CN113337799A - Tubular target material and preparation method thereof - Google Patents
Tubular target material and preparation method thereof Download PDFInfo
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- CN113337799A CN113337799A CN202110612746.8A CN202110612746A CN113337799A CN 113337799 A CN113337799 A CN 113337799A CN 202110612746 A CN202110612746 A CN 202110612746A CN 113337799 A CN113337799 A CN 113337799A
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- stainless steel
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- pipe
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- 239000013077 target material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000010935 stainless steel Substances 0.000 claims abstract description 128
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 128
- 239000000843 powder Substances 0.000 claims abstract description 34
- 238000007872 degassing Methods 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000003466 welding Methods 0.000 claims abstract description 29
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 28
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 19
- 239000000956 alloy Substances 0.000 claims abstract description 19
- 238000011049 filling Methods 0.000 claims abstract description 12
- 238000005488 sandblasting Methods 0.000 claims abstract description 9
- 238000003754 machining Methods 0.000 claims abstract description 6
- 229910000676 Si alloy Inorganic materials 0.000 claims description 23
- DYRBFMPPJATHRF-UHFFFAOYSA-N chromium silicon Chemical compound [Si].[Cr] DYRBFMPPJATHRF-UHFFFAOYSA-N 0.000 claims description 23
- 238000004519 manufacturing process Methods 0.000 claims description 17
- 239000012298 atmosphere Substances 0.000 claims description 8
- 230000001681 protective effect Effects 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910001182 Mo alloy Inorganic materials 0.000 claims description 4
- VNTLIPZTSJSULJ-UHFFFAOYSA-N chromium molybdenum Chemical compound [Cr].[Mo] VNTLIPZTSJSULJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910000990 Ni alloy Inorganic materials 0.000 claims description 2
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 12
- 239000001301 oxygen Substances 0.000 abstract description 12
- 229910052760 oxygen Inorganic materials 0.000 abstract description 12
- 238000007751 thermal spraying Methods 0.000 description 7
- 239000011651 chromium Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000012300 argon atmosphere Substances 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 238000005477 sputtering target Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000008520 organization Effects 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- 229910019819 Cr—Si Inorganic materials 0.000 description 2
- 238000005219 brazing Methods 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910000967 As alloy Inorganic materials 0.000 description 1
- 241000357293 Leptobrama muelleri Species 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000005429 filling process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 238000009849 vacuum degassing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 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
- B22F3/12—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
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
- B22F7/08—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools with one or more parts not made from powder
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/06—Alloys based on chromium
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Composite Materials (AREA)
- Powder Metallurgy (AREA)
- Physical Vapour Deposition (AREA)
- Pressure Welding/Diffusion-Bonding (AREA)
Abstract
The invention provides a tubular target material and a preparation method thereof, wherein the preparation method comprises the following steps: preparing a stainless steel inner pipe and a stainless steel outer pipe, performing thread machining on the outer surface of the stainless steel inner pipe, and performing sand blasting on the inner surface of the stainless steel outer pipe; coaxially welding the obtained processed stainless steel inner pipe and the processed stainless steel outer pipe on a first stainless steel cover plate to form an annular cavity; filling the mixed alloy powder into the annular cavity for tamping, welding a second stainless steel cover plate at the other ends of the stainless steel inner tube and the stainless steel outer tube, and sequentially performing degassing treatment and hot isostatic pressing treatment to obtain a tubular target material; the preparation method adopts a hot isostatic pressing integrated forming method, improves the inner tube and the outer tube of the stainless steel, effectively improves the density and the uniformity of the tubular target material, reduces the oxygen content of the tubular target material, improves the yield of the tubular target material, and has better industrial application prospect.
Description
Technical Field
The invention belongs to the technical field of target preparation, and particularly relates to a tubular target and a preparation method thereof.
Background
The chromium-silicon alloy sputtering target is a novel sputtering target and can be widely applied to the fields of electronics, military use, decoration, functional films and the like. At present, most of chromium-silicon alloy targets are planar targets. Because the magnetic fields in the planar target and the sputtering equipment do not move relatively, the utilization rate of the planar target is only about 30 percent, which not only causes the waste of target materials, but also causes great influence on the production process because the work of the sputtering equipment must be interrupted when the target is replaced.
In order to increase the utilization of the target, tubular targets (tube targets for short) are increasingly being manufactured and used, i.e. the target is shaped as a tube, which is provided with stationary magnets. During sputtering, the tube target rotates at a certain speed and is therefore also called a rotating target. Because the relative motion occurs between the rotating tube target and the static magnet, the sputtering occurs uniformly on the whole tube target surface, and the utilization rate of the target material can reach more than 70%.
Currently known methods for producing chromium silicon alloy tube targets are thermal spraying, brazing, casting and hot isostatic pressing. The thermal spraying is to spray the metal powder to the workpiece by adopting a plasma thermal spraying mode, and the tube target prepared by the method has low density, extremely uneven structure, a large number of holes and high oxygen content, and can only be used in the coating industry with low requirements such as glass and the like; the brazing method is to weld the target tube to the liner tube by using a solder, and the solder is difficult to be uniformly distributed due to the small gap between the target tube and the liner tube, so that the overall welding of the target tube with the length of more than 1000mm is difficult to realize; the casting method is to directly cast the target material on the liner tube, but only used for the target material with lower melting point such as Sn, Zn and the like; the tube target prepared by the hot isostatic pressing integral forming method has uniform components, no segregation, fine grains and high purity, but the problems of mismatch of thermal expansion coefficients between the chromium-silicon alloy and the liner tube, hard and brittle metal characteristics of the chromium-silicon alloy and the like easily cause stress concentration to generate cracks, and the yield is reduced.
CN103774101A discloses a thermal spraying tube target with ultra-low oxygen content and a preparation method thereof, the method is to place thermal spraying equipment and a spraying matrix in an argon protective atmosphere, spray metal powder to a workpiece by adopting a plasma thermal spraying mode, and then mechanically process the sprayed workpiece, thus obtaining the thermal spraying tube target.
CN111058004A discloses a chromium-silicon alloy sputtering target material and a preparation method thereof, the method comprises the steps of loading chromium-silicon alloy powder into a mould, degassing, carrying out vacuum degassing under a heating state, sealing and welding, and then carrying out hot isostatic pressing, machining and other procedures to obtain the chromium-silicon alloy plane sputtering target material with high density, uniform microstructure and low oxygen content.
In summary, how to provide a method for improving the utilization rate of a target material, reducing the oxygen content of the target material, and solving the problem of mismatch between the thermal expansion coefficients of the chromium-silicon alloy and the liner tube, and improving the yield is a problem to be solved at present.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a tubular target and a preparation method thereof, wherein the preparation method adopts a hot isostatic pressing integrated forming method, and improves a stainless steel inner tube and an outer tube, so that the density and the uniformity of the tubular target are effectively improved, the oxygen content of the tubular target is reduced, and the yield of the tubular target is improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
in one aspect, the invention provides a preparation method of a tubular target, which comprises the following steps:
(1) preparing a stainless steel inner pipe and a stainless steel outer pipe, performing thread machining on the outer surface of the stainless steel inner pipe, and performing sand blasting on the inner surface of the stainless steel outer pipe;
(2) coaxially welding the processed stainless steel inner pipe and the processed stainless steel outer pipe obtained in the step (1) on a first stainless steel cover plate to form an annular cavity;
(3) and filling the mixed alloy powder into the annular cavity for tamping, welding a second stainless steel cover plate at the other ends of the stainless steel inner tube and the stainless steel outer tube, and sequentially performing degassing treatment and hot isostatic pressing treatment to obtain the tubular target.
In the invention, the preparation method adopts a hot isostatic pressing integrated forming method, so that the density of the target material and the uniformity of an internal organization structure can be effectively improved, and the oxygen content is reduced; in addition, the stress generated due to the mismatching of the thermal expansion coefficients of the alloy and the stainless steel inner tube can be released by processing the outer surface of the stainless steel inner tube through the screw threads, the risk of cracking caused by cracks generated due to stress concentration is reduced, the welding bonding rate between the stainless steel inner tube and the target material is improved, the thickness and the yield of the tubular target material are effectively ensured, and the industrial application is facilitated.
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.
In a preferred embodiment of the present invention, the thread width after the threading in step (1) is 0.5 to 2mm, for example, 0.5mm, 0.8mm, 1.0mm, 1.2mm, 1.5mm, 1.8mm, or 2mm, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the thread depth after the thread cutting in the step (1) is 0.25 to 1mm, 0.25mm, 0.3mm, 0.4mm, 0.5mm, 0.6mm, 0.7mm, 0.8mm, 0.9mm, 1mm, or the like, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
In the present invention, the width and depth of the thread must be controlled. If the thread is too wide and too deep, the dressing amount is increased, the wall thickness of the stainless steel inner pipe is increased, and the cost is increased; if the thread is too narrow and shallow, the effect of releasing all stress is not achieved, and fine diffusion cracks still occur.
As a preferable technical scheme of the invention, the stainless steel inner pipe and the stainless steel outer pipe processed in the step (2) are cleaned and dried before being welded.
As a preferred embodiment of the present invention, the thickness of the annular cavity in step (2) is 2 to 3 times, for example, 2 times, 2.2 times, 2.4 times, 2.6 times, 2.8 times or 3 times, of the thickness of the tubular target, but the invention is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
In the invention, after hot isostatic pressing treatment, alloy can be obtained from alloy powder, the density is increased from original 45-50% to not less than 99%, the whole sheath can shrink, and meanwhile, enough allowance is left for subsequent mechanical processing, so that the size of the powder-loading cavity is designed to be 2-3 times of that of a finished target.
In a preferred embodiment of the present invention, the alloy powder in step (3) includes one of a chromium-silicon alloy powder, a chromium-molybdenum alloy powder, and a chromium-nickel alloy powder.
Preferably, the chromium silicon alloy powder has a Si content of 30 to 70 wt%, such as 30 wt%, 35 wt%, 40 wt%, 45 wt%, 50 wt%, 55 wt%, 60 wt%, 65 wt% or 70 wt%, but not limited to the recited values, and other non-recited values within this range are equally applicable, preferably 40 to 50 wt%.
In the present invention, the total content of silicon and chromium is 100 wt%.
As a preferable embodiment of the present invention, the alloy powder in the step (3) is mixed in a protective atmosphere.
Preferably, the protective atmosphere comprises argon and/or nitrogen.
In the present invention, mixing in a protective atmosphere can reduce oxidation of the powder.
As a preferable technical scheme of the invention, the second stainless steel cover plate in the step (3) is provided with a degassing hole.
Preferably, the degassing treatment in step (3) is performed at a temperature of 400 to 700 ℃, for example, 400 ℃, 450 ℃, 500 ℃, 550 ℃, 600 ℃, or 700 ℃, 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 (3) is carried out for 6-9 h, 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 range of the values are also applicable.
Preferably, the pressure after the degassing treatment in the step (3) is 10-3～10-2Pa, e.g. 10-3、2×10-3、4×10-3、6×10-3、7×10-3Or 10-2And the like, but are not limited to the recited values, and other values not recited within the numerical range are also applicable.
In the present invention, the degassing treatment has a significant effect on the oxygen content in the final finished target. The higher the treatment temperature and the longer the treatment time, the higher the vacuum after treatment and the lower the oxygen content in the final product.
In a preferred embodiment of the present invention, the hot isostatic pressing treatment in step (3) is carried out at a temperature of 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 pressure of the hot isostatic pressing treatment in step (3) is 120 to 170MPa, such as 120MPa, 130MPa, 140MPa, 150MPa, 160MPa or 170MPa, but not limited to the recited values, and other values not recited in the range of the recited values are also applicable.
In the present invention, the temperature and pressure of the hot isostatic pressing treatment need to be controlled to some extent.
Preferably, the hot isostatic pressing treatment in step (3) is performed for 3 to 6 hours, such as 3 hours, 4 hours, 5 hours, or 6 hours, but not limited to the recited values, and other values in the range are also applicable.
Preferably, the tubular target is obtained by machining after the hot isostatic pressing treatment in the step (3).
In the invention, the stainless steel outer pipe and the two stainless steel cover plates are removed from the workpiece after the hot isostatic pressing treatment to obtain a blank material with the inner stainless steel and the outer stainless steel as alloy targets, and then the blank material is machined according to requirements to obtain the final tubular target.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) preparing a stainless steel inner pipe and a stainless steel outer pipe, and carrying out thread turning on the outer surface of the stainless steel inner pipe, wherein the width of a thread is 0.5-2 mm, and the depth of the thread is 0.25-1 mm; carrying out sand blasting treatment on the inner surface of the stainless steel outer pipe, and cleaning and drying the processed stainless steel inner pipe and the processed stainless steel outer pipe;
(2) coaxially welding the stainless steel inner tube and the stainless steel outer tube dried in the step (1) on a first stainless steel cover plate to form an annular cavity, wherein the thickness of the annular cavity is 2-3 times of that of the tubular target;
(3) filling alloy powder mixed in a protective atmosphere into the annular cavity for tamping treatment, welding a second stainless steel cover plate with degassing holes at the other ends of the stainless steel inner pipe and the stainless steel outer pipe, degassing for 6-9 h at 400-700 ℃, wherein the pressure after degassing is 10-3～10-2Pa; and hot isostatic pressing for 3-6 h at 1000-1250 ℃ and 120-170 MPa to obtain the tubular target.
In another aspect, the present invention provides a tubular target prepared by the above preparation method, wherein the thickness of the tubular target is 3-20 mm, such as 3mm, 4mm, 5mm, 6mm, 7mm, 8mm, 9mm, 10mm, 12mm, 14mm, 16mm, 18mm, 19mm or 20mm, but not limited to the recited values, and other values in the range of the recited values are also applicable.
Compared with the prior art, the invention has the following beneficial effects:
(1) the preparation method adopts a hot isostatic pressing integrated forming method, and carries out thread turning on the outer surface of the stainless steel inner tube, thereby effectively improving the density of the target material and the uniformity of an internal organization structure, reducing the oxygen content, solving the problem of crack generation caused by stress concentration due to mismatching of thermal expansion coefficients between the alloy and the stainless steel inner tube, and further controlling the width and the depth of the thread, so that the welding bonding rate between the stainless steel inner tube and the target material reaches more than 99.90 percent, the welding bonding strength reaches more than 75MPa, the highest can reach 100MPa, and the yield reaches more than 98 percent;
(2) the preparation process disclosed by the invention is simple in flow, low in cost and good in 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 tubular target material and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) preparing a stainless steel inner pipe and a stainless steel outer pipe, and carrying out thread turning on the outer surface of the stainless steel inner pipe, wherein the width of a thread is 0.5mm, and the depth of the thread is 0.25 mm; carrying out sand blasting treatment on the inner surface of the stainless steel outer pipe, and cleaning and drying the processed stainless steel inner pipe and the processed stainless steel outer pipe;
(2) coaxially welding the stainless steel inner pipe and the stainless steel outer pipe dried in the step (1) on a first stainless steel cover plate to form an annular cavity, wherein the thickness of the annular cavity is 9 mm;
(3) filling chromium-silicon alloy powder mixed in an argon atmosphere into the annular cavity for tamping treatment, wherein the content of Si in the chromium-silicon alloy powder is 30 wt%, and the content of Cr in the chromium-silicon alloy powder is 70 wt%; then welding a second stainless steel cover plate with degassing holes on the other ends of the stainless steel inner pipe and the stainless steel outer pipe, degassing at 400 deg.C for 6h, and degassing at 10 deg.C-2Pa; hot isostatic pressing for 3h at 1250 ℃ and 170MPa to obtain the Cr-Si alloy tube with the thickness of 3mmA target material.
Example 2:
the embodiment provides a tubular target material and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) preparing a stainless steel inner pipe and a stainless steel outer pipe, and carrying out thread turning on the outer surface of the stainless steel inner pipe, wherein the width of a thread is 2mm, and the depth of the thread is 1 mm; carrying out sand blasting treatment on the inner surface of the stainless steel outer pipe, and cleaning and drying the processed stainless steel inner pipe and the processed stainless steel outer pipe;
(2) coaxially welding the stainless steel inner pipe and the stainless steel outer pipe dried in the step (1) on a first stainless steel cover plate to form an annular cavity, wherein the thickness of the annular cavity is 40 mm;
(3) filling chromium-silicon alloy powder mixed in an argon atmosphere into the annular cavity for tamping treatment, wherein the content of Si in the chromium-silicon alloy powder is 70 wt%, and the content of Cr in the chromium-silicon alloy powder is 30 wt%; then welding a second stainless steel cover plate with degassing holes on the other ends of the stainless steel inner pipe and the stainless steel outer pipe, degassing at 600 deg.C for 9h, and degassing at 10 deg.C-3Pa; hot isostatic pressing is carried out for 6 hours at the temperature of 1000 ℃ and under the pressure of 120MPa, and the chromium-silicon alloy tubular target with the thickness of 20mm is obtained.
Example 3:
the embodiment provides a tubular target material and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) preparing a stainless steel inner pipe and a stainless steel outer pipe, and carrying out thread turning on the outer surface of the stainless steel inner pipe, wherein the width of a thread is 1mm, and the depth of the thread is 0.5 mm; carrying out sand blasting treatment on the inner surface of the stainless steel outer pipe, and cleaning and drying the processed stainless steel inner pipe and the processed stainless steel outer pipe;
(2) coaxially welding the stainless steel inner pipe and the stainless steel outer pipe dried in the step (1) on a first stainless steel cover plate to form an annular cavity, wherein the thickness of the annular cavity is 8 mm;
(3) filling chromium-silicon alloy powder mixed in argon atmosphere into the annular cavity for tamping treatment, wherein S in the chromium-silicon alloy powderThe content of i is 50 wt%, and the content of Cr is 50 wt%; then welding a second stainless steel cover plate with degassing holes on the other ends of the stainless steel inner tube and the stainless steel outer tube, degassing at 500 deg.C for 8 hr, and degassing at 2 × 10-3Pa; hot isostatic pressing for 4h at 1100 ℃ and 150MPa to obtain the Cr-Si alloy tubular target with the thickness of 5 mm.
Example 4:
the embodiment provides a tubular target material and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) preparing a stainless steel inner pipe and a stainless steel outer pipe, and carrying out thread turning on the outer surface of the stainless steel inner pipe, wherein the width of a thread is 1.5mm, and the depth of the thread is 0.8 mm; carrying out sand blasting treatment on the inner surface of the stainless steel outer pipe, and cleaning and drying the processed stainless steel inner pipe and the processed stainless steel outer pipe;
(2) coaxially welding the stainless steel inner pipe and the stainless steel outer pipe dried in the step (1) on a first stainless steel cover plate to form an annular cavity, wherein the thickness of the annular cavity is 15 mm;
(3) filling chromium-molybdenum alloy powder mixed in an argon atmosphere into the annular cavity for tamping treatment, wherein the chromium content in the chromium-silicon alloy powder is 60 wt%, and the molybdenum content is 40 wt%; then welding a second stainless steel cover plate with degassing holes on the other ends of the stainless steel inner tube and the stainless steel outer tube, degassing at 450 deg.C for 7h, and degassing at 5 × 10-3Pa; hot isostatic pressing for 5h at 1200 ℃ and 140MPa to obtain the chromium-molybdenum alloy tubular target with the thickness of 10 mm.
Example 5:
the present embodiment provides a tubular target material and a method for manufacturing the same, which is different from the method for manufacturing in embodiment 3 only in that: degassing at 700 deg.C for 9 hr in step (3) under 2 × 10-3Pa。
Example 6:
the present embodiment provides a tubular target material and a method for manufacturing the same, which is different from the method in embodiment 1 only in that: the width of the thread in the step (1) is 0.2 mm.
Example 7:
the present embodiment provides a tubular target material and a method for manufacturing the same, which is different from the method for manufacturing in embodiment 2 only in that: the width of the thread in the step (1) is 2.5 mm.
Example 8:
the present embodiment provides a tubular target material and a method for manufacturing the same, which is different from the method in embodiment 1 only in that: the depth of the thread in the step (1) is 0.1 mm.
Example 9:
the present embodiment provides a tubular target material and a method for manufacturing the same, which is different from the method for manufacturing in embodiment 2 only in that: the depth of the thread in the step (1) is 1.2 mm.
Comparative example 1:
this comparative example provides a tubular target material and a method for producing the same, which is comparable to the production method in example 1 except that: and (2) in the step (1), the stainless steel inner pipe is not subjected to thread turning.
100 pieces of tubular targets were prepared by the preparation methods described in examples 1 to 9 and comparative example 1, respectively, and the average weld bonding rate, average weld bonding strength, average oxygen content, and yield were measured, and the measurement results are shown in table 1.
TABLE 1
In examples 1 to 5, the preparation method of the present invention was adopted, and the width and depth of the thread were further controlled, so that the average weld bonding rate of the obtained tubular target material was more than 99.90%, the average weld bonding strength was more than 75MPa, and the yield was more than 98%; in example 6, the width of the thread is reduced, so that stress caused by mismatch of thermal expansion coefficients cannot be completely released, penetrating cracks occur on the surface of the target, and the yield is reduced; in example 7, the width of the thread is increased, and although the requirement of stress release is met, more mixed powder is added for filling during powder filling, so that waste of materials is caused, and the cost is increased; in the embodiment 8, the depth of the thread is reduced, so that the diffusion layer of the alloy target and the stainless steel back tube is reduced, the welding bonding rate is reduced, the welding bonding strength is reduced, and the risk of target use desoldering is increased; in example 9, the depth of the screw thread is deepened, so that the wall thickness of the back tube is increased, and more alloy powder is added for filling in the powder filling process, thereby increasing the preparation cost.
In the comparative example 1, the stainless steel inner tube is not threaded, so that the difference of the thermal expansion coefficients between the alloy tube target and the stainless steel inner tube is large, the welding bonding rate and the welding bonding strength are reduced, the obtained tube target is easy to crack, and the yield is only 10%.
It can be seen from the above examples and comparative examples that the preparation method of the present invention adopts the hot isostatic pressing integrated forming method, and performs thread turning on the outer surface of the stainless steel inner tube, thereby effectively improving the density of the target material and the uniformity of the internal organization structure, reducing the oxygen content, solving the problem of crack generation caused by stress concentration due to mismatch of thermal expansion coefficients between the alloy and the stainless steel inner tube, and further controlling the width and depth of the thread, so that the welding bonding rate between the stainless steel inner tube and the target material reaches more than 99.90%, the welding bonding strength reaches more than 75MPa, the highest 100MPa, and the yield reaches more than 98%; the preparation process is simple in flow, low in cost and good in 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 tubular target material is characterized by comprising the following steps:
(1) preparing a stainless steel inner pipe and a stainless steel outer pipe, performing thread machining on the outer surface of the stainless steel inner pipe, and performing sand blasting on the inner surface of the stainless steel outer pipe;
(2) coaxially welding the processed stainless steel inner pipe and the processed stainless steel outer pipe obtained in the step (1) on a first stainless steel cover plate to form an annular cavity;
(3) and filling the mixed alloy powder into the annular cavity for tamping, welding a second stainless steel cover plate at the other ends of the stainless steel inner tube and the stainless steel outer tube, and sequentially performing degassing treatment and hot isostatic pressing treatment to obtain the tubular target.
2. The manufacturing method according to claim 1, wherein the thread width after the thread cutting in the step (1) is 0.5 to 2 mm;
preferably, the thread depth after the thread turning in the step (1) is 0.25-1 mm.
3. The manufacturing method according to claim 1 or 2, wherein the processed stainless steel inner pipe and the processed stainless steel outer pipe in the step (2) are cleaned and dried before being welded.
4. The method according to any one of claims 1 to 3, wherein the thickness of the annular cavity in the step (2) is 2 to 3 times the thickness of the tubular target.
5. The production method according to any one of claims 1 to 4, wherein the alloy powder in the step (3) comprises any one of a chromium-silicon alloy powder, a chromium-molybdenum alloy powder or a chromium-nickel alloy powder;
preferably, the content of Si in the chromium-silicon alloy powder is 30-70 wt%, preferably 40-50 wt%.
6. The production method according to any one of claims 1 to 5, wherein the alloy powder of step (3) is mixed in a protective atmosphere;
preferably, the protective atmosphere comprises argon and/or nitrogen.
7. The manufacturing method according to any one of claims 1 to 6, wherein the second stainless steel cover plate of step (3) is provided with a degassing hole;
preferably, the temperature of the degassing treatment in the step (3) is 400-700 ℃;
preferably, the time of the degassing treatment in the step (3) is 6-9 h;
preferably, the pressure after the degassing treatment in the step (3) is 10-3～10-2Pa。
8. The production method according to any one of claims 1 to 7, wherein the hot isostatic pressing treatment in step (3) is performed at a temperature of 1000 to 1250 ℃;
preferably, the pressure of the hot isostatic pressing treatment in the step (3) is 120-170 MPa;
preferably, the hot isostatic pressing treatment in the step (3) is carried out for 3-6 h;
preferably, the tubular target is obtained by machining after the hot isostatic pressing treatment in the step (3).
9. The method of any one of claims 1 to 8, comprising the steps of:
(1) preparing a stainless steel inner pipe and a stainless steel outer pipe, and carrying out thread turning on the outer surface of the stainless steel inner pipe, wherein the width of a thread is 0.5-2 mm, and the depth of the thread is 0.25-1 mm; carrying out sand blasting treatment on the inner surface of the stainless steel outer pipe, and cleaning and drying the processed stainless steel inner pipe and the processed stainless steel outer pipe;
(2) coaxially welding the stainless steel inner tube and the stainless steel outer tube dried in the step (1) on a first stainless steel cover plate to form an annular cavity, wherein the thickness of the annular cavity is 2-3 times of that of the tubular target;
(3) filling alloy powder mixed in a protective atmosphere into the annular cavity for tamping treatment, welding a second stainless steel cover plate with degassing holes at the other ends of the stainless steel inner pipe and the stainless steel outer pipe, degassing for 6-9 h at 400-700 ℃, wherein the pressure after degassing is 10-3～10-2Pa; and hot isostatic pressing for 3-6 h at 1000-1250 ℃ and 120-170 MPa to obtain the tubular target.
10. The tubular target prepared by the preparation method according to any one of claims 1 to 9, wherein the thickness of the tubular target is 3 to 20 mm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114043065A (en) * | 2021-11-25 | 2022-02-15 | 宁波江丰电子材料股份有限公司 | Hot isostatic pressing diffusion welding method for aluminum rotary target |
| CN114086130A (en) * | 2021-11-16 | 2022-02-25 | 宁波江丰电子材料股份有限公司 | Preparation method of tungsten-titanium alloy tube target |
| CN116213703A (en) * | 2023-03-15 | 2023-06-06 | 先导薄膜材料有限公司 | Preparation method of chromium rotary target |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1985345A (en) * | 2004-07-16 | 2007-06-20 | 贝卡尔特先进涂层公司 | Cylindrical target obtained by hot isostatic pressing |
| CN102806353A (en) * | 2012-08-17 | 2012-12-05 | 苏州晶纯新材料有限公司 | Production method of molybdenum alloy tube target |
| CN103397301A (en) * | 2013-07-17 | 2013-11-20 | 中国南玻集团股份有限公司 | Cylinder rotating silver target and preparation method thereof |
| CN105817627A (en) * | 2016-03-28 | 2016-08-03 | 航天材料及工艺研究所 | Preparation method for integrally-formed tungsten tube target material with large length-to-diameter ratio |
| CN112743075A (en) * | 2020-12-29 | 2021-05-04 | 宁波江丰电子材料股份有限公司 | Binding method of tubular target |
-
2021
- 2021-06-02 CN CN202110612746.8A patent/CN113337799A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1985345A (en) * | 2004-07-16 | 2007-06-20 | 贝卡尔特先进涂层公司 | Cylindrical target obtained by hot isostatic pressing |
| CN102806353A (en) * | 2012-08-17 | 2012-12-05 | 苏州晶纯新材料有限公司 | Production method of molybdenum alloy tube target |
| CN103397301A (en) * | 2013-07-17 | 2013-11-20 | 中国南玻集团股份有限公司 | Cylinder rotating silver target and preparation method thereof |
| CN105817627A (en) * | 2016-03-28 | 2016-08-03 | 航天材料及工艺研究所 | Preparation method for integrally-formed tungsten tube target material with large length-to-diameter ratio |
| CN112743075A (en) * | 2020-12-29 | 2021-05-04 | 宁波江丰电子材料股份有限公司 | Binding method of tubular target |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114086130A (en) * | 2021-11-16 | 2022-02-25 | 宁波江丰电子材料股份有限公司 | Preparation method of tungsten-titanium alloy tube target |
| CN114043065A (en) * | 2021-11-25 | 2022-02-15 | 宁波江丰电子材料股份有限公司 | Hot isostatic pressing diffusion welding method for aluminum rotary target |
| CN114043065B (en) * | 2021-11-25 | 2023-01-13 | 宁波江丰电子材料股份有限公司 | Hot isostatic pressing diffusion welding method for aluminum rotary target |
| CN116213703A (en) * | 2023-03-15 | 2023-06-06 | 先导薄膜材料有限公司 | Preparation method of chromium rotary target |
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