein the vacuum degree of the vacuum sintering is less than or equal to 5 multiplied by 10 -4 Pa; placing the blank after vacuum sintering into a sheath for welding, degassing at 400-600 deg.C for 6-9h, wherein the vacuum degree in the sheath is 1.0 × 10 -3 -1.0×10 -2 Pa, hot isostatic pressing for 3-6h at 1250 ℃ and 180MPa at 1000-.
The invention also provides a low-oxygen tantalum target material which is prepared by the preparation method.
The oxygen content of the low-oxygen tantalum target material is less than or equal to 100ppm, for example, 50ppm, 60ppm, 70ppm, 80ppm, 90ppm, 100ppm, etc., but the low-oxygen tantalum target material is not limited to the recited values, and other values not recited in the numerical range are also applicable.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method prepares the tantalum hydride source into the tantalum hydride source after heat treatment, adopts a vacuum sintering mode, and escapes gas in air holes under a certain vacuum degree by increasing the sintering temperature; the method combines cold isostatic pressing, vacuum sintering and hot isostatic pressing, the oxygen content of the tantalum target material is lower than 100ppm, the purity and the density of the tantalum target material are ensured, the density is as high as 99.9%, the purity is as high as 99.9999%, and the method has a good industrial application prospect.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a preparation method of a low-oxygen tantalum target material, which comprises the following steps:
(1) placing tantalum ingots with the purity of 99.993% in a hydrogenation device, vacuumizing, introducing hydrogen, heating to 650 ℃, and stopping heating when the pressure in the hydrogenation device does not decrease any more to obtain a tantalum hydride source;
(2) crushing the tantalum hydride source in the step (1) by adopting a roll crusher and a jet mill, then carrying out heat treatment at 500 ℃ for 120min, and screening to obtain the tantalum hydride powder with the granularity of 250 meshes;
(3) sealing the dehydrotantalum powder obtained in the step (2) in a rubber sleeve, carrying out cold isostatic pressing for 15min under 175Mpa to obtain a cold-pressed blank, and carrying out vacuum sintering at 2400 ℃ for 5h with the vacuum degree of 5 multiplied by 10 -5 Pa; placing the blank after vacuum sintering into a stainless steel sheath for welding, degassing at 500 deg.C for 8 hr, wherein the vacuum degree in the stainless steel sheath is 5.0 × 10 -3 And Pa, hot isostatic pressing for 5 hours at 1100 ℃ and 175Mpa, removing the stainless steel ladle sleeve, and machining to obtain the low-oxygen tantalum target material.
Example 2
The embodiment provides a preparation method of a low-oxygen tantalum target material, which comprises the following steps:
(1) placing tantalum ingots with the purity of 99.999% in a hydrogenation device, vacuumizing, introducing hydrogen, heating to 600 ℃, and stopping heating when the pressure in the hydrogenation device does not decrease any more to obtain a tantalum hydride source;
(2) crushing the tantalum hydride source in the step (1) by adopting a roll crusher and a jet mill, then carrying out heat treatment at 400 ℃ for 140min, and screening to obtain the tantalum hydride powder with the granularity of 180 meshes;
(3) sealing the dehydrotantalum powder obtained in the step (2) in a rubber sleeve, carrying out cold isostatic pressing for 20min under 160Mpa to obtain a cold-pressed blank, and carrying out vacuum sintering at 2200 ℃ for 6h, wherein the vacuum degree of the vacuum sintering is 9 multiplied by 10 -5 Pa; placing the blank after vacuum sintering into a stainless steel sheath for welding, degassing for 9h at 400 ℃, wherein the vacuum degree in the stainless steel sheath is 1.0 multiplied by 10 -3 And Pa, hot isostatic pressing for 6h at 1000 ℃ and 170Mpa, removing the stainless steel ladle sleeve, and machining to obtain the low-oxygen tantalum target material.
Example 3
The embodiment provides a preparation method of a low-oxygen tantalum target material, which comprises the following steps:
(1) placing tantalum ingots with the purity of 99.991% in a hydrogenation device, vacuumizing, introducing hydrogen, heating to 700 ℃, and stopping heating when the pressure in the hydrogenation device does not decrease any more to obtain a tantalum hydride source;
(2) crushing the tantalum hydride source in the step (1) by adopting a roll crusher and a jet mill, then carrying out heat treatment at 600 ℃ for 100min, and screening to obtain 325-mesh dehydrotantalum powder;
(3) sealing the dehydrotantalum powder obtained in the step (2) in a rubber sleeve, carrying out cold isostatic pressing for 10min under 190Mpa to obtain a cold-pressed blank, and carrying out vacuum sintering at 2600 ℃ for 4h with the vacuum degree of 5 multiplied by 10 -4 Pa; placing the blank after vacuum sintering into a stainless steel sheath for welding, degassing for 6h at 600 ℃, wherein the vacuum degree in the stainless steel sheath is 1.0 multiplied by 10 -2 PaAnd hot isostatic pressing at 1250 ℃ and 180Mpa for 3h, removing the stainless steel ladle sleeve, and machining to obtain the low-oxygen tantalum target material.
Example 4
This example is different from example 1 only in that the conditions are the same as example 1 except that the temperature of the heat treatment in step (2) is 350 ℃.
Example 5
This example is different from example 1 only in that the conditions are the same as example 1 except that the temperature of the heat treatment in step (2) is 650 ℃.
Example 6
This example is different from example 1 only in that the conditions were the same as example 1 except that the temperature of the vacuum sintering in step (3) was 2100 ℃.
Example 7
This example is different from example 1 only in that the conditions were the same as example 1 except that the temperature of the vacuum sintering in step (3) was 2700 ℃.
Example 8
This example is different from example 1 only in that the conditions were the same as in example 1 except that the hot isostatic pressing pressure in step (3) was 160 MPa.
Example 9
This example is different from example 1 only in that the conditions of example 1 were the same except that the hot isostatic pressing pressure in step (3) was 190 MPa.
Comparative example 1
This comparative example is different from example 1 only in that example 1 is identical in all conditions except that the step (2) of the production method is not heat-treated.
Comparative example 2
This comparative example is different from example 1 only in that example 1 is identical in other conditions than the preparation method step (3) in which vacuum sintering is not performed.
50 tantalum targets were prepared by the methods described in examples 1-9 and comparative examples 1-2, and the average oxygen content, average purity, and average density were determined, with the results shown in Table 1.
TABLE 1
From table 1 it can be derived: according to the preparation method of the low-oxygen tantalum target material, the oxygen content in the tantalum target material is lower than 160ppm, the average purity is as high as 99.9999%, and the average density is as high as more than 99%; according to the preparation method, the tantalum hydride source is prepared to obtain the dehydrotantalum source after heat treatment, gas in the air holes is escaped at a specific sintering temperature and a certain vacuum degree by adopting a vacuum sintering mode, and the dehydrotantalum powder is subjected to a mode of combining cold isostatic pressing, vacuum sintering and hot isostatic pressing, so that the oxygen content of the tantalum target material is greatly reduced, and the purity and the density of the tantalum target material are ensured.
In the step (2) of the comparative example 1, the dehydrotantalum powder cannot be obtained without heat treatment, so that the oxygen content of the tantalum target material is increased; in contrast, in the step (3) of the comparative example 2, vacuum sintering is not performed, and more oxygen is introduced, so that the oxygen content of the tantalum target is increased and the compactness of the tantalum target is reduced.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. The preparation method of the low-oxygen tantalum target is characterized by comprising the following steps:
(1) placing the tantalum source in a hydrogenation device, vacuumizing, introducing hydrogen for heating, and stopping heating when the pressure in the hydrogenation device does not decrease any more to obtain a tantalum hydride source;
(2) sequentially crushing and heat-treating the tantalum hydride source in the step (1) to obtain tantalum hydride powder;
(3) and (3) sequentially carrying out cold isostatic pressing, vacuum sintering, degassing treatment and hot isostatic pressing on the dehydrotantalum powder in the step (2) to obtain the low-oxygen tantalum target material.
2. The method of claim 1, wherein the tantalum source of step (1) has a purity of > 99.99%.
3. The production method according to claim 1 or 2, wherein the temperature of the hydrogenation heating in step (1) is 600-700 ℃.
4. The method according to any one of claims 1 to 3, wherein the temperature of the heat treatment in step (2) is 400-600 ℃;
preferably, the time of the heat treatment in the step (2) is 100-140 min;
preferably, the heat treatment in the step (2) is followed by a sieving treatment;
preferably, the sieving treatment screens out tantalum hydride powder with the granularity of 180-325 meshes.
5. The method according to any one of claims 1 to 4, wherein the cold isostatic pressing in step (3) is carried out at a pressure of 160-240 MPa;
preferably, the pressure holding time of the cold isostatic pressing in the step (3) is 10-20 min;
preferably, a cold pressed blank is obtained after said cold isostatic pressing of step (3).
6. The production method according to any one of claims 1 to 5, wherein the degree of vacuum in the vacuum sintering in the step (3) is 5X 10 or less -4 Pa；
Preferably, the temperature of the vacuum sintering in the step (3) is 2200-2600 ℃;
preferably, the vacuum sintering in the step (3) has the holding time of 4-6 h.
7. The method according to any one of claims 1 to 6, wherein before the degassing treatment in step (3), the vacuum-sintered blank is put into a sheath for welding;
preferably, the temperature of the degassing treatment in the step (3) is 400-600 ℃;
preferably, the degassing treatment time in the step (3) is 6-9 h;
preferably, the vacuum degree in the envelope in the step (3) is 1.0 × 10 -3 -1.0×10 -2 Pa。
8. The method according to any one of claims 1-7, wherein the temperature of the hot isostatic pressing in step (3) is 1000-1250 ℃;
preferably, the pressure of the hot isostatic pressing in the step (3) is 170-180 MPa;
preferably, the dwell time of the hot isostatic pressing in step (3) is 3-6 h;
preferably, a tantalum target crude product is obtained after the hot isostatic pressing in the step (3);
preferably, the tantalum target crude product is machined to obtain the low-oxygen tantalum target.
9. The method of any one of claims 1 to 8, comprising the steps of:
(1) placing the tantalum source with the purity of more than 99.99 percent in a hydrogenation device, vacuumizing, introducing hydrogen, heating to 600-700 ℃, and stopping heating when the pressure in the hydrogenation device is not reduced any more to obtain the tantalum hydride source;
(2) crushing the tantalum hydride source in the step (1), performing heat treatment at the temperature of 400-;
(3) performing cold isostatic pressing on the dehydrogenation tantalum powder in the step (2) for 10-20min at the pressure of 160-240Mpa to obtain a cold-pressed blank, and then performing vacuum sintering at the temperature of 2200-2600 ℃ for 4-6h, wherein the vacuum degree of the vacuum sintering is less than or equal to 5 multiplied by 10 -4 Pa; placing the blank after vacuum sintering into a sheath for welding, degassing for 6-9h at the temperature of 400-,the vacuum degree in the envelope is 1.0 multiplied by 10 -3 -1.0×10 -2 Pa, hot isostatic pressing for 3-6h at 1250 ℃ and 180MPa at 1000-.
10. A tantalum target material with low oxygen content, wherein the tantalum target material with low oxygen content is prepared by the preparation method according to any one of claims 1 to 9;
the oxygen content of the low-oxygen tantalum target material is less than or equal to 100 ppm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116332645A (en) * | 2023-03-29 | 2023-06-27 | 宁波江丰电子材料股份有限公司 | Molybdenum oxide tantalum target material and preparation method and application thereof |
| CN116970913A (en) * | 2023-07-31 | 2023-10-31 | 宁波江丰电子材料股份有限公司 | Tantalum target material and preparation method and application thereof |
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| CN113235056A (en) * | 2021-05-19 | 2021-08-10 | 宁波江丰电子材料股份有限公司 | Preparation method of high-purity tantalum target material |
| CN113981390A (en) * | 2021-10-29 | 2022-01-28 | 宁波江丰半导体科技有限公司 | Preparation method of high-purity low-oxygen tantalum target material |
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| CN113235056A (en) * | 2021-05-19 | 2021-08-10 | 宁波江丰电子材料股份有限公司 | Preparation method of high-purity tantalum target material |
| CN113981390A (en) * | 2021-10-29 | 2022-01-28 | 宁波江丰半导体科技有限公司 | Preparation method of high-purity low-oxygen tantalum target material |
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| CN116970913A (en) * | 2023-07-31 | 2023-10-31 | 宁波江丰电子材料股份有限公司 | Tantalum target material and preparation method and application thereof |
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