CN114378304A - Process method for preparing tungsten-based composite sheet by combining selective laser melting and hot isostatic pressing technology - Google Patents

Process method for preparing tungsten-based composite sheet by combining selective laser melting and hot isostatic pressing technology Download PDF

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Publication number
CN114378304A
CN114378304A CN202210051631.0A CN202210051631A CN114378304A CN 114378304 A CN114378304 A CN 114378304A CN 202210051631 A CN202210051631 A CN 202210051631A CN 114378304 A CN114378304 A CN 114378304A
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tungsten
based composite
sheet
powder
composite layer
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王万景
许华旗
杜培松
李强
谢春意
罗广南
黄伶明
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Hefei Institutes of Physical Science of CAS
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Hefei Institutes of Physical Science of CAS
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20Direct sintering or melting
    • B22F10/28Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • B22F3/15Hot isostatic pressing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00Manufacture 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
    • B22F7/02Manufacture 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 layers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00Processes of additive manufacturing

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Composite Materials (AREA)
  • Pressure Welding/Diffusion-Bonding (AREA)

Abstract

The invention provides a process method for preparing a tungsten-based composite sheet by combining selective laser melting and hot isostatic pressing, which belongs to the technical field of dissimilar metal compounding and comprises the following key technical steps: 1) the tungsten-based composite sheet consists of a tungsten sheet and a tungsten-based composite layer; 2) the tungsten sheet is made of rolled pure tungsten or tungsten alloy material; 3) depositing a tungsten-based composite layer on the tungsten sheet in a selective laser melting mode, and then improving the diffusion connection between the tungsten sheet and the composite layer and the composite diffusion and densification of tungsten and composite metal in the tungsten-based composite layer by adopting a hot isostatic pressing method; 4) the tungsten-based composite layer can be made of selected metals including tungsten, copper, nickel, chromium, vanadium, iron, titanium and the like. According to the invention, the tungsten sheet and the tungsten-based composite layer are combined together by combining the selective laser melting and hot isostatic pressing processes, and the prepared tungsten-based composite sheet can effectively release stress and increase the strength and the irradiation resistance, so that the tungsten-based composite sheet is easy to produce in batches and apply to fusion reactor high-heat-load parts.

Description

Process method for preparing tungsten-based composite sheet by combining selective laser melting and hot isostatic pressing technology
Technical Field
The invention discloses a process method for preparing a tungsten-based composite sheet by combining selective laser melting and hot isostatic pressing technologies, and belongs to the technical field of dissimilar metal compounding.
Background
The development and application of fusion energy are hopes for thoroughly solving the human energy crisis, the development of magnetic confinement nuclear fusion energy has already entered the engineering verification stage at present, and the design and development of fusion reactor internal components are the last barriers in front of researchers at home and abroad.
The internal parts of the fusion reactor directly face high-temperature plasma, the working environment is extremely severe, the materials are required to have high thermal conductivity and high mechanical strength, particularly, the plasma materials are required to have good compatibility with the plasma, the internal parts of the fusion reactor are usually designed by composite welding of multiple materials, for example, a divertor part is designed by tungsten-copper composite, a cladding part is designed by tungsten-steel composite, the tungsten material is a protective armor material, copper and steel are heat sink structural materials, and in order to improve the service temperature and the irradiation resistance of the copper and steel, copper alloy and low activation steel (RAFM) are generally selected. In order to alleviate the problem of mismatch of thermo-mechanical properties between the tungsten armor and the copper alloy heat sink or the RAFM steel, an intermediate transition layer, such as an oxygen-free copper intermediate layer, is usually added between the tungsten armor and the copper alloy or the RAFM steel, and the preparation process mainly comprises the following steps: firstly, preparing a tungsten/oxygen-free copper composite sheet (the thickness of a tungsten layer is 2mm, the thickness of a copper layer is 1mm) by adopting a hot isostatic pressing or pouring technology, then welding the tungsten copper sheet and a copper alloy or RAFM steel by adopting a hot isostatic pressing diffusion welding technology, and finally processing and manufacturing an internal part with required size. The oxygen-free copper is taken as high-purity copper, has high thermal conductivity and high plasticity, is easily subjected to high-temperature creep deformation and irradiation embrittlement after being used for a long time in the high-temperature and high-neutron flux environment of a fusion reactor, and is easily subjected to joint fracture behavior in the plastic deformation process, so that the component failure is caused, and the safety of the device is influenced.
In order to enhance the high-temperature mechanical property and the neutron irradiation resistance of the pure copper intermediate layer, a solution of adding composite enhanced copper layers of tungsten, SiC and the like is provided in the current research. The tungsten and SiC substances are added mainly in two forms of fibers and particles, namely, the particles or short fibers of the tungsten and the SiC are mixed with the copper powder, and then the tungsten and the SiC particles or the short fibers are compounded together by adopting a high-temperature liquid-phase fusion method. Because the densities of tungsten and SiC particles or fibers and copper are different, the segregation problem of the added dopant is easily caused in the copper melting process, the reinforcing effect is reduced, and the integral high-temperature performance of the composite layer is out of control. Therefore, a method of pre-weaving tungsten and SiC fibers and then pouring copper melt is adopted, and although the process can realize the orderly addition of dopants, the process is complex, the manufacturing cost is high, and the mass production is not facilitated. In addition, the deposition of the composite layer is also performed by PVD or the like, but the efficiency is too low.
Disclosure of Invention
The invention aims at the problems and provides a method for preparing a tungsten-based compact by combining selective laser melting and hot isostatic pressing. The selective laser melting technology has been developed for more than ten years, is relatively mature, and is particularly suitable for preparing sheets in an array manner. This lays a solid technical foundation for the implementation of the invention. On the other hand, the hot isostatic pressing technology is also very suitable for densification and internal diffusion welding of the composite material, thereby improving the performance of the composite material. Therefore, the tungsten-based composite sheet is prepared by combining the selective laser melting and hot isostatic pressing welding method, and is further applied to the welding manufacture of the internal parts of the fusion reactor in a large scale.
The invention provides a new preparation method for the tungsten-based composite sheet.
In order to achieve the purpose, the invention adopts the following specific scheme:
a process method for preparing a tungsten-based composite sheet by combining selective laser melting and hot isostatic pressing technology comprises the following steps:
a) structural design: the tungsten-based composite sheet comprises a tungsten sheet and a tungsten-based composite layer, wherein the thickness of the tungsten sheet is 1-6mm, and the thickness of the tungsten-based composite layer is 0.01-2 mm.
b) The connection process comprises the following steps: the method comprises the steps of taking a tungsten sheet as a matrix, carrying out selective melting of composite powder on the tungsten sheet by adopting a selective laser melting technology, cladding the tungsten sheet on a tungsten-based composite layer to a certain thickness through multiple layers, putting the tungsten-based composite sheet into a hot isostatic pressing furnace, and carrying out diffusion welding of the tungsten sheet and the tungsten-based composite layer as well as tungsten and other metals in the composite layer by selecting proper hot isostatic pressing parameters.
Further, the tungsten sheet is made of pure tungsten or tungsten-based alloy materials.
Further, the tungsten-based composite layer is made of tungsten copper, tungsten nickel, tungsten iron, tungsten chromium, tungsten vanadium, tungsten titanium, tungsten zirconium, tungsten vanadium chromium, tungsten vanadium copper or tungsten copper iron.
Further, elements of the tungsten-based composite layer are distributed in proportion in the thickness direction.
Further, the tungsten-based composite layer is coated on the tungsten sheet by adopting a selective laser melting method, the base material used by the tungsten-based composite layer is tungsten powder, and the other material is copper powder, nickel powder, iron powder, chromium powder, vanadium powder, titanium powder or zirconium powder, or is directly prepared from tungsten-vanadium alloy powder, copper-coated tungsten powder, nickel-coated tungsten powder, iron-coated tungsten powder, tungsten-chromium alloy powder, tungsten-vanadium alloy powder, tungsten-titanium alloy powder, tungsten-zirconium alloy powder, tungsten-vanadium-chromium alloy powder, tungsten-vanadium-copper alloy powder or tungsten-copper-iron alloy powder.
Furthermore, the selective laser melting refers to placing and fixing one or more tungsten sheets in a melting chamber, then spreading powder, performing selective melting on each tungsten sheet, and performing selective melting for multiple times according to thickness requirements to prepare the tungsten-based composite sheet.
Furthermore, in the hot isostatic pressing process, element diffusion can occur to the composite elements in the tungsten-based composite layer, and meanwhile, some closed gaps in the tungsten-based composite layer can be closed, so that the densification of the tungsten-based composite layer is realized.
Further, the external dimension of the tungsten-based composite sheet is determined by design, and the external dimension of the tungsten-based composite sheet is processed after hot isostatic pressing; the tungsten sheet is tungsten potassium, tungsten rhenium alloy or zirconium carbide doped tungsten alloy.
Further, the atomic fraction of tungsten in the tungsten-based composite layer continuously changes from 100% to 0% in the thickness direction.
Further, the tungsten-based composite layer is divided into four layers, and the atomic fraction of tungsten changes in a gradient manner in the thickness direction.
The invention has the following beneficial effects:
the invention prepares the tungsten-based composite sheet by combining two technologies of selective laser melting and hot isostatic pressing, wherein the selective laser melting is a process for realizing instantaneous liquid melting composite welding of one or two metal materials, and the hot isostatic pressing is a process for slowly realizing solid hot pressing diffusion welding of the two materials, and the two processes are combined, so that the problem of large residual stress in the instantaneous melting solidification process can be overcome, and the compact diffusion of the composite material can be realized, thereby achieving the improvement of the properties of the composite layer such as strengthening and toughening, radiation resistance and the like; in addition, the technology introduced by the invention can realize the mass production of the tungsten-based composite sheet, and is particularly beneficial to the industrial application of the tungsten-based composite sheet in the fusion field.
Drawings
FIG. 1 is a schematic view of a tungsten based composite sheet;
FIG. 2 is a schematic view of the arrangement and cladding of a tungsten-based composite sheet in a selective laser melting printing chamber;
in the figure, 1 is a tungsten plate, 2 is a tungsten-based composite layer, 3 is a print chamber substrate, and 4 is a laser beam.
Detailed Description
The invention is described in detail below with reference to the figures and the embodiments. The following examples are only for explaining the present invention, the scope of the present invention shall include the full contents of the claims, and the full contents of the claims of the present invention can be fully realized by those skilled in the art through the following examples.
The invention discloses a process method for preparing a tungsten-based composite sheet by combining selective laser melting and hot isostatic pressing technologies, which comprises the following steps of:
(1) the structure of the prepared tungsten-based composite sheet is shown in figure 1, and the tungsten-based composite sheet comprises a tungsten sheet 1 and a printed tungsten-based composite layer 2.
(2) Firstly, cutting a tungsten sheet 1 on a rolled tungsten plate, then grinding the tungsten sheet 1 into a required size, controlling the surface roughness Ra of the processed tungsten sheet to be less than 1.6 mu m, then cleaning the tungsten sheet to remove oil stains and oxide scales, drying the tungsten sheet, placing the tungsten sheet in a printing chamber of selective laser melting equipment, and discharging the tungsten sheet 1 to be flat to ensure that the upper surface is on a plane, as shown in figure 2.
(3) And carrying out powder paving operation in the printing chamber under the protection of atmosphere, wherein the height of the composite powder is required to just cover the tungsten sheet 1.
(4) Selecting proper parameters to carry out selective melting of the composite powder in the area of the tungsten sheet 1, melting a layer of composite powder on the tungsten sheet 1 and depositing the composite powder on the tungsten sheet 1 to form a tungsten-based composite layer 2.
(5) And (4) repeating the steps (3) and (4), carrying out multi-layer selective area melting, and stopping selective area melting after the thickness of the tungsten-based composite layer 2 reaches the required size.
(6) And putting the tungsten-based composite sheet into a hot isostatic pressing furnace, and selecting proper hot isostatic pressing parameters to carry out diffusion welding.
(7) The tungsten-based composite sheet is machined to the required dimensions according to the design, and the general dimension of the tungsten-based composite sheet is 45 x12x2.5mm.
Preferably, the tungsten sheet 1 is made of pure tungsten or tungsten-based alloy material.
Preferably, the material of the tungsten-based composite layer 2 is tungsten copper, tungsten nickel, tungsten iron, tungsten chromium, tungsten vanadium, tungsten titanium, tungsten zirconium, tungsten vanadium chromium, tungsten vanadium copper or tungsten copper iron.
Preferably, the elements of the tungsten-based composite layer 2 are proportionally distributed in the thickness direction, such as the atomic fraction of tungsten in the tungsten-based composite layer 2 continuously varies from 100% to 0% in the thickness direction or the tungsten-based composite layer 2 is divided into four layers, and the atomic fraction of tungsten varies in a gradient in the thickness direction.
Preferably, the tungsten-based composite layer 2 is coated on the tungsten sheet 1 by adopting a selective laser melting method, the base material used by the tungsten-based composite layer 2 is tungsten powder, and the other material is copper powder, nickel powder, iron powder, chromium powder, vanadium powder, titanium powder or zirconium powder, or tungsten-vanadium alloy powder, copper-coated tungsten powder, nickel-coated tungsten powder, iron-coated tungsten powder, tungsten-chromium alloy powder, tungsten-vanadium alloy powder, tungsten-titanium alloy powder, tungsten-zirconium alloy powder, tungsten-vanadium-chromium alloy powder, tungsten-vanadium-copper alloy powder or tungsten-copper-iron alloy powder is directly used.
Preferably, the selective laser melting refers to placing and fixing one or more tungsten sheets 1 in a melting chamber, then spreading powder, performing selective melting on each tungsten sheet 1, and performing selective melting for multiple times according to thickness requirements to prepare the tungsten-based composite sheet.
Preferably, in the hot isostatic pressing process, element diffusion occurs in the composite elements in the tungsten-based composite layer 2, and meanwhile, some closed gaps in the tungsten-based composite layer 2 are closed, so as to achieve densification of the tungsten-based composite layer 2.
Preferably, the tungsten-based compact has a form factor determined by design, and the form factor is machined after hot isostatic pressing.
Preferably, the tungsten sheet 1 is tungsten potassium, tungsten rhenium alloy, or zirconium carbide doped tungsten alloy. The preparation of the W-Cu composite sheet for the first wall of the water-cooled ceramic cladding of the Chinese Fusion Engineering Test Reactor (CFETR) is further described. The method comprises the following key points and steps:
(1) and cutting the tungsten sheet 1 from the rolled tungsten plate on a line, then grinding each surface of the tungsten sheet 1 to Ra of less than 1.6 mu m by an upper grinding machine, cleaning and drying for later use.
(2) Putting the cleaned tungsten sheet 1 into a selective melting equipment printing chamber, and arranging the tungsten sheets 1 in a fixed tool according to a 2x10 array to ensure that the upper surface of the tungsten sheet 1 is on a plane.
(3) And (3) spreading tungsten powder and copper powder in a printing chamber in proportion, wherein the atomic proportion of the tungsten powder is 80% at the beginning, and after the tungsten piece is covered by the composite powder to a high degree, the composite powder is smoothed by a scraper, and the thickness of the composite powder is about 25 mu m.
(4) Selecting proper parameters to carry out selective melting of the composite powder in the area of the tungsten sheet 1, melting a layer of composite powder on the tungsten sheet 1 and depositing the composite powder on the tungsten sheet 1 to form a tungsten-based composite layer 2.
(5) According to the program, the printing plate automatically reduces the thickness of a printing layer, powder is spread again and is smoothed by a scraper, and then secondary selective melting is carried out.
(6) And carrying out multi-layer selective melting, and stopping selective melting after the thickness of the tungsten-based composite layer 2 reaches 0.2 mm.
(7) The tungsten-based composite layer 2 is divided into four layers, each layer is 50 mu m thick, and the proportion of tungsten in the four layers is 80%, 60%, 40% and 20% in sequence.
(8) And (3) placing the tungsten-based composite sheet into a hot isostatic pressing furnace, selecting proper hot isostatic pressing parameters to carry out diffusion welding, and selecting the hot isostatic pressing temperature of the tungsten-copper composite sheet to be 1050 ℃.
(9) The tungsten based compacts are machined to the required dimensions, typically 45x12x2.2mm, according to design.
The invention has not been described in detail and is part of the common general knowledge of a person skilled in the art. The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (10)

1. A process method for preparing a tungsten-based composite sheet by combining selective laser melting and hot isostatic pressing technology is characterized by comprising the following steps of:
a) structural design: the tungsten-based composite sheet comprises a tungsten sheet (1) and a tungsten-based composite layer (2), wherein the thickness of the tungsten sheet (1) is 1-6mm, and the thickness of the tungsten-based composite layer (2) is 0.01-2 mm;
b) the connection process comprises the following steps: the method comprises the steps of taking a tungsten sheet (1) as a matrix, carrying out selective melting of composite powder on the tungsten sheet (1) by adopting a selective laser melting technology, carrying out multilayer cladding, enabling a tungsten-based composite layer (2) to reach a certain thickness, placing the tungsten-based composite sheet into a hot isostatic pressing furnace, and carrying out diffusion welding of tungsten in the tungsten sheet (1) and the tungsten-based composite layer (2) and tungsten and other metals in the tungsten-based composite layer (2) by selecting proper hot isostatic pressing parameters.
2. The process according to claim 1, characterized in that: the tungsten sheet (1) is made of pure tungsten or tungsten-based alloy materials.
3. The process according to claim 1, characterized in that: the tungsten-based composite layer (2) is made of tungsten copper, tungsten nickel, ferrotungsten, tungsten chromium, tungsten vanadium, tungsten titanium, tungsten zirconium, tungsten vanadium chromium, tungsten vanadium copper or tungsten copper iron.
4. The process according to claim 1, characterized in that: the elements of the tungsten-based composite layer (2) are distributed in proportion in the thickness direction.
5. The process according to claim 1, characterized in that: the tungsten-based composite layer (2) is coated on the tungsten sheet (1) by adopting a selective laser melting method, the base material used by the tungsten-based composite layer (2) is tungsten powder, and the other material is copper powder, nickel powder, iron powder, chromium powder, vanadium powder, titanium powder or zirconium powder, or tungsten-vanadium alloy powder, copper-coated tungsten powder, nickel-coated tungsten powder, iron-coated tungsten powder, tungsten-chromium alloy powder, tungsten-vanadium alloy powder, tungsten-titanium alloy powder, tungsten-zirconium alloy powder, tungsten-vanadium-chromium alloy powder, tungsten-vanadium-copper alloy powder or tungsten-copper-iron alloy powder is directly used.
6. The process according to claim 1, characterized in that: the selective laser melting refers to placing and fixing one or more tungsten sheets (1) in a melting chamber, then spreading powder, performing selective melting on each tungsten sheet (1), and performing selective melting for multiple times according to thickness requirements to prepare the tungsten-based composite sheet.
7. The process according to claim 1, characterized in that: in the hot isostatic pressing process, element diffusion can occur to composite elements in the tungsten-based composite layer (2), and meanwhile, some closed gaps in the tungsten-based composite layer (2) can be closed, so that densification of the tungsten-based composite layer (2) is realized.
8. The process according to claim 1, characterized in that: the tungsten sheet (1) is tungsten potassium, tungsten rhenium alloy or zirconium carbide doped tungsten alloy; the external dimension of the tungsten-based composite sheet is determined by design, and the external dimension of the tungsten-based composite sheet is processed after hot isostatic pressing.
9. The process of claim 4, wherein: the atomic fraction of tungsten in the tungsten-based composite layer (2) continuously changes from 100% to 0% in the thickness direction.
10. The process of claim 4, wherein: the tungsten-based composite layer (2) is divided into four layers, and the atomic fraction of tungsten is changed in a gradient manner in the thickness direction.
CN202210051631.0A 2022-01-17 2022-01-17 Process method for preparing tungsten-based composite sheet by combining selective laser melting and hot isostatic pressing technology Pending CN114378304A (en)

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CN115194146A (en) * 2022-07-22 2022-10-18 合肥综合性国家科学中心能源研究院(安徽省能源实验室) Functional gradient layer material suitable for fusion reactor tungsten and steel connection
CN115216720A (en) * 2022-06-13 2022-10-21 深圳大学 Tungsten composite coating applied to first wall of cladding of nuclear fusion device and preparation method thereof
CN117123779A (en) * 2023-07-28 2023-11-28 西安欧中材料科技有限公司 Warhead shell and powder hot isostatic pressing forming method thereof

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CN111889676A (en) * 2020-08-06 2020-11-06 哈尔滨工业大学 Method for preparing diamond copper-based composite material by additive manufacturing process
CN113649594A (en) * 2021-08-13 2021-11-16 东北大学 Hot isostatic pressing method for manufacturing 24CrNiMo alloy steel by laser additive manufacturing

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Publication number Priority date Publication date Assignee Title
CN115216720A (en) * 2022-06-13 2022-10-21 深圳大学 Tungsten composite coating applied to first wall of cladding of nuclear fusion device and preparation method thereof
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CN117123779A (en) * 2023-07-28 2023-11-28 西安欧中材料科技有限公司 Warhead shell and powder hot isostatic pressing forming method thereof

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