CN113235056A - Preparation method of high-purity tantalum target material - Google Patents
Preparation method of high-purity tantalum target material Download PDFInfo
- Publication number
- CN113235056A CN113235056A CN202110548252.8A CN202110548252A CN113235056A CN 113235056 A CN113235056 A CN 113235056A CN 202110548252 A CN202110548252 A CN 202110548252A CN 113235056 A CN113235056 A CN 113235056A
- Authority
- CN
- China
- Prior art keywords
- tantalum
- isostatic pressing
- purity
- target material
- cold
- 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.)
- Pending
Links
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 118
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 79
- 239000013077 target material Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 48
- 239000000843 powder Substances 0.000 claims abstract description 32
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 28
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 27
- 238000007872 degassing Methods 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000001257 hydrogen Substances 0.000 claims abstract description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 11
- 229910001220 stainless steel Inorganic materials 0.000 claims description 21
- 239000010935 stainless steel Substances 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 13
- 238000003466 welding Methods 0.000 claims description 7
- 238000003754 machining Methods 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000012216 screening Methods 0.000 claims description 5
- 239000012043 crude product Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 239000000956 alloy Substances 0.000 claims 1
- 229910001256 stainless steel alloy Inorganic materials 0.000 claims 1
- 230000003068 static effect Effects 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 26
- 239000001301 oxygen Substances 0.000 abstract description 26
- 229910052760 oxygen Inorganic materials 0.000 abstract description 26
- 239000000047 product Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 229920000742 Cotton Polymers 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000005240 physical vapour deposition Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 238000005477 sputtering target Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000010884 ion-beam technique Methods 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
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
- 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]
-
- 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
-
- 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
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
-
- 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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention provides a preparation method of a high-purity tantalum target material, which comprises the following steps: placing the high-purity tantalum source in a hydrogenation furnace, vacuumizing, introducing hydrogen for heating after vacuumizing, and stopping heating after the pressure in the hydrogenation furnace is not reduced any more to obtain a tantalum hydride source; crushing the obtained tantalum hydride source, and then sequentially carrying out cold isostatic pressing, degassing treatment and hot isostatic pressing to obtain a high-purity tantalum target material; the preparation method adopts tantalum hydride powder, and combines a cold isostatic pressing process and a hot isostatic pressing process, so that the oxygen content of the obtained tantalum target material is effectively reduced, the yield of the tantalum target material is improved, 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 preparation method of a high-purity tantalum target.
Background
Physical Vapor Deposition (PVD) refers to a process of evaporating a material source by using a low-voltage and large-current arc discharge technique under a vacuum condition, ionizing both evaporated substances and gas by using gas discharge, and then depositing the evaporated substances and reaction products thereof on a workpiece by an acceleration action of an electric field to form a film with a special function. The PVD technology is the core technology of various industries such as semiconductor chip manufacturing industry, solar energy industry, LCD manufacturing industry and the like, and the main methods comprise vacuum evaporation, arc plasma plating, ion coating, molecular beam epitaxy, sputtering coating and the like.
Sputtering is one of the main techniques for preparing thin film materials, and is characterized in that ions generated by an ion source are accelerated and gathered in vacuum to form ion beam flow with high speed energy, the ion beam flows bombard the surface of a solid, kinetic energy exchange is carried out between the ions and atoms on the surface of the solid, the atoms on the surface of the solid leave the solid and are deposited on the surface of a substrate, and the bombarded solid is a raw material for preparing a thin film deposited by a sputtering method and is generally called as a sputtering target material.
Sputtering targets are generally obtained by powder metallurgy sintering molding processes because the sputtering targets prepared by the processes have unique chemical compositions and mechanical and physical properties that cannot be obtained by conventional fusion casting methods. The tantalum target material is used as a common target material for preparing a film electrode, an interconnection line and a barrier layer of a semiconductor device, and has very high requirements on the purity and the gas content in the using process. The tantalum target material prepared by the powder metallurgy method is beneficial to obtaining an internal structure with uniform granularity and no texture, and simultaneously, the processing performance of the tantalum target material is greatly improved, but oxygen is introduced into the steps of crushing, high-temperature dehydrogenation, acid washing and the like involved in the raw material powder preparation process, and the oxygen content is difficult to control, so that the oxygen content of the tantalum target material exceeds the standard; in addition, the tantalum powder has low loose packing density, so that the yield is low when the tantalum powder is directly sintered. Therefore, the method for reducing the oxygen content in the tantalum target and improving the yield of the tantalum target has important significance.
CN103147050A discloses a production method of a high-purity tantalum target, which comprises the steps of (1) placing a tantalum block with the size of 5-10 mm multiplied by 5-10 mm in a hydrogenation furnace for hydrogen absorption; (2) crushing the tantalum after hydrogen absorption into powder of 200 meshes, placing the powder in a steel sheath, heating and exhausting according to a certain speed and stage, then placing the steel sheath in a hot isostatic pressing machine for sintering, wherein the sintering temperature is 1100-1500 ℃, the atmosphere pressure is 50-200 MPa, finally machining and cutting the powder into a specified shape. According to the method, the obtained powder is directly subjected to degassing treatment, the powder is low in loose packing density and easy to escape, subsequent hot isostatic pressing is influenced, the deformation amount of the sintered target material is large, and the yield is low.
In summary, it is an urgent need to provide a method for reducing oxygen content and increasing target yield while ensuring target purity.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a preparation method of a high-purity tantalum target material, wherein tantalum hydride powder is adopted in the preparation method, and a cold isostatic pressing process and a hot isostatic pressing process are combined, so that the oxygen content of the obtained tantalum target material is effectively reduced, and the yield of the tantalum target material is improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a high-purity tantalum target material, which comprises the following steps:
(1) placing the high-purity tantalum source in a hydrogenation furnace, vacuumizing, introducing hydrogen for heating after vacuumizing, and stopping heating after the pressure in the hydrogenation furnace is not reduced any more to obtain a tantalum hydride source;
(2) and (2) crushing the tantalum hydride source obtained in the step (1), and then sequentially carrying out cold isostatic pressing, degassing treatment and hot isostatic pressing to obtain the high-purity tantalum target material.
According to the preparation method, the crushed tantalum hydride source is subjected to cold isostatic pressing forming, so that powder is changed into a tightly combined block from a granular state, high-temperature cotton is not required to be added in the subsequent degassing process to prevent powder pumping, oxygen element introduced by the addition of the high-temperature cotton is avoided, and then the tantalum hydride source is sintered through hot isostatic pressing, so that the oxygen content in the tantalum target material is effectively reduced, the compactness and the yield of the tantalum target material are improved, and the preparation method is favorable for industrial application.
According to the invention, the tantalum hydride powder is simple to prepare and strong in operability, the subsequent acid washing and drying processes can be avoided by preparing the tantalum target material through the tantalum hydride powder, the introduction of oxygen is effectively avoided, and hydrogen and oxygen in the later-stage tantalum hydride can be removed through degassing treatment.
The following technical solutions are preferred technical solutions of the present invention, but not limited to the technical solutions provided by the present invention, and technical objects and advantageous effects of the present invention can be better achieved and achieved by the following technical solutions.
As a preferable technical scheme of the invention, the high-purity tantalum source in the step (1) comprises tantalum ingots.
In a preferred embodiment of the present invention, the purity of the high purity tantalum source in step (1) is not less than 4N, such as 99.99%, 99.991%, 99.992%, or 99.999%, but not limited to the recited values, and other values not recited in the range of values are also applicable.
In a preferred embodiment of the present invention, the heating temperature in the step (1) is 600 to 700 ℃, for example, 600 ℃, 620 ℃, 640 ℃, 660 ℃, 680 ℃, or 700 ℃, but the temperature is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
As a preferable technical scheme of the invention, the crushing in the step (2) is carried out by adopting a double-roller mill and an air flow pulverizer in sequence.
Preferably, the twin-roll mill and the air flow mill are both provided with an inner liner.
Preferably, the liner is made of tantalum having a purity of not less than 4N, such as 99.99%, 99.991%, 99.992%, 99.999%, and the like, but not limited to the recited values, and other values not recited in the range are also applicable.
In the crushing and screening process, the inner lining of the equipment in contact with the tantalum source is made of tantalum with the purity not less than 4N, so that the introduction of impurity elements is effectively reduced, and acid washing and purification are not required in the later stage, thereby reducing the introduction of oxygen and reducing the oxygen content.
In a preferred embodiment of the present invention, after the crushing in step (2), the tantalum hydride powder having a particle size of 180 to 325 mesh, for example, 180 mesh, 200 mesh, 230 mesh, 270 mesh or 325 mesh, is screened, but the method is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
As a preferable technical scheme of the invention, the cold isostatic pressing in the step (2) is carried out by adopting rubber sleeve sealing.
Preferably, the cold isostatic pressing in step (2) has a pressure of 160 to 190MPa, such as 160MPa, 170MPa, 180MPa or 190MPa, but not limited to the recited values, and other values not recited in the range of values are also applicable.
In the present invention, the pressure of the cold isostatic pressing needs to be controlled. If the pressure is too low, the density does not reach the standard, and the blank is easy to deform when hot isostatic pressing treatment is carried out at the later stage; if the pressure is too high, the billet will break.
Preferably, the cold isostatic pressing in step (2) is performed for 20-30 min, such as 20min, 22min, 24min, 26min, 28min or 30min, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the cold isostatic pressing in step (2) is carried out to obtain a cold pressed blank.
As a preferable technical scheme of the invention, before the degassing treatment in the step (2), the cold-pressed blank is placed in a stainless steel sheath for welding.
Preferably, the degassing treatment in step (2) is performed at a temperature of 400 to 600 ℃, for example, 400 ℃, 450 ℃, 500 ℃, 550 ℃ or 600 ℃, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the degassing treatment in step (2) is carried out for 6-9 h, such as 6h, 7h, 8h or 9h, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the degassing treatment of step (2)Then, the pressure in the stainless steel jacket is 10-3～10-2Pa, e.g. 10-3Pa、2×10-3Pa、5×10-3Pa、7×10-3Pa or 10-2Pa, etc., but are not limited to the recited values, and other values not recited within the range of values are also applicable.
In a preferred embodiment of the present invention, the hot isostatic pressing temperature in step (2) is 1000 to 1250 ℃, for example, 1000 ℃, 1050 ℃, 1100 ℃, 1150 ℃, 1200 ℃ or 1250 ℃, but the temperature is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the hot isostatic pressing in step (2) is performed at a pressure of 170 to 180MPa, such as 170MPa, 175MPa or 180MPa, but not limited to the recited values, and other values not recited in the range of values are also applicable.
In the present invention, the temperature and pressure of hot isostatic pressing need to work synergistically. If the temperature and pressure are too high, the material is easy to melt and damage equipment; if the temperature and pressure are too low, the density of the product will be affected.
Preferably, the hot isostatic pressing in step (2) is performed at a pressure of 3-6 h, such as 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 heat is isostatic in the step (2).
Preferably, the tantalum target crude product is machined to obtain the high-purity tantalum target.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) placing a high-purity tantalum ingot with the purity not less than 4N in a hydrogenation furnace, vacuumizing, introducing hydrogen after vacuumizing, heating to 600-700 ℃, and stopping heating after the pressure in the hydrogenation furnace does not decrease any more to obtain a tantalum hydride source;
(2) crushing the tantalum hydride ingot obtained in the step (1) by using a roll-to-roll machine and a jet mill, wherein the lining material is tantalum with the purity not less than 4N, and screening out tantalum hydride powder with the granularity of 180-325 meshes;placing the screened tantalum hydride powder into a rubber sleeve for sealing, and carrying out cold isostatic pressing for 20-30 min under the condition of 160-190 MPa to obtain a cold-pressed blank; placing the cold-pressed blank into a stainless steel sheath for welding, degassing for 6-9 h at 400-600 ℃ until the pressure in the stainless steel sheath is 10-3～10-2Pa; and hot isostatic pressing for 3-6 h at 1000-1250 ℃ and 170-180 MPa, removing the stainless steel sleeve and machining to obtain the high-purity tantalum target material.
Compared with the prior art, the invention has the following beneficial effects:
according to the preparation method, tantalum hydride powder is adopted, and a cold isostatic pressing process and a hot isostatic pressing process are combined, so that the oxygen content of the obtained tantalum target material is effectively reduced, the compactness and the yield of the tantalum target material are improved, the oxygen content of the obtained tantalum target material is below 458ppm, the compactness is above 88.6%, and the yield is above 83.2%; and by further controlling the lining material in contact with the tantalum source in the powder preparation process, the oxygen content of the target material is further reduced, so that the oxygen content is below 350ppm, the density is above 98.3%, the yield is above 87.5%, and the method has a good industrial application prospect.
Detailed Description
In order to better illustrate the present invention and facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below. However, the following examples are only simple examples of the present invention and do not represent or limit the scope of the present invention, which is defined by the claims.
The following are typical but non-limiting examples of the invention:
example 1:
the embodiment provides a preparation method of a high-purity tantalum target material, which comprises the following steps:
(1) placing a high-purity tantalum ingot with the purity of 4N in a hydrogenation furnace, vacuumizing, introducing hydrogen after vacuumizing, heating to 600 ℃, and stopping heating after the pressure in the hydrogenation furnace is not reduced any more to obtain a tantalum hydride source;
(2) sequentially adopting lining materials as the tantalum hydride ingot obtained in the step (1)Crushing the tantalum with the purity of 4N by a double-roller crusher and a jet mill, and screening out tantalum hydride powder with the granularity of 180 meshes; placing the screened tantalum hydride powder into a rubber sleeve for sealing, and carrying out cold isostatic pressing for 30min under the condition of 160MPa to obtain a cold-pressed blank; placing the cold-pressed blank into a stainless steel sheath, welding, degassing at 400 deg.C for 9 hr until the pressure in the stainless steel sheath is 10-3Pa; and hot isostatic pressing for 6h at 1000 ℃ and 170MPa, removing the stainless steel ladle sleeve and machining to obtain the high-purity tantalum target material.
Example 2:
the embodiment provides a preparation method of a high-purity tantalum target material, which comprises the following steps:
(1) placing a high-purity tantalum ingot with the purity of 99.993% in a hydrogenation furnace, vacuumizing, introducing hydrogen after vacuumizing, heating to 700 ℃, and stopping heating after the pressure in the hydrogenation furnace does not decrease any more to obtain a tantalum hydride source;
(2) crushing the tantalum hydride ingot obtained in the step (1) by using a roll-pair machine and a jet mill, wherein the lining material is tantalum with the purity of 99.991%, and screening out tantalum hydride powder with the particle size of 325 meshes; placing the screened tantalum hydride powder into a rubber sleeve for sealing, and carrying out cold isostatic pressing for 20min under the condition of 190MPa to obtain a cold-pressed blank; placing the cold-pressed blank into a stainless steel sheath, welding, degassing at 600 deg.C for 6 hr until the pressure in the stainless steel sheath is 10-2Pa; and hot isostatic pressing for 3h at 1250 ℃ and 180MPa, removing the stainless steel ladle sleeve and machining to obtain the high-purity tantalum target material.
Example 3:
the embodiment provides a preparation method of a high-purity tantalum target material, which comprises the following steps:
(1) placing a high-purity tantalum ingot with the purity of 5N in a hydrogenation furnace, vacuumizing, introducing hydrogen after vacuumizing, heating to 650 ℃, and stopping heating after the pressure in the hydrogenation furnace is not reduced any more to obtain a tantalum hydride source;
(2) crushing the tantalum hydride ingot obtained in the step (1) by using a double-roller mill and a jet mill which are sequentially provided with inner lining materials of tantalum with the purity of 4N, and screeningTantalum hydride powder with the particle size of 270 meshes; placing the screened tantalum hydride powder into a rubber sleeve for sealing, and carrying out cold isostatic pressing for 25min under the condition of 170MPa to obtain a cold-pressed blank; welding the cold-pressed blank in a stainless steel sheath, degassing at 500 deg.C for 7 hr until the pressure in the stainless steel sheath is 2 × 10-3Pa; and hot isostatic pressing for 5h at 1100 ℃ and 175MPa, removing the stainless steel ladle sleeve, and machining to obtain the high-purity tantalum target material.
Example 4:
this example provides a method for preparing a high-purity tantalum target material, which is similar to the method of example 1 except that: and (3) in the step (2), the linings of the roll crusher and the jet mill are made of zirconia materials.
Example 5:
this example provides a method for preparing a high-purity tantalum target material, which is similar to the method of example 1 except that: and (3) carrying out cold isostatic pressing under the condition of 140MPa in the step (2).
Example 6:
this example provides a method for preparing a high-purity tantalum target material, which is similar to the method of example 2 except that: and (3) carrying out cold isostatic pressing under the condition of 210MPa in the step (2).
Example 7:
this example provides a method for preparing a high-purity tantalum target material, which is similar to the method of example 1 except that: the temperature of hot isostatic pressing in step (2) was 900 ℃.
Example 8:
this example provides a method for preparing a high-purity tantalum target material, which is similar to the method of example 2 except that: the temperature of hot isostatic pressing in step (2) was 1400 ℃.
Comparative example 1:
this comparative example provides a method of preparing a high purity tantalum target material, which is comparable to the method of example 1, except that: and (3) directly putting the screened tantalum hydride powder into a stainless steel sheath without carrying out cold isostatic pressing, putting high-temperature cotton into the stainless steel sheath to prevent powder pumping, and then carrying out degassing treatment.
100 tantalum targets were prepared by the preparation methods described in examples 1 to 8 and comparative example 1, and the average oxygen content, average density and yield were measured, and the results are shown in table 1.
TABLE 1
Embodiments 1-3 adopt the preparation method of the invention, make the oxygen content in the tantalum target material reach below 350ppm, the density reach above 98.3%, the yield reaches 87.5%; in the embodiment 4, the conventional lining material is adopted, so that a little impurity is introduced in the powder preparation process, and the yield is reduced; example 5 the cold isostatic pressing pressure is too low, resulting in a decrease in the density of the product; example 6 cold isostatic pressing with excessive pressure resulted in billet fracture during the manufacturing process; the hot isostatic pressing temperature in example 7 is too low, which affects the overall quality of the product; in example 8, the hot isostatic pressing temperature is too high, so that the compactness of the product is improved, but the oxygen content of the product is increased.
In contrast, in comparative example 1, cold isostatic pressing is not performed, so that high-temperature cotton needs to be added to prevent powder extraction in the degassing treatment process, so that more oxygen elements are introduced, the oxygen content of the product is increased, and the yield is reduced.
It can be seen from the above examples and comparative examples that the preparation method of the present invention adopts tantalum hydride powder, and combines the cold isostatic pressing process and the hot isostatic pressing process, thereby effectively reducing the oxygen content of the obtained tantalum target, improving the density and yield of the tantalum target, wherein the oxygen content of the obtained tantalum target is below 458ppm, the density is above 88.6%, and the yield is above 83.2%; and by further controlling the lining material in contact with the tantalum source in the powder preparation process, the oxygen content of the target material is further reduced, so that the oxygen content is below 350ppm, the density is above 98.3%, the yield is above 87.5%, and the method has a good industrial application prospect.
The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It will be apparent to those skilled in the art that any modifications to the present invention, equivalents thereof, additions of additional operations, selection of specific ways, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. The preparation method of the high-purity tantalum target material is characterized by comprising the following steps:
(1) placing the high-purity tantalum source in a hydrogenation furnace, vacuumizing, introducing hydrogen for heating after vacuumizing, and stopping heating after the pressure in the hydrogenation furnace is not reduced any more to obtain a tantalum hydride source;
(2) and (2) crushing the tantalum hydride source obtained in the step (1), and then sequentially carrying out cold isostatic pressing, degassing treatment and hot isostatic pressing to obtain the high-purity tantalum target material.
2. The method of claim 1, wherein said high purity tantalum source of step (1) comprises an ingot of tantalum.
3. The method of claim 1 or 2, wherein the purity of the high purity tantalum source of step (1) is not less than 4N.
4. The method according to any one of claims 1 to 3, wherein the heating temperature in the step (1) is 600 to 700 ℃.
5. The production method according to any one of claims 1 to 4, wherein the crushing in step (2) is carried out by using a twin-roll mill and an air-jet mill in this order;
preferably, the double-roller mill and the airflow crusher are both provided with inner liners;
preferably, the material of the lining is tantalum with purity not less than 4N.
6. The method according to any one of claims 1 to 5, wherein after the crushing in step (2), the tantalum hydride powder having a particle size of 180 to 325 mesh is screened.
7. The method according to any one of claims 1 to 6, wherein the cold isostatic pressing in step (2) is performed using a gum cover seal;
preferably, the pressure of the cold isostatic pressing in the step (2) is 160-190 MPa;
preferably, the time of the cold isostatic pressing in the step (2) is 20-30 min;
preferably, the cold isostatic pressing in step (2) is carried out to obtain a cold pressed blank.
8. The method for preparing a stainless steel alloy material according to any one of claims 1 to 7, wherein the cold-pressed blank is placed in a stainless steel sheath for welding before the degassing treatment in the step (2);
preferably, the temperature of the degassing treatment in the step (2) is 400-600 ℃;
preferably, the time of the degassing treatment in the step (2) is 6-9 h;
preferably, after the degassing treatment in the step (2), the pressure in the stainless steel jacket is 10-3～10-2Pa。
9. The method of any one of claims 1-8, wherein the hot isostatic pressing in step (2) is performed at a temperature of 1000 to 1250 ℃;
preferably, the hot isostatic pressing pressure in the step (2) is 170-180 MPa;
preferably, the hot isostatic pressing pressure in the step (2) is 3-6 h;
preferably, the tantalum target crude product is obtained after the heat is kept static in the step (2);
preferably, the tantalum target crude product is machined to obtain the high-purity tantalum target.
10. The method of any one of claims 1 to 9, comprising the steps of:
(1) placing a high-purity tantalum ingot with the purity not less than 4N in a hydrogenation furnace, vacuumizing, introducing hydrogen after vacuumizing, heating to 600-700 ℃, and stopping heating after the pressure in the hydrogenation furnace does not decrease any more to obtain a tantalum hydride source;
(2) crushing the tantalum hydride ingot obtained in the step (1) by using a roll-to-roll machine and a jet mill, wherein the lining material is tantalum with the purity not less than 4N, and screening out tantalum hydride powder with the granularity of 180-325 meshes; placing the screened tantalum hydride powder into a rubber sleeve for sealing, and carrying out cold isostatic pressing for 20-30 min under the condition of 160-190 MPa to obtain a cold-pressed blank; placing the cold-pressed blank into a stainless steel sheath for welding, degassing for 6-9 h at 400-600 ℃ until the pressure in the stainless steel sheath is 10-3～10- 2Pa; and hot isostatic pressing for 3-6 h at 1000-1250 ℃ and 170-180 MPa, removing the stainless steel sleeve and machining to obtain the high-purity tantalum target material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110548252.8A CN113235056A (en) | 2021-05-19 | 2021-05-19 | Preparation method of high-purity tantalum target material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110548252.8A CN113235056A (en) | 2021-05-19 | 2021-05-19 | Preparation method of high-purity tantalum target material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113235056A true CN113235056A (en) | 2021-08-10 |
Family
ID=77137966
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110548252.8A Pending CN113235056A (en) | 2021-05-19 | 2021-05-19 | Preparation method of high-purity tantalum target material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113235056A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113695732A (en) * | 2021-09-10 | 2021-11-26 | 宁波江丰电子材料股份有限公司 | Welding method of aluminum target material assembly |
| 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 |
| CN114481055A (en) * | 2022-01-28 | 2022-05-13 | 宁波江丰电子材料股份有限公司 | Sintering fixture and method for preparing tantalum target material through powder metallurgy |
| CN114875369A (en) * | 2022-05-12 | 2022-08-09 | 宁波江丰电子材料股份有限公司 | Low-oxygen tantalum target material and preparation method thereof |
| CN115584482A (en) * | 2022-10-27 | 2023-01-10 | 大连科利德光电子材料有限公司 | Purification method of tantalum source precursor |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103147050A (en) * | 2013-02-26 | 2013-06-12 | 昆山海普电子材料有限公司 | Production method of high-purity tantalum target material |
| CN110952064A (en) * | 2019-11-25 | 2020-04-03 | 宁波江丰电子材料股份有限公司 | Tantalum-silicon alloy sputtering target material and preparation method thereof |
| CN110983264A (en) * | 2019-12-23 | 2020-04-10 | 有研亿金新材料有限公司 | Preparation method of high-density fine-grain easily-formed W target |
| CN111945121A (en) * | 2020-08-06 | 2020-11-17 | 宁波江丰电子材料股份有限公司 | Tantalum-aluminum alloy sputtering target and preparation method thereof |
-
2021
- 2021-05-19 CN CN202110548252.8A patent/CN113235056A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103147050A (en) * | 2013-02-26 | 2013-06-12 | 昆山海普电子材料有限公司 | Production method of high-purity tantalum target material |
| CN110952064A (en) * | 2019-11-25 | 2020-04-03 | 宁波江丰电子材料股份有限公司 | Tantalum-silicon alloy sputtering target material and preparation method thereof |
| CN110983264A (en) * | 2019-12-23 | 2020-04-10 | 有研亿金新材料有限公司 | Preparation method of high-density fine-grain easily-formed W target |
| CN111945121A (en) * | 2020-08-06 | 2020-11-17 | 宁波江丰电子材料股份有限公司 | Tantalum-aluminum alloy sputtering target and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 杜海清等编: "《工业陶瓷》", 31 December 1989 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113695732A (en) * | 2021-09-10 | 2021-11-26 | 宁波江丰电子材料股份有限公司 | Welding method of aluminum target material assembly |
| 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 |
| CN114481055A (en) * | 2022-01-28 | 2022-05-13 | 宁波江丰电子材料股份有限公司 | Sintering fixture and method for preparing tantalum target material through powder metallurgy |
| CN114875369A (en) * | 2022-05-12 | 2022-08-09 | 宁波江丰电子材料股份有限公司 | Low-oxygen tantalum target material and preparation method thereof |
| CN114875369B (en) * | 2022-05-12 | 2023-09-08 | 宁波江丰电子材料股份有限公司 | Low-oxygen tantalum target material and preparation method thereof |
| CN115584482A (en) * | 2022-10-27 | 2023-01-10 | 大连科利德光电子材料有限公司 | Purification method of tantalum source precursor |
| CN115584482B (en) * | 2022-10-27 | 2023-04-11 | 大连科利德光电子材料有限公司 | Purification method of tantalum source precursor |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113235056A (en) | Preparation method of high-purity tantalum target material | |
| WO2021134972A1 (en) | Chromium-silicon alloy sputtering target material and preparation method therefor | |
| EP1066899B1 (en) | Method of making a sputtering target | |
| CN113981390A (en) | Preparation method of high-purity low-oxygen tantalum target material | |
| CN113073299B (en) | Preparation method of chromium-silicon alloy sputtering target material | |
| CN111230096A (en) | Alloy sputtering target material and preparation method and application thereof | |
| CN111778487A (en) | Chromium-aluminum alloy sputtering target material and preparation method thereof | |
| CN110539067A (en) | Diffusion welding method for high-purity copper target | |
| CN111945121A (en) | Tantalum-aluminum alloy sputtering target and preparation method thereof | |
| CN102366833A (en) | Production method of tungsten-titanium target blank | |
| JP2001342506A (en) | Method for production of powder material and method for producing target material | |
| TWI617680B (en) | Cu-Ga alloy sputtering target and manufacturing method thereof | |
| CN114875369B (en) | Low-oxygen tantalum target material and preparation method thereof | |
| CN114561628A (en) | Preparation method and application of high-purity tantalum by cyclic chemical vapor deposition | |
| CN110904364B (en) | Preparation method of aluminum alloy target material | |
| JP2757287B2 (en) | Manufacturing method of tungsten target | |
| CN114774865A (en) | Aluminum-scandium alloy target material and preparation method thereof | |
| CN112111719A (en) | Tungsten titanium silicon alloy sputtering target material and preparation method thereof | |
| US10050160B2 (en) | Cu—Ga target, method of producing same, light-absorbing layer formed from Cu—Ga based alloy film, and CIGS system solar cell having the light-absorbing layer | |
| CN110788318A (en) | Preparation method of high-density rare earth tungsten electrode | |
| CN114075651A (en) | Tantalum-silicon dioxide sputtering target material and preparation method thereof | |
| CN109385566B (en) | High-strength high-wear-resistance multi-principal-element alloy coating material for PVD (physical vapor deposition) and preparation method thereof | |
| CN111438356A (en) | Titanium-aluminum target material for physical vapor deposition and preparation method thereof | |
| CN115255367B (en) | Nickel-aluminum alloy sputtering target material and hot pressing preparation method thereof | |
| CN115261806B (en) | Nickel-aluminum alloy sputtering target material and hot isostatic pressing 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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210810 |
|
| RJ01 | Rejection of invention patent application after publication |