CN116200639A - CrW alloy target and preparation method thereof - Google Patents
CrW alloy target and preparation method thereof Download PDFInfo
- Publication number
- CN116200639A CN116200639A CN202211734636.XA CN202211734636A CN116200639A CN 116200639 A CN116200639 A CN 116200639A CN 202211734636 A CN202211734636 A CN 202211734636A CN 116200639 A CN116200639 A CN 116200639A
- Authority
- CN
- China
- Prior art keywords
- target
- powder
- treatment
- alloy
- sheath
- 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
- 239000000956 alloy Substances 0.000 title claims abstract description 63
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 32
- 238000003466 welding Methods 0.000 claims abstract description 28
- 239000013077 target material Substances 0.000 claims abstract description 27
- 238000001513 hot isostatic pressing Methods 0.000 claims description 24
- 238000009792 diffusion process Methods 0.000 claims description 20
- 238000007872 degassing Methods 0.000 claims description 18
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 9
- 238000005488 sandblasting Methods 0.000 claims description 9
- 238000005520 cutting process Methods 0.000 claims description 7
- 238000009713 electroplating Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- 238000007747 plating Methods 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 7
- 238000011049 filling Methods 0.000 claims description 6
- 229910052804 chromium Inorganic materials 0.000 claims description 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 239000011812 mixed powder Substances 0.000 claims description 3
- 238000005422 blasting Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 10
- 238000005054 agglomeration Methods 0.000 abstract description 4
- 230000002776 aggregation Effects 0.000 abstract description 4
- 238000005204 segregation Methods 0.000 abstract description 3
- 239000011651 chromium Substances 0.000 description 36
- 230000000052 comparative effect Effects 0.000 description 25
- 239000010949 copper Substances 0.000 description 6
- 238000003754 machining Methods 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 5
- 229910016525 CuMo Inorganic materials 0.000 description 4
- 238000000713 high-energy ball milling Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 229910001080 W alloy Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000013475 authorization Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- QNHZQZQTTIYAQM-UHFFFAOYSA-N chromium tungsten Chemical compound [Cr][W] QNHZQZQTTIYAQM-UHFFFAOYSA-N 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
-
- 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
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/02—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating by means of a press ; Diffusion bonding
- B23K20/021—Isostatic pressure welding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/02—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating by means of a press ; Diffusion bonding
- B23K20/023—Thermo-compression bonding
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/10—Nuclear fusion reactors
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physical Vapour Deposition (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a CrW alloy target and a preparation method thereof, in particular to a CrW alloy target with the W atomic ratio up to 50% is prepared by optimizing the powder granularity and the forming process. The CrW alloy target material has uniform structure, no segregation, no agglomeration and the like, and the compactness is more than 99 percent. In addition, the invention also solves the difficult problems that the target is brittle, hard and difficult to process into the target with complex shape by welding a layer of material easy to machine at the bottom of the target, so that the target is widely applied.
Description
Technical Field
The invention belongs to the technical field of hard coatings, and particularly relates to a CrW alloy target and a preparation method thereof.
Background
The application field of CrW targets is more and more extensive, the existing target preparation processes mainly comprise two processes, one process is that the targets are prepared by hot-pressing sintering, and alloying reaction is carried out on chromium and tungsten under high temperature and high pressure for a long time, so that the prepared targets are hard and brittle, and are not beneficial to subsequent machining; and the other is to prepare prealloy powder by high-energy ball milling and prepare a target material by degassing and hot isostatic pressing treatment, so that the process is complicated, the high-energy ball milling cost is high, and the industrial production is not facilitated.
In addition, the CrW target material is harder and more brittle along with the increase of the W element proportion, the shape of a processed product is limited, and the machining difficulty and the cost are greatly increased. At present, the proportion of W element of the CrW target material prepared by hot pressing and high-energy ball milling process is generally less than 20% by atomic ratio, such as the chromium-tungsten alloy target material obtained by the invention patent with the authorization number of CN105345007B, wherein the atomic percentage of chromium is 80-99% and tungsten is 1-20%. However, a CrW target of 20% atomic ratio W element has not been able to meet the needs of a wide range of applications.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a CrW alloy target and a preparation method thereof. The invention prepares the CrW alloy target material with the W atomic ratio up to 50% by optimizing the powder granularity and the forming process.
In order to achieve the above purpose, the invention provides a preparation method of a CrW alloy target, which specifically comprises the following steps:
s1, uniformly mixing Cr powder and W powder according to a given proportion, wherein the atomic proportion of W element in the given proportion is 5-50%, and the granularity of Cr powder is less than 30 mu m;
s2, filling the mixed powder into a sheath die for degassing treatment;
s3, performing hot isostatic pressing forming on the degassed sheath;
s4, removing the sheath from the blank subjected to the hot isostatic pressing, cutting the blank into target pieces with corresponding sizes, and grinding two end surfaces of the target pieces;
s5, carrying out sand blasting on two end faces of the target piece after grinding;
s6, electroplating the two end surfaces of the target piece subjected to sand blasting;
s7, stacking the target piece subjected to the electroplating treatment and an alloy backboard with the same size together, and filling the target piece and the alloy backboard into a sheath die for degassing treatment;
s8, performing diffusion welding treatment on the degassed sheath;
s9, removing the sheath from the target piece subjected to diffusion welding treatment, and then processing the target piece to a target material with a required shape to obtain the CrW alloy target material with the backboard.
According to the technical scheme, a simple three-dimensional mixer is adopted for mixing during mixing, the process is simple, the operation is easy, the use of complex high-energy ball milling equipment is avoided, the mixing process is complicated, and the cost is relatively high; and the granularity of Cr powder is controlled to be smaller than 30 mu m during mixing, so that the granularity of Cr powder is smaller when Cr powder and W powder are mixed, the granularity of Cr powder is closer to the granularity of W powder, the W element is uniformly dispersed in a Cr matrix, the phenomenon that high-content W is not uniformly dispersed in the Cr matrix and is not easily and locally agglomerated and not easily densified is avoided, the W atomic ratio can reach 50%, and the target compactness is good. Through carrying out the electroplating of two sides to the both ends face of target, that is the positive and negative of target for the workman need not distinguish two sides when operating, can put by arbitrary face, prevents makeing mistakes. Finally, a layer of material easy to machine is welded at the bottom of the target, so that the difficult problem that the target is brittle, hard and difficult to machine to a target with a complex shape is solved, and the target is widely applied. And the back plate is connected with the target material by combining the hot isostatic pressing and the diffusion welding, so that the processing difficulty is reduced and the combination is realized compared with the process that the back plate is directly combined with the target material powder by one hot isostatic pressing. Because it is difficult to combine the target powder and the backing plate by hot isostatic pressing once, the powder is packed in the sheath and becomes compact target material by hot isostatic pressing, the external shrinkage is very large, even up to 40% shrinkage according to the powder granularity composition, while the backing plate is compact material, and will not shrink in the process of hot isostatic pressing, in addition, the two hot isostatic pressing processes are different, the required temperature for diffusion welding cannot be too high, and must be lower than the melting point of the backing plate (such as Cu), while the temperature of the first hot isostatic pressing of CrW reaches 1300 ℃, which is far higher than the melting point of the copper backing plate, so that the first hot isostatic pressing cannot be realized.
Further, in step S1, the particle size of the W powder is 10-30 μm.
Further, in step S1, the atomic ratio of the W element in the predetermined ratio is 20 to 50%.
Further, in step S2, the degassing temperature is 350-500 deg.C (e.g. 350 deg.C, 400 deg.C, 450 deg.C, 500 deg.C).
Further, in step S2, the degassing vacuum degree in the degassing treatment is 1×10 -3 ～9*10 -3 Pa (e.g. 1 x 10 -3 Pa、2*10 -3 Pa、3*10 -3 Pa、4*10 -3 Pa、5*10 -3 Pa、6*10 -3 Pa、7*10 -3 Pa、8*10 -3 Pa、9*10 -3 Pa)。
Further, in step S3, the treatment temperature at the time of the hot isostatic pressing treatment is 1200 ℃ -1400 ℃ (e.g. 1200 ℃, 1250 ℃, 1300 ℃, 1350 ℃, 1400 ℃), preferably 1300 ℃.
Further, in step S3, the pressure during the hot isostatic pressing treatment is 100 to 150MPa (e.g., 100MPa, 110MPa, 120MPa, 130MPa, 140MPa, 150 MPa), preferably 130MPa.
Further, in step S3, the heat-preserving and pressure-maintaining time during the hot isostatic pressing treatment is 1-4 h (e.g. 1h, 2h, 3h, 4 h).
Further, in step S4, the cutting is performed using a medium-speed wire cutting machine.
Further, in step S4, the flatness of both end surfaces of the target sheet after the grinding process is less than 0.05mm (e.g., 0.01mm,0.02mm,0.03mm,0.04 mm). And (3) through grinding processing, the linear cutting marks are ground flat, so that the two end surfaces of the target piece are ensured to be flat.
Further, in step S5, the roughness of the two end surfaces of the target after the sandblasting is not less than ra3.6 (e.g., ra3.6, ra3.7, ra3.8, ra3.9, ra 4.0). The roughness is improved by sand blasting, and the welding binding force is further improved, and the roughness is lower and the coating binding force is poorer after the plane is ground, so that the surface is roughened by sand blasting.
Further, in step S6, the plating treatment is a nickel plating treatment, and the plating thickness is about 0.1-0.3mm (e.g., 0.1mm, 0.15mm, 0.2mm, 0.25mm, 0.3 mm). The electroplated nickel layer has high chemical stability, strong binding force with the CrW target material matrix, infinite solid solution of the nickel coating and the copper backboard, mutual diffusion, easy formation of a better welding interface, and meanwhile, the thermal expansion coefficient of nickel is between two welding materials, so that the welding stress can be effectively reduced, the welding interface is more excellent, and the welding rate is higher.
Further, in step S7, the material of the alloy back plate may be Cu, mo, or alloys thereof. Cu has better heat and electric conductivity, and is a preferable backboard material for the target material; mo has a small coefficient of thermal expansion and relatively high strength, and is also a preferred backing plate material; the CuMo and the CuMo can be made into alloys, and materials with good comprehensive performance can be designed and manufactured to be used as the back plate by regulating and controlling the proportion of the CuMo and the CuMo.
Further, in step S7, the degassing temperature at the time of the degassing treatment is 300-400 ℃ (e.g., 300 ℃, 350 ℃, 400 ℃).
Further, in step S7, the degassing vacuum degree at the time of the degassing treatment is not more than 2×10 -2 Pa (e.g. 2 x 10 - 2 Pa、1*10 -2 Pa、9*10 -3 Pa、8*10 -3 Pa、7*10 -3 Pa、6*10 -3 Pa、5*10 -3 Pa)。
Further, in step S8, the treatment temperature at the time of the diffusion welding treatment is 500 ℃ -950 ℃ (e.g., 500 ℃, 550 ℃, 600 ℃, 650 ℃, 700 ℃, 750 ℃, 800 ℃, 850 ℃, 900 ℃, 950 ℃), preferably 750 ℃.
Further, in step S8, the pressure at the time of the diffusion welding treatment is 100 to 150MPa (e.g., 100MPa, 110MPa, 120MPa, 130MPa, 140MPa, 150 MPa).
Further, in step S8, the holding time during the diffusion welding process is 3-6h (e.g., 3h, 4h, 5h, 6 h).
Further, in step S8, the diffusion welding process is performed by a hot isostatic press.
Further, in step S9, the machining is machining, in particular machining by means of a microtome.
The CrW alloy target material prepared by the preparation method comprises Cr and W in a given proportion, wherein the atomic proportion of W is 5-50%.
Further, the relative density of the CrW alloy target is more than or equal to 99 percent.
The CrW alloy target material has uniform structure, no segregation, no agglomeration and the like, and the compactness is more than 99 percent.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the CrW alloy target material with the atomic ratio of W reaching 50% is prepared by the HIP process, the density is over 99%, and the back plate and the target piece achieve good diffusion welding effect by surface modification nickel plating and HIP diffusion welding, so that the problem of difficult machining is solved.
Drawings
FIG. 1 is a schematic flow chart of the preparation method of the invention;
FIG. 2 is a drawing of Cr obtained in example 1 95 W 5 An alloy microcosmic appearance map;
FIG. 3 is a drawing of Cr obtained in example 2 92 W 8 An alloy microcosmic appearance map;
FIG. 4 is a drawing of Cr obtained in example 3 90 W 10 An alloy microcosmic appearance map;
FIG. 5 is a Cr obtained in example 4 70 W 30 An alloy microcosmic appearance map;
FIG. 6 is a Cr obtained in example 5 50 W 50 An alloy microcosmic appearance map;
FIG. 7 is a sample of Cr obtained in example 6 90 W 10 An alloy microcosmic appearance map;
FIG. 8 is a Cr obtained in example 7 90 W 10 An alloy microcosmic appearance map;
FIG. 9 is a Cr obtained in comparative example 1 95 W 5 An alloy microcosmic appearance map;
FIG. 10 is a Cr obtained in comparative example 2 70 W 30 An alloy microcosmic appearance map;
FIG. 11 is a Cr obtained in comparative example 3 70 W 30 An alloy microcosmic appearance map;
FIG. 12 is a Cr obtained in comparative example 4 70 W 30 And (5) an alloy microcosmic topography map.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The examples of the present invention are implemented on the premise of the technical scheme of the present invention, and detailed implementation modes and processes are given, but the protection scope of the present invention is not limited to the following examples, in which the process parameters of specific conditions are not noted, and generally according to conventional conditions.
The endpoints of the ranges and any values disclosed in the present invention are not limited to the precise range or value, and the range or value should be understood to include values close to the range or value. For numerical ranges, one or more new numerical ranges may be obtained in combination with each other between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point values, and are to be considered as specifically disclosed in the present invention.
In the present invention, all values relating to the amounts of the components are "parts by weight" throughout unless specified and/or indicated otherwise. The process parameters for the specific conditions not noted in the examples below are generally as usual.
Examples 1 to 5
The preparation method of the CrW alloy target material is shown in a figure 1, and specifically comprises the following steps:
s1, uniformly mixing Cr powder and W powder according to a given proportion, wherein the atomic proportion of W element in the given proportion is 5-50%, the granularity of the Cr powder is 25 mu m, and the granularity of the W powder is 10 mu m;
s2, filling the mixed powder into a sheath die for degassing treatment, wherein the degassing heat preservation temperature is 400 ℃, and the degassing vacuum degree is 4 x 10 -3 Pa；
S3, placing the degassed sheath into a hot isostatic pressing furnace for hot isostatic pressing, wherein the treatment temperature is 1300 ℃, the pressure is 130MPa, and the heat preservation and pressure maintaining time is 1h;
s4, removing the sheath from the blank subjected to the hot isostatic pressing treatment, cutting the blank into target pieces with corresponding sizes by using a medium-speed wire cutting machine, and grinding the two end surfaces of the target pieces until the flatness is less than 0.05mm;
s5, carrying out sand blasting on two end faces of the target piece after grinding treatment, so that the roughness of the two end faces of the target piece is not less than Ra3.6;
s6, electroplating the two end surfaces of the target piece subjected to sand blasting, namely electroplating a nickel layer, wherein the thickness of the electroplated layer is about 0.01-0.1mm;
s7, stacking the electroplated target pieces and alloy backboard with the same size together, and filling the stacked target pieces and alloy backboard into a sheath die for degassing treatment, wherein the alloy backboard is made of Cu, the degassing heat preservation temperature is 300-400 ℃, and the degassing vacuum degree is 2 x 10 -2 Pa；
S8, putting the degassed sheath into a hot isostatic pressing machine for diffusion welding treatment, wherein the treatment temperature is 900 ℃, the pressure is 100-150MPa, and the heat preservation time is 4 hours;
s9, removing the sheath from the target piece subjected to diffusion welding treatment, and then processing the target piece to a target material with a required shape through a slicing machine to obtain the CrW alloy target material with the backboard;
examples 1-5 specific preparation process parameters and results of the resulting CrW alloy target composition and the like are recorded in table 1, and the microstructure morphologies of the resulting alloys are shown in fig. 2-6, respectively.
Example 6
S8, putting the degassed sheath into a hot isostatic pressing machine for diffusion welding treatment, wherein the treatment temperature is 600 ℃, the pressure is 135MPa, and the heat preservation time is 4 hours;
the rest of the settings were the same as in example 3.
Example 6 specific preparation process parameters and the results of the resulting CrW alloy target composition and the like are reported in table 1. The microstructure morphology of the resulting alloy is shown in fig. 7.
Example 7
S8, putting the degassed sheath into a hot isostatic pressing machine for diffusion welding treatment, wherein the treatment temperature is 800 ℃, the pressure is 135MPa, and the heat preservation time is 4 hours;
the rest of the settings were the same as in example 3.
Example 7 specific preparation process parameters and the results of the resulting CrW alloy target composition and the like are reported in table 1. The microstructure morphology of the resulting alloy is shown in fig. 8.
Comparative example 1
A preparation method of a CrW alloy target material is different from the preparation method in the embodiment 1 in that the preparation method comprises the following steps that S1, cr powder and W powder are uniformly mixed according to a given proportion, wherein the atomic proportion of W element in the given proportion is 5%, the granularity of the Cr powder is 150 mu m, and the granularity of the W powder is 10 mu m;
the rest of the settings are the same as in example 1.
Comparative example 1 specific preparation process parameters and the results of the resulting CrW alloy target components and the like are recorded in table 1. The microstructure morphology of the resulting alloy is shown in fig. 9.
Comparative example 2
A preparation method of a CrW alloy target material is different from that of the embodiment 4 in that the step S1 is that Cr powder and W powder are uniformly mixed according to a preset proportion, wherein the atomic proportion of W element in the preset proportion is 30%, the granularity of the Cr powder is 150 mu m, and the granularity of the W powder is 10 mu m;
the rest of the settings were the same as in example 4.
Comparative example 2 specific preparation process parameters and the results of the resulting CrW alloy target components and the like are recorded in table 1. The microstructure morphology of the resulting alloy is shown in fig. 10.
Comparative example 3
A preparation method of a CrW alloy target material is different from that of the embodiment 4 in that the step S1 is that Cr powder and W powder are uniformly mixed according to a preset proportion, wherein the atomic proportion of W element in the preset proportion is 30%, the granularity of the Cr powder is 25 mu m, and the granularity of the W powder is 45 mu m;
the rest of the settings were the same as in example 4.
Comparative example 3 specific preparation process parameters and the results of the resulting CrW alloy target components and the like are recorded in table 1. The microstructure morphology of the resulting alloy is shown in fig. 11.
Comparative example 4
A preparation method of a CrW alloy target material is different from that of the embodiment 4 in that the step S1 is that Cr powder and W powder are uniformly mixed according to a preset proportion, wherein the atomic proportion of W element in the preset proportion is 30%, the granularity of the Cr powder is 150 mu m, and the granularity of the W powder is 45 mu m;
the rest of the settings were the same as in example 4.
Comparative example 4 specific preparation process parameters and the results of the resulting CrW alloy target components and the like are recorded in table 1. The microstructure morphology of the resulting alloy is shown in fig. 12.
TABLE 1 preparation method parameters and results recording Table of CrW alloy targets in examples 1-7 and comparative examples 1-4
As can be seen from the data in Table 1, the target material with the atomic ratio of up to 50% is prepared by optimizing the powder granularity and the forming process in the embodiments 1-7, and the target material of the CrW alloy has the advantages of good surrounding structure dispersion, uniform structure, no segregation, no agglomeration and the like, and the compactness of over 99% as can be seen from the figures 2-8. In addition, in comparative example 1 and example 1, although 150 μm of Cr powder material was used in comparative example 1, the density was not greatly affected by the less 5% of W content, but the microstructure difference was large, as shown in FIG. 2 and FIG. 9, and the dispersion of W in the Cr matrix in comparative example 1 in FIG. 9 was significantly poor.
By comparing comparative example 2 with example 4, although 150 μm Cr powder material was selected in comparative example 2, the density was greatly affected by the addition of W to 30%, the density of example 4 was 99.1%, and the density of comparative example 2 was 98.3%, and the microstructures of both were compared, as shown in FIG. 5 and FIG. 10, it can be seen that the dispersion of W in comparative example 2 in FIG. 10 was inferior to that of example 4.
By comparison of comparative example 3 and comparative example 4, it was found that although both of the W raw materials of 45 μm were selected, cr raw materials were 25 μm and 150 μm, respectively, and the compactibility of comparative example 3 and comparative example 4 was 98.9% and 98.1%, respectively, with a clear difference, and both were less than the target values of 99%. From the microscopic observation of both, as shown in fig. 11 and 12, it can be seen that the W particles are mainly because they are larger and are not easily dispersed in the Cr matrix, and particularly in comparative example 4 of fig. 12, the W agglomeration is more remarkable due to the larger difference in particle size between W and Cr, resulting in lower density after hot isostatic pressing.
In addition, it was found from comparison of examples 3, 6 and 7 that the diffusion welding temperature did not greatly affect the final strength and the welding rate of diffusion welding, and that excellent welding effect was achieved in the process range of the present application.
Claims (10)
1. The preparation method of the CrW alloy target is characterized by comprising the following steps of:
s1, uniformly mixing Cr powder and W powder according to a given proportion, wherein the atomic proportion of W element in the given proportion is 5-50%, and the granularity of Cr powder is less than 30 mu m;
s2, filling the mixed powder into a sheath die for degassing treatment;
s3, performing hot isostatic pressing forming on the degassed sheath;
s4, removing the sheath from the blank subjected to the hot isostatic pressing, cutting the blank into target pieces with corresponding sizes, and grinding two end surfaces of the target pieces;
s5, carrying out sand blasting on two end faces of the target piece after grinding;
s6, electroplating the two end surfaces of the target piece subjected to sand blasting;
s7, stacking the target piece subjected to the electroplating treatment and an alloy backboard with the same size together, and filling the target piece and the alloy backboard into a sheath die for degassing treatment;
s8, performing diffusion welding treatment on the degassed sheath;
s9, removing the sheath from the target piece subjected to diffusion welding treatment, and then processing the target piece to a target material with a required shape to obtain the CrW alloy target material with the backboard.
2. The method according to claim 1, wherein in step S1, the particle size of the W powder is 10 to 30 μm.
3. The method according to claim 1, wherein in step S1, the atomic ratio of W element in the predetermined ratio is 20 to 50%.
4. The method according to claim 1, wherein in step S3, the treatment temperature at the time of the hot isostatic pressing treatment is 1200 ℃ to 1400 ℃; the pressure is 100-150 MPa.
5. The method according to claim 1, wherein in step S4, the flatness of both end surfaces of the target sheet after the grinding process is less than 0.05mm.
6. The method according to claim 1, wherein in step S5, the roughness of both end surfaces of the target after the blasting is not less than ra3.6.
7. The method of claim 1, wherein in step S6, the plating process is a nickel plating process, and the plating thickness is about 0.1 to 0.3mm.
8. The method of claim 1, wherein in step S7, the alloy backing plate is made of Cu, mo or alloys thereof.
9. The method according to claim 1, wherein in step S8, the treatment temperature at the time of the diffusion welding treatment is 500 ℃ to 950 ℃; the pressure is 100-150MPa; the heat preservation time is 3-6h.
10. A CrW alloy target prepared by the preparation method as set forth in any one of claims 1 to 9, wherein the CrW alloy target comprises Cr and W in a predetermined proportion, wherein the atomic proportion of W is 5 to 50%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211734636.XA CN116200639A (en) | 2022-12-30 | 2022-12-30 | CrW alloy target and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211734636.XA CN116200639A (en) | 2022-12-30 | 2022-12-30 | CrW alloy target and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116200639A true CN116200639A (en) | 2023-06-02 |
Family
ID=86506930
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211734636.XA Pending CN116200639A (en) | 2022-12-30 | 2022-12-30 | CrW alloy target and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116200639A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001262325A (en) * | 2000-03-14 | 2001-09-26 | Hitachi Metals Ltd | Cr-W ALLOY BASED SPUTTERING TARGET MATERIAL AND ITS PRODUCING METHOD |
| CN101537530A (en) * | 2009-03-16 | 2009-09-23 | 宁波江丰电子材料有限公司 | Manufacturing method of target structure |
| CN103320756A (en) * | 2013-06-20 | 2013-09-25 | 安泰科技股份有限公司 | Method for preparing high-purity, high-density and large-size molybdenum alloy target |
| CN104259644A (en) * | 2014-07-24 | 2015-01-07 | 有研亿金新材料有限公司 | Welding method of tungsten-titanium alloy target |
| CN104694895A (en) * | 2013-12-05 | 2015-06-10 | 有研亿金新材料股份有限公司 | W-Ti alloy target material and manufacturing method thereof |
| CN104708192A (en) * | 2013-12-12 | 2015-06-17 | 有研亿金新材料有限公司 | Diffusion welding method for W-Ti alloy target assembly |
| CN113579233A (en) * | 2021-07-14 | 2021-11-02 | 先导薄膜材料有限公司 | Tungsten-titanium alloy target material and preparation method and application thereof |
-
2022
- 2022-12-30 CN CN202211734636.XA patent/CN116200639A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001262325A (en) * | 2000-03-14 | 2001-09-26 | Hitachi Metals Ltd | Cr-W ALLOY BASED SPUTTERING TARGET MATERIAL AND ITS PRODUCING METHOD |
| CN101537530A (en) * | 2009-03-16 | 2009-09-23 | 宁波江丰电子材料有限公司 | Manufacturing method of target structure |
| CN103320756A (en) * | 2013-06-20 | 2013-09-25 | 安泰科技股份有限公司 | Method for preparing high-purity, high-density and large-size molybdenum alloy target |
| CN104694895A (en) * | 2013-12-05 | 2015-06-10 | 有研亿金新材料股份有限公司 | W-Ti alloy target material and manufacturing method thereof |
| CN104708192A (en) * | 2013-12-12 | 2015-06-17 | 有研亿金新材料有限公司 | Diffusion welding method for W-Ti alloy target assembly |
| CN104259644A (en) * | 2014-07-24 | 2015-01-07 | 有研亿金新材料有限公司 | Welding method of tungsten-titanium alloy target |
| CN113579233A (en) * | 2021-07-14 | 2021-11-02 | 先导薄膜材料有限公司 | Tungsten-titanium alloy target material and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108060322B (en) | Preparation method of hard high-entropy alloy composite material | |
| CN108823478B (en) | Ultra-fine high-entropy alloy binding phase metal ceramic and preparation method thereof | |
| CN109371307A (en) | It is a kind of using high-entropy alloy powder as the preparation method of the WC base cemented carbide of binder | |
| CN108941537B (en) | Method for 3D printing of special high-temperature alloy by using electron beams | |
| CN114481053B (en) | Magnesium zinc aluminum nickel vanadium alloy target and manufacturing method thereof | |
| CN109338193B (en) | Coreless-ring structure metal ceramic alloy and preparation method thereof | |
| CN103667844A (en) | Hard alloy for low-load high-speed punching precision mold and preparation method thereof | |
| CN112680646B (en) | Preparation method of TiC-based metal ceramic with high-entropy alloy binder phase | |
| CN113881875B (en) | Three-dimensional framework structure metal reinforced aluminum matrix composite material and preparation method thereof | |
| CN106799496A (en) | A kind of graphite and alusil alloy composite electron encapsulating material and preparation method thereof | |
| CN111304479A (en) | Preparation method of VCrNbMoW refractory high-entropy alloy | |
| CN109576546A (en) | A kind of preparation method of the high-strength tenacity without magnetic Ti (C, N) based ceramic metal | |
| CN110229989B (en) | Multi-element hard alloy and preparation method thereof | |
| CN116804265B (en) | CrAlCuFe alloy target and preparation method thereof | |
| CN111438356B (en) | Titanium-aluminum target material for physical vapor deposition and preparation method thereof | |
| CN111822708B (en) | Preparation method of powder metallurgy Ti-W metal-metal heterostructure composite material | |
| KR20080091921A (en) | Wc-ni hard metal and method for producing the same | |
| CN110983152B (en) | Fe-Mn-Si-Cr-Ni based shape memory alloy and preparation method thereof | |
| CN112024891A (en) | Hard alloy composite material and manufacturing method thereof | |
| CN116200639A (en) | CrW alloy target and preparation method thereof | |
| CN107034375A (en) | A kind of method that utilization hydride powder prepares high-compactness titanium article | |
| CN111136265A (en) | Titanium-silicon alloy target and manufacturing method thereof | |
| TWI518185B (en) | Composite of carbide cermet/blending metal | |
| CN116079055A (en) | CrAlFe-based alloy target and preparation method thereof | |
| CN113088781B (en) | High-entropy hard alloy and preparation method and application 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 |