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WO2021254480A1 - 镍基高温合金及其制造方法、部件和应用 - Google Patents

镍基高温合金及其制造方法、部件和应用 Download PDF

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Publication number
WO2021254480A1
WO2021254480A1 PCT/CN2021/100852 CN2021100852W WO2021254480A1 WO 2021254480 A1 WO2021254480 A1 WO 2021254480A1 CN 2021100852 W CN2021100852 W CN 2021100852W WO 2021254480 A1 WO2021254480 A1 WO 2021254480A1
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nickel
printing
based superalloy
less
laser
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PCT/CN2021/100852
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English (en)
French (fr)
Inventor
毕中南
张少明
夏天
王睿
曲敬龙
马惠萍
韩寿波
孙广宝
Original Assignee
北京钢研高纳科技股份有限公司
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Priority to ES21825515T priority Critical patent/ES3000633T3/es
Priority to JP2022571333A priority patent/JP7368641B2/ja
Priority to EP21825515.6A priority patent/EP4134459B1/en
Priority to US17/928,472 priority patent/US20230193424A1/en
Publication of WO2021254480A1 publication Critical patent/WO2021254480A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
    • C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
    • C22C19/055—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 20% but less than 30%
    • 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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20—Direct sintering or melting
    • B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
    • 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
    • B22F10/00—Additive manufacturing of workpieces or articles from 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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30—Process control
    • B22F10/36—Process control of energy beam parameters
    • 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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30—Process control
    • B22F10/36—Process control of energy beam parameters
    • B22F10/366—Scanning parameters, e.g. hatch distance or scanning strategy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
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    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/60—Treatment of workpieces or articles after build-up
    • B22F10/64—Treatment of workpieces or articles after build-up by thermal means
    • 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
    • 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
    • B22F3/24—After-treatment of workpieces or articles
    • 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
    • B22F5/04—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of turbine blades
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE 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
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE 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
    • B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
    • B33Y40/20—Post-treatment, e.g. curing, coating or polishing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE 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
    • B33Y50/00—Data acquisition or data processing for additive manufacturing
    • B33Y50/02—Data acquisition or data processing for additive manufacturing for controlling or regulating additive manufacturing processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE 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
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE 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
    • B33Y80/00—Products made by additive manufacturing
    • 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
    • C22C1/0433—Nickel- or cobalt-based alloys
    • 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
    • C22C1/10—Alloys containing non-metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
    • 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • 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
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment
    • 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
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/15—Nickel or cobalt
    • 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
    • B22F2304/00—Physical aspects of the powder
    • B22F2304/10—Micron size particles, i.e. above 1 micrometer up to 500 micrometer
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Definitions

  • the present disclosure relates to the field of alloy technology, and in particular to a nickel-based high-temperature alloy and its manufacturing method, components and applications.
  • Superalloys have good oxidation resistance and corrosion resistance, as well as higher strength at high temperatures, and are key materials for the hot end components of aviation and aerospace power systems. With the continuous development of the aviation and aerospace industries, the design requirements for core components have gradually increased, and more complicated internal runners and thin-walled structures have appeared inside the parts. The high-temperature alloys obtained by the traditional casting forge welding process can no longer meet the design requirements.
  • the purpose of the present disclosure is to provide a nickel-based superalloy and a manufacturing method thereof.
  • the alloy has no cracks on the surface and inside, high high-temperature strength, and still has excellent performance at a temperature of 1100°C, which can meet the requirements of aviation and aerospace.
  • the nickel-based superalloy provided in the present disclosure is prepared by 3D printing using the following raw materials;
  • the raw materials include the following components in mass percentage: C is less than or equal to 0.3%, Co is less than 5%, W is 13-15%, Cr is 20-24%, Mo is 1-3%, Al is 0.2-0.5%, and Ti is less than 0.1% , Fe is less than 3%, B is less than 0.015%, La 0.001-0.004%, Mn 0.01-0.2%, Si 0.02-0.2%, and the balance Ni;
  • the nickel-based superalloy has no cracks; the average carbide size in the structure of the nickel-based superalloy is 150-200nm, and the carbide size distribution is 50nm-4 ⁇ m.
  • the raw material includes the following components in mass percentage:
  • the raw material includes the following components in mass percentage:
  • the carbides in the nickel-based superalloy include primary carbides and secondary carbides
  • the size of the primary carbide is 200nm-4 ⁇ m, and it is located in the area where W and Mo are enriched between dendrites and cellular crystals;
  • the size of the secondary carbide is 50-150nm, partly located at the interface and partly located in the crystal.
  • the 3D printing includes laser selective melting 3D printing or electron beam melting 3D printing, for example, laser selective melting 3D printing.
  • the nickel-based superalloy is prepared by using the following steps: first prepare the raw material into powder with a particle size of 15-75 ⁇ m, and then perform the laser selective melting 3D printing;
  • the laser selective melting and 3D printing is followed by hot isostatic pressing and heat treatment.
  • the yield strength of the nickel-based superalloy at 1100° C. is greater than or equal to 50 MPa;
  • the density of the nickel-based superalloy obtained before hot isostatic pressing is greater than or equal to 99%, and the density of the nickel-based superalloy obtained after hot isostatic pressing is greater than or equal to 99.95 %.
  • the process parameters in the laser selective melting 3D printing process include:
  • the laser scanning speed is 600-2000mm/s
  • the laser spacing is 80-120 ⁇ m
  • the thickness of spreading powder is 20-80 ⁇ m.
  • the present disclosure provides a method for manufacturing a nickel-based superalloy, which includes the following steps:
  • the nickel-based superalloy is prepared by using the raw materials in the aforementioned nickel-based superalloy and adopting 3D printing.
  • the 3D printing includes laser selective melting 3D printing or electron beam melting 3D printing, for example, laser selective melting 3D printing.
  • the raw material is first prepared into powder with a particle size of 15-75 ⁇ m, and then the laser selective melting 3D printing is performed to obtain the nickel-based superalloy;
  • the method includes the following steps: first prepare the raw material into a powder with a particle size of 15-75 ⁇ m, then perform the laser selective melting 3D printing, and then perform hot isostatic pressing and heat treatment to obtain the The nickel-based superalloy;
  • the process parameters in the laser selective melting 3D printing process include:
  • the laser scanning speed is 600-2000mm/s
  • the laser spacing is 80-120 ⁇ m
  • the thickness of spreading powder is 20-80 ⁇ m.
  • the present disclosure provides a component including the above-mentioned nickel-based superalloy or the nickel-based superalloy manufactured by the above-mentioned manufacturing method.
  • the present disclosure provides an aviation, aerospace engine, aircraft, or gas turbine, including the above-mentioned components.
  • the present disclosure can at least achieve the following beneficial effects:
  • a nickel-based high-temperature alloy is prepared by 3D printing, especially a laser selective melting 3D printing method, using materials with specific element composition, which can give the alloy a special structure, so as to obtain a compact, crack-free, and meet the strength requirements in a high-temperature environment. Complex parts.
  • Materials with specific element composition can significantly reduce the crack sensitivity during the selective laser melting forming process in the application of 3D printing methods, especially laser selective melting 3D printing, and can still maintain a non-cracking state under the nickel alloy composition with high carbon content.
  • the obtained alloy has no cracks on the surface and inside, high high-temperature strength, and still has excellent performance when the service temperature is 1100°C.
  • the obtained alloy body has excellent high-temperature performance.
  • Figure 1 is a metallographic structure diagram of a high-temperature alloy sample in Example 1;
  • Figure 2 is a microstructure diagram of a high-temperature alloy sample in Example 1;
  • FIG. 3 is a metallographic structure diagram of an alloy sample of Comparative Example 3.
  • FIG. 3 is a metallographic structure diagram of an alloy sample of Comparative Example 3.
  • the mechanical parts made by the traditional casting, forging and welding process can no longer meet the design requirements of the aerospace industry.
  • 3D printing technology is used.
  • the high-temperature alloy materials currently used in the 3D printing field mainly include IN625, IN718, Hastelloy X and so on.
  • Hastelloy X domestic grade GH3536
  • Inconel 625 domestic grade GH3625
  • Inconel 718 domestic grade GH4169
  • GH3230 alloy is a nickel-based deformed high-temperature alloy.
  • the traditional process route is casting, forging, rolling, etc. It can be used for a long time above 1000°C, surpassing alloys such as IN718, IN625 and HastelloyX.
  • GH3230 alloy also has a certain degree of weldability, so it has the feasibility of 3D printing process.
  • the present disclosure is improved on the basis of the GH3230 alloy composition, so as to better adapt to the special process requirements of 3D printing, and solve the technical problem of cracking, while ensuring the use performance at 1100°C.
  • the present disclosure provides a nickel-based superalloy prepared by 3D printing using the following raw materials; the raw materials include the following components in mass percentage: C is less than or equal to 0.3%, Co is less than 5%, and W is 13-15% , Cr 20-24%, Mo 1-3%, Al 0.2-0.5%, Ti less than 0.1%, Fe less than 3%, B less than 0.015%, La 0.001-0.004%, Mn 0.01-0.2%, Si 0.02-0.2 %, and the balance of Ni; the nickel-based superalloy has no cracks; the average carbide size in the structure of the nickel-based superalloy is 150-200nm, and the carbide size distribution is 50nm-4 ⁇ m.
  • Raw material: C is less than or equal to 0.3% (for example, it can be 0.01%, 0.02%, 0.05%, 0.08%, 0.09%, 0.1%, 0.12%, 0.15%, 0.16%, 0.18%, 0.2%, 0.22%, 0.24%, 0.25%, 0.26%, 0.28% or 0.3%, etc.), Co is less than 5% (for example, it can be 0.01%, 0.1%, 1%, 2%, 3%, 4% or 4.8%, etc.), W 13-15% (For example, it can be 13%, 13.5%, 14%, 14.5%, or 15%, etc.), Cr 20-24% (for example, it can be 20%, 21%, 22%, or 24%, etc.), Mo 1-3% (For example, it can be 1%, 2%, or 3%, etc.), Al 0.2-0.5% (for example, it can be 0.2%, 0.3%, 0.4% or 0.5%, etc.), Ti is less than 0.1% (for example, it can be 0.01%, 0.02 %, 0.03%
  • Ni in the raw material, in addition to other components other than Ni mentioned above, it can also include other optional components (residual components or total impurities).
  • Element that is, in the raw material, the sum of the mass percentages of Ni, other components except Ni, and other optional components is 100%.
  • the Cr plays a solid solution strengthening effect in nickel-based superalloys, and forms an oxide layer on the metal surface at high temperatures to improve the oxidation resistance of the alloy.
  • the Cr content exceeds 24%, it will promote the precipitation of harmful secondary phases, increase the tendency of cracking, and affect the high-temperature mechanical properties of the alloy. Therefore, in the nickel-based superalloy raw materials of the present disclosure, the Cr content is controlled at 20-24%.
  • Al can form a dense oxide film and improve the oxidation resistance of nickel-based superalloys.
  • the Al content is controlled at 0.2-0.5%.
  • W plays a solid solution strengthening effect in nickel-based superalloys.
  • W content exceeding 15% will promote the formation of TCP harmful phases. Therefore, in the nickel-based superalloy raw materials of the present disclosure, the W content is controlled at 13-15%.
  • C can form carbides in nickel-based superalloys and play a high-temperature strengthening effect.
  • excessive C content will cause carbides to precipitate at the grain boundaries and form a continuous carbide film, which is not conducive to the mechanical properties of the alloy. Therefore, the C content of the existing GH3230 alloy is controlled at 0.05-0.15%.
  • the process characteristics of rapid solidification and rapid cooling in the 3D printing process can make carbides tend to form fine, dispersed distributions, which become strengthening phases to improve mechanical properties. Therefore, the upper limit of C content in the nickel-based superalloy raw material of the present disclosure is increased from 0.15% to 0.3%.
  • Si is beneficial to improve the oxidation resistance of the alloy.
  • the Si content in the existing GH3230 alloy is 0.25-0.75%.
  • Si will significantly increase the tendency of cracking, and the content of Si needs to be strictly limited. Therefore, the Si content in the nickel-based superalloy raw materials of the present disclosure is controlled at 0.02-0.2%.
  • Mn is a deoxidizing element and can react with sulfur to form MnS, reducing the harmful effects of sulfur.
  • the Mn content in the existing GH3230 alloy is 0.3-1%. But Mn increases the tendency of printing to crack. Therefore, the Mn content in the nickel-based superalloy raw materials of the present disclosure is controlled at 0.01-0.2%.
  • La element affects the composition and morphology of the oxide film of nickel-based superalloys, and improves the oxidation resistance and high-temperature mechanical properties of nickel-based superalloys.
  • the La content in the existing GH3230 alloy is 0.005-0.05%.
  • the La content in the nickel-based superalloy raw materials of the present disclosure is controlled within 0.001-0.004%.
  • B is a grain boundary strengthening element, and an appropriate amount of B element will increase the grain boundary strength of nickel-based superalloys.
  • the content of B in the nickel-based superalloy raw materials of the present disclosure is controlled to be less than 0.015%.
  • the raw material includes the following components in mass percentage: C 0.05-0.3%, Co less than 5%, W 13-15%, Cr 20-24%, Mo 1-3%, Al 0.2- 0.5%, Ti is less than 0.1%, Fe is less than 3%, B is less than 0.015%, La is 0.001-0.004%, Mn is 0.01-0.1%, Si is 0.02-0.1%, and the balance is Ni.
  • the raw material includes the following components in mass percentage:
  • the raw material is, for example, powder.
  • the 3D printing includes laser selective melting 3D printing or electron beam melting 3D printing, for example, laser selective melting 3D printing.
  • the selective laser fusion (SLM) 3D printing process is a fast 3D printing technology that can melt metal powder layer by layer, and finally realize metal parts without abrasive tools, high density, and near net shape.
  • Laser selective melting technology has the characteristics of high forming efficiency and can prepare complex structure parts, and it has become the most potential preparation technology for complex structure superalloy parts.
  • the nickel-based superalloy is prepared by adopting the following steps: firstly prepare the above-mentioned raw materials into powder with a particle size of 15-75 ⁇ m, and then perform laser selective melting 3D printing. In one or more embodiments, hot isostatic pressing and heat treatment are performed after laser selective melting and 3D printing to obtain a nickel-based superalloy.
  • the process parameters in the laser selective melting 3D printing process include:
  • Laser power 100-700W such as 100W, 200W, 300W, 400W, 500W, 600W or 700W;
  • the spot diameter is 40-110 ⁇ m, such as 40 ⁇ m, 50 ⁇ m, 60 ⁇ m, 70 ⁇ m, 80 ⁇ m, 90 ⁇ m, 100 ⁇ m or 110 ⁇ m;
  • the laser pitch is 80-120 ⁇ m, such as 80 ⁇ m, 90 ⁇ m, 100 ⁇ m, 110 ⁇ m or 120 ⁇ m;
  • the thickness of spreading powder is 20-80 ⁇ m, for example, 20 ⁇ m, 30 ⁇ m, 40 ⁇ m, 50 ⁇ m, 60 ⁇ m, 70 ⁇ m or 80 ⁇ m.
  • the SLM process parameters are selected so that the laser volume energy density E v during the laser selective melting of the present disclosure is in the range of 50-100 J/mm 3.
  • E v is calculated as follows:
  • P is the laser power
  • V is the laser scanning speed
  • H is the laser distance
  • t is the thickness of the powder.
  • the laser volume energy density E v is maintained within the range of 50-100 J/mm 3 during laser selective melting. If it is not within this range, a large number of holes and defects will be formed in the alloy, resulting in Decline in alloy performance.
  • the raw materials used in the nickel-based superalloy of the present disclosure control the content of Si, Mn and La in the composition, making it particularly suitable for laser selective melting 3D printing, which significantly reduces crack sensitivity during selective laser melting forming; in addition; , While the crack sensitivity is significantly reduced, the C content in the raw material is also high, the high temperature strength is high, and it still has excellent performance at a service temperature of 1100°C.
  • the alloy product after printing can still be kept from cracking under the nickel alloy component with high carbon content.
  • the nickel-based superalloy formed by 3D printing with the above-mentioned raw material composition has no cracks on the surface and inside.
  • the carbide size is significantly smaller and the distribution is more dispersed.
  • the average carbide size is 150-200nm (e.g. 160, 170, 180, 190nm), and the carbide size distribution is 50nm-4 ⁇ m (e.g. including 50-100nm, 50-150nm, 50-200nm, 300nm-4 ⁇ m, 300nm-2 ⁇ m , 500nm-2 ⁇ m, 200nm-3 ⁇ m, etc.).
  • the typical microstructure in the nickel-based superalloy include primary carbides and secondary carbides;
  • the primary carbide size is 200nm-4 ⁇ m (for example, it can also be 200nm-1 ⁇ m, 200nm-2 ⁇ m, 200nm-3 ⁇ m, 300nm-1 ⁇ m, 300nm-2 ⁇ m, 300nm-3 ⁇ m, 300nm-4 ⁇ m, 400nm-1 ⁇ m, 400nm-2 ⁇ m, 400nm -3 ⁇ m, 400nm-4 ⁇ m, 500nm-1 ⁇ m, 500nm-2 ⁇ m, 500nm-3 ⁇ m, 500nm-4 ⁇ m), located in the area where W and Mo are enriched between dendrites and cellular crystals;
  • the size of the secondary carbide is 50-150nm (for example, it can also be 50-100nm, 60-120nm, 70-130nm, 80-140nm, 90-150nm, 100-150nm), partly located at the interface and partly located in the crystal.
  • the nickel-based superalloy of the present disclosure is proposed based on the applicability in the 3D printing process and the problem of printing cracking.
  • the alloy raw materials are optimized and improved on the basis of the original GH3230 alloy composition to have good weldability. There is almost no cracking phenomenon during laser selective melting 3D printing, and the high temperature strength is high.
  • an alloy product with high density, no cracks, and high strength in a high temperature environment is obtained.
  • the yield strength of the nickel-based superalloy of the present disclosure at high temperature (1100° C.) is greater than or equal to 50 MPa (for example, 55 MPa, 56 MPa, 58 MPa, 60 MPa).
  • the yield strength is measured by the metal material tensile test method (GB/T 228.1-2010).
  • the elongation after fracture of the nickel-based superalloy of the present disclosure at room temperature is greater than or equal to 16%.
  • the elongation after fracture is measured by the metal material tensile test method (GB/T 228.1-2010).
  • the density of the nickel-based superalloy obtained before hot isostatic pressing is greater than or equal to 99%, and the density of the nickel-based superalloy obtained after hot isostatic pressing is greater than or equal to 99.95%.
  • the density is measured by GB/T 3850-2015 "Density Measurement Method for Dense Sintered Metal Materials and Cemented Carbide”.
  • the present disclosure provides a method for manufacturing a nickel-based superalloy, which includes the following steps: preparing the nickel-based superalloy by 3D printing using the raw materials in the above-mentioned nickel-based superalloy.
  • the method disclosed in the present disclosure selects materials with a specific element composition, and obtains a nickel-based superalloy through 3D printing.
  • the proposed method provides a new way to obtain dense, excellent high-temperature performance, crack-free alloy parts.
  • 3D printing includes laser selective melting 3D printing or electron beam melting 3D printing, for example, laser selective melting 3D printing.
  • the raw material is first prepared into powder with a particle size of 15-75 ⁇ m, and then the laser selective melting 3D printing is performed to obtain the nickel-based superalloy;
  • the method includes the following steps: first prepare the raw material into a powder with a particle size of 15-75 ⁇ m, then perform the laser selective melting 3D printing, and then perform hot isostatic pressing to obtain the density after hot isostatic pressing >99.95% of nickel-based superalloy, after heat treatment to obtain the required mechanical properties.
  • the process parameters in the laser selective melting 3D printing process include:
  • the laser scanning speed is 600-2000mm/s
  • the laser spacing is 80-120 ⁇ m
  • the thickness of spreading powder is 20-80 ⁇ m.
  • the nickel-based superalloy obtained by the manufacturing method has the same microstructure and properties as the nickel-based superalloy of the first aspect.
  • the size of carbides in the nickel-based superalloy formed by laser selective melting and 3D printing is significantly smaller and the distribution is more dispersed.
  • the application of the material with the specific element composition of the nickel-based superalloy of the present disclosure to the method disclosed in the present disclosure makes the manufactured parts less prone to cracking and has excellent performance.
  • the present disclosure provides a component including the above-mentioned nickel-based superalloy or the nickel-based superalloy manufactured by the above-mentioned manufacturing method.
  • the part has no cracks on the surface and inside, high density, high high temperature strength, and meets the needs of aviation and aerospace applications.
  • Typical but non-limiting components are engine intake ducts, flame tubes, heat shields, etc.
  • the present disclosure provides an aviation, aerospace engine, aircraft, or gas turbine, including the above-mentioned components.
  • the raw material of nickel-based superalloy for 3D printing includes the following components by mass percentage:
  • the nickel-based superalloy raw material for 3D printing described in Example 1 was prepared into 15-75 ⁇ m powder, and the superalloy sample was prepared by laser selective melting technology (SLM). During the printing process, 240W laser power and 1000mm/s laser were used. Scanning speed, 100 ⁇ m spot diameter, 90 ⁇ m laser spacing, 30 ⁇ m spreading thickness.
  • SLM laser selective melting technology
  • the high-temperature alloy sample has a uniform, compact and crack-free metallographic structure, and the density test result is 99.2%.
  • the microstructure of the superalloy sample is shown in Figure 2.
  • the grains are distributed in long cells along the deposition direction, a large number of carbide particles are precipitated on the grain boundaries (including the cell boundaries), and there are fine carbides uniformly distributed inside the grains.
  • the carbides in the superalloy samples mainly include primary carbides with a large size (200nm-4 ⁇ m), which are precipitated from the liquid phase during the solidification process, and are mostly located in the dendrite/cellular crystal interstitial area where W, Mo and other elements are enriched; in addition, There are also secondary carbides precipitated in the solid phase, which are relatively small (50-150nm), partly located at the interface, and partly located in the crystal.
  • the size of carbides in the alloys formed by 3D printing is significantly smaller and the distribution is more dispersed.
  • the average carbide size is 150-200nm, the smallest reaches tens of nm, and the largest does not exceed 5 ⁇ m.
  • carbide has a higher hardness than austenite matrix, especially when the interface is continuously distributed, it may reduce the bonding force of the material interface and affect the mechanical properties of the alloy.
  • the size of the discontinuous distribution Smaller carbides will instead have a strengthening effect.
  • the preparation method of the casting alloy sample is as follows: using the composition of the above-mentioned nickel-based superalloy raw material for 3D printing for casting, specifically including the following steps:
  • the yield strength of the 3D printed superalloy sample is higher than that of the cast alloy sample at different temperatures. To be higher.
  • Example 2 The mass percentages of the components of the nickel-based superalloy raw materials for 3D printing in Examples 2-4 are shown in Table 2, and the others are the same as in Example 1.
  • the alloy raw materials of Examples 2-4 and Comparative Examples 1-3 were prepared into 15-75 ⁇ m powder, and the same selective laser melting technology (SLM) as in Example 1 was used to prepare alloy samples (wherein, the alloy samples of Comparative Example 3 were used
  • SLM selective laser melting technology
  • the metallographic structure of the alloy sample prepared by the alloy powder is shown in Figure 3.
  • the metallographic structure has a large number of microcracks).
  • the yield strength of each alloy sample at room temperature (25°C) is shown in Table 4 below:

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Abstract

本公开提供了一种镍基高温合金及其制造方法、部件和应用，涉及合金技术领域，镍基高温合金采用如下原料经3D打印制备得到；原料包括(质量百分比)：C小于等于0.3％，Co小于5％，W 13-15％，Cr 20-24％，Mo 1-3％，Al 0.2-0.5％，Ti小于0.1％，Fe小于3％，B小于0.015％，La 0.001-0.004％，Mn 0.01-0.2％，Si 0.02-0.2％，以及余量的Ni；组织中平均碳化物尺寸150-200nm，碳化物尺寸分布50nm-4μm。该合金表面及内部无裂纹，高温强度高，在温度为1100℃时仍具有优良的性能，可以满足航空、航天的使用要求。

Description

镍基高温合金及其制造方法、部件和应用
相关申请的交叉引用
本公开要求于2020年6月19日提交中国专利局的申请号为202010571208.4、名称为“镍基高温合金及其制造方法、部件和应用”的中国专利申请的优先权，其全部内容通过引用结合在本公开中。
技术领域
本公开涉及合金技术领域，尤其是涉及一种镍基高温合金及其制造方法、部件和应用。
背景技术
高温合金具有良好的抗氧化性和耐腐蚀性能，以及高温下较高的强度，是航空、航天动力系统热端部件的关键材料。随着航空、航天产业的不断发展，核心部件设计要求的逐步提升，零件内部出现了较多的复杂内流道及薄壁结构，传统铸锻焊工艺得到的高温合金已无法满足设计要求。
发明内容
本公开的目的在于提供一种镍基高温合金及其制造方法，该合金表面及内部无裂纹，高温强度高，在温度为1100℃时仍具有优良的性能，可以满足航空、航天的使用要求。
第一方面，本公开提供的镍基高温合金，采用如下原料经3D打印制备得到；
所述原料包括质量百分比的如下组分：C小于等于0.3％，Co小于5％，W 13-15％，Cr 20-24％，Mo 1-3％，Al 0.2-0.5％，Ti小于0.1％，Fe小于3％，B小于0.015％，La 0.001-0.004％，Mn 0.01-0.2％，Si 0.02-0.2％，以及余量的Ni；
所述镍基高温合金无裂纹；所述镍基高温合金的组织中平均碳化物尺寸大小为150-200nm，碳化物尺寸分布为50nm-4μm。
在一种或多种实施方式中，所述原料包括质量百分比的如下组分：
C 0.05-0.3％，Co小于5％，W 13-15％，Cr 20-24％，Mo 1-3％，Al 0.2-0.5％，Ti小于0.1％，Fe小于3％，B小于0.015％，La 0.001-0.004％，Mn 0.01-0.1％，Si 0.02-0.1％，以及余量的Ni。
在一种或多种实施方式中，所述原料包括质量百分比的如下组分：
C 0.08-0.25％，Co小于5％，W 13-15％，Cr 20-24％，Mo 1-3％，Al 0.2-0.5％，Ti小于0.1％，Fe小于3％，B小于0.015％，La 0.001-0.004％，Mn 0.01-0.06％，Si 0.02-0.06％，以及余量的Ni。
在一种或多种实施方式中，所述镍基高温合金中的碳化物包括一次碳化物，以及二次碳化物；
一次碳化物尺寸为200nm-4μm，位于枝晶和胞状晶间富集W、Mo元素区域；
二次碳化物尺寸为50-150nm，部分位于界面，部分位于晶内。
在一种或多种实施方式中，所述3D打印包括激光选区熔融3D打印或电子束熔融3D打印，例如激光选区熔融3D打印。
在一种或多种实施方式中，所述镍基高温合金采用如下步骤制备得到：先将所述原料制备成粒径为15-75μm的粉末再进行所述激光选区熔融3D打印；
在一种或多种实施方式中，所述激光选区熔融3D打印后进行热等静压和热处理。
在一种或多种实施方式中，所述镍基高温合金在1100℃下的屈服强度大于等于50MPa；
在一种或多种实施方式中，热等静压前得到的所述镍基高温合金的致密度大于等于99％，热等静压后得到的所述镍基高温合金的致密度大于等于99.95％。
在一种或多种实施方式中，所述激光选区熔融3D打印过程中的工艺参数包括：
(a)激光功率100-700W；
(b)激光扫描速度600-2000mm/s；
(c)光斑直径40-110μm；
(d)激光间距80-120μm；
(e)铺粉厚度20-80μm。
第二方面，本公开提供了一种镍基高温合金的制造方法，包括以下步骤：
利用上述镍基高温合金中的所述原料并采用3D打印制备得到所述镍基高温合金。
在一种或多种实施方式中，所述3D打印包括激光选区熔融3D打印或电子束熔融3D打印，例如激光选区熔融3D打印。
在一种或多种实施方式中，先将所述原料制备成粒径为15-75μm的粉末再进行所述激光选区熔融3D打印，得到所述镍基高温合金；
在一种或多种实施方式中，包括以下步骤：先将所述原料制备成粒径为15-75μm的粉末再进行所述激光选区熔融3D打印，然后进行热等静压和热处理，得到所述镍基高温合金；
在一种或多种实施方式中，所述激光选区熔融3D打印过程中的工艺参数包括：
(a)激光功率100-700W；
(b)激光扫描速度600-2000mm/s；
(c)光斑直径40-110μm；
(d)激光间距80-120μm；
(e)铺粉厚度20-80μm。
第三方面，本公开提供了一种部件，包括上述镍基高温合金或上述制造方法制造的镍基高温合金。
第四方面，本公开提供了一种航空、航天发动机、飞行器或燃气轮机，包括上述部件。
与现有技术相比，本公开至少可以取得以下有益效果：
本公开采用特定元素组成的材料经3D打印特别是激光选区熔融3D打印方法制备得到镍基高温合金，能够赋予该合金特殊的组织结构，从而获得致密的、无裂纹的、满足高温环境下强度需求的复杂零部件。
特定元素组成的材料在应用3D打印方法特别是激光选区熔融3D打印中能显著降低其在选区激光熔融成形过程中裂纹敏感性，在高碳含量的镍合金组分下仍能够保持不开裂状态，获得合金表面及内部无裂纹，高温强度高，在服役温度为1100℃时仍具有优良的性能。
此外，在一种或多种实施方式中，采用与合金材料相匹配的工艺参数，获得的合金体高温性能优异。
附图说明
图1为实施例1中的高温合金试样的金相组织图；
图2为实施例1中的高温合金试样的微观结构图；
图3为对比例3的合金试样的金相组织图。
具体实施方式
为使本公开实施例的目的、技术方案和优点更加清楚，下面将结合本公开实施例中的附图，对本公开实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例是本公开一部分实施例，而不是全部的实施例。通常在此处附图中描述和示出的本公开实施例的组件可以以各种不同的配置来布置和设计。
传统铸锻焊工艺制作的机械零部件已无法满足航空航天领域的设计要求。为了提升机械零部件的性能，利用3D打印技术。
在将3D打印技术推广到高性能高温合金时，发现虽然现有高性能高温合金种类繁多，但均是针对传统制备工艺而研发的。为了保证可打印性，目前用于3D打印领域的高温合金材料主要包括IN625、IN718、Hasttelloy X等。目前，Hastelloy X(国内牌号GH3536)、Inconel 625(国内牌号GH3625)和Inconel 718(国内牌号GH4169)三个牌号的高温合金经过研究优化，已经有较为成熟的打印工艺技术，被用于航空、航天发动机燃烧室等部件。
GH3230合金作为一种镍基变形高温合金，传统工艺路线为铸造、锻造、轧制等，可在1000℃以上长期使用，超越了IN718、IN625和HastelloyX等合金。GH3230合金同时拥有一定的可焊接性，因此具备了3D打印工艺可行性。
发明人发现，GH3230合金在3D打印特殊工艺条件下，尤其是进行复杂结构制备时，打印后的部件易出现裂纹缺陷。
本公开是在GH3230合金成分的基础上进行改进，以更好适应3D打印特殊工艺要求，且解决开裂的技术问题，同时保证1100℃使用性能。
一个方面，本公开提供了一种镍基高温合金，采用如下原料经3D打印制备得到；所述原料包括质量百分比的如下组分：C小于等于0.3％，Co小于5％，W 13-15％，Cr 20-24％，Mo 1-3％，Al 0.2-0.5％，Ti小于0.1％，Fe小于3％，B小于0.015％，La 0.001-0.004％，Mn 0.01-0.2％，Si 0.02-0.2％，以及余量的Ni；所述镍基高温合金无裂纹；所述镍基高温合金的组织中平均碳化物尺寸大小为150-200nm，碳化物尺寸分布为50nm-4μm。
原料：C小于等于0.3％(例如可以为0.01％、0.02％、0.05％、0.08％、0.09％、0.1％、0.12％、0.15％、0.16％、0.18％、0.2％、0.22％、0.24％、0.25％、0.26％、0.28％或者0.3％等)，Co小于5％(例如可以为0.01％、0.1％、1％、2％、3％、4％或者4.8％等)，W 13-15％(例如可以为13％、13.5％、14％、14.5％、或者15％等)，Cr 20-24％(例如可以为20％、21％、22％或者24％等)，Mo 1-3％(例如可以为1％、2％或者3％等)，Al 0.2-0.5％(例如可以为0.2％、0.3％、0.4％或者0.5％等)，Ti小于0.1％(例如可以为0.01％、0.02％、0.03％、0.04％、0.05％、0.06％、0.07％、0.08％或者0.09％等)，Fe小于3％(例如可以为0.01％、0.1％、0.5％、1％、1.5％、2％、2.5％、或者2.9％等)，B小于0.015％(例如可以为0.001％、0.002％、0.005％、0.008％、0.01％或者0.014％等)，La 0.001-0.004％(例如可以为0.001％、0.002％、0.003％或者0.004％等)，Mn 0.01-0.2％(例如可以为0.01％、0.02％、0.03％、0.04％、0.05％、0.06％、0.08％、0.1％、0.12％、0.15％、0.16％、0.18％或者0.2％等)，Si 0.02-0.2％(例如可以为0.02％、0.05％、0.06％、0.08％、0.1％、0.12％、0.15％、0.16％、0.18％或者0.2％等)，以及余量的Ni。
需要说明的是，余量的Ni指的是在原料中，除了包括如上所提及的除Ni之外的其他组分之外，还可以包括其他任选地组分(残余成分或杂质的总元素)，也就是说，在原料中，Ni、除Ni之外的其他组分以及其他任选地组分的质量百分比之和为100％。
Cr在镍基高温合金中起固溶强化效果，高温下在金属表面形成氧化层提高合金抗氧化性能。但是，若Cr含量超过24％则会促进有害二次相析出，增加开裂倾向，并对合金高温力学性能造成影响。因此，本公开镍基高温合金原料中，Cr含量控制在20-24％。
Al可以形成致密的氧化膜，提高镍基高温合金的抗氧化性。在本公开镍基高温合金原料中，Al含量控制在0.2-0.5％。
W在镍基高温合金中起到固溶强化作用。但W含量超过15％则会促进TCP有害相的形成。因此，在本公开镍基高温合金原料中，W含量控制在13-15％。
C在镍基高温合金中可以形成碳化物，起到高温强化作用。但是，传统铸锻工艺制备后，过高C含量会导致碳化物在晶界析出并形成连续碳化膜，不利于合金的力学性能，因此现有GH3230合金C含量控制在0.05-0.15％。但是3D打印过程中快速凝固快速冷却的工艺特性，能够使碳化物倾向于形成细小、弥散分布物，成为强化相提高力学性能。因此，本公开的镍基高温合金原料中C含量上限从0.15％提高至0.3％。
Si有利于提高合金抗氧化性能。在现有GH3230合金中Si含量为0.25-0.75％。但在3D打印工艺工程中，Si会显著增加开裂倾向，需严格限制Si的含量。因此，本公开的镍基高温合金原料中Si含量控制在0.02-0.2％。
Mn是脱氧元素，并且可以和硫反应形成MnS，减轻硫的有害作用。在现有GH3230合金中Mn含量为0.3-1％。但是Mn会增加打印开裂的倾向。因此，本公开的镍基高温合金原料中Mn含量控制在0.01-0.2％。
La元素影响镍基高温合金氧化膜组成和形貌，改善镍基高温合金的抗氧化性能和高温力学性能。在现有GH3230合金中La含量为0.005-0.05％。但是在3D打印工艺过程中，会产生偏析或形成镧化物，增加开裂倾向。因此，本公开的镍基高温合金原料中La含量控制在0.001-0.004％。
B是晶界强化元素，适量的B元素会提高镍基高温合金晶界强度。但B含量高于0.015％时，则形成的大量硼化物不利于合金力学性能，同时产生的低熔点硼化物也会增加打印开裂倾向。因此，本公开的镍基高温合金原料中B含量控制在小于0.015％。
在一些典型实施方式中，所述原料包括质量百分比的如下组分：C 0.05-0.3％，Co小于5％，W 13-15％，Cr 20-24％，Mo 1-3％，Al 0.2-0.5％，Ti小于0.1％，Fe小于3％，B小于0.015％，La 0.001-0.004％，Mn 0.01-0.1％，Si 0.02-0.1％，以及余量的Ni。
在一些更典型实施方式中，所述原料包括质量百分比的如下组分：
C 0.08-0.25％，Co小于5％，W 13-15％，Cr 20-24％，Mo 1-3％，Al 0.2-0.5％，Ti小于0.1％，Fe小于3％，B小于0.015％，La 0.001-0.004％，Mn 0.01-0.06％，Si 0.02-0.06％，以及余量的Ni。
所述原料例如为粉末。
在一种或多种实施方式中，所述3D打印包括激光选区熔融3D打印或电子束熔融3D打印，例如激光选区熔融3D打印。
激光选区熔融(SLM)3D打印工艺是一种可以逐层熔化金属粉末，最终实现金属零件无磨具、高致密度、近净成形的快速3D打印技术。激光选区熔化技术具有成形效率高，可制备复杂结构零件的特点，已成为复杂结构高温合金零部件最具潜力的制备技术。
具体的，镍基高温合金采用如下步骤制备得到：先将上述原料制备成粒径为15-75μm的粉末再进行激光选区熔融3D打印。在一种或多种实施方式中，在激光选区熔融3D打印后进行热等静压和热处理，获得镍基高温合金。
在一种或多种实施方式中，激光选区熔融3D打印过程中的工艺参数包括：
(a)激光功率100-700W，例如100W、200W、300W、400W、500W、600W或700W；
(b)激光扫描速度600-2000mm/s，例如600mm/s、700mm/s、800mm/s、900mm/s、1000mm/s、1200mm/s、1500mm/s、1800mm/s或2000mm/s；
(c)光斑直径40-110μm，例如40μm、50μm、60μm、70μm、80μm、90μm、100μm或110μm；
(d)激光间距80-120μm，例如80μm、90μm、100μm、110μm或120μm；
(e)铺粉厚度20-80μm，例如20μm、30μm、40μm、50μm、60μm、70μm或80μm。
SLM工艺参数经选择使得本公开的激光选区熔融期间激光体积能量密度E v在50-100J/mm 3范围内。E v计算如下：
Figure PCTCN2021100852-appb-000001
其中P为激光功率，V为激光扫描速度，H为激光间距，t为铺粉厚度。
通过这四个工艺参数的相互配合，使得激光选区熔融期间激光体积能量密度E v保持在50-100J/mm 3范围内，如果不在此范围内，会造成合金内部形成大量的孔洞以及缺陷，导致合金性能的下降。
本公开镍基高温合金所使用的原料通过控制成分中的Si，Mn和La的含量，使得其尤其适用于激光选区熔融3D打印，使其在选区激光熔融成形过程中裂纹敏感性显著降 低；另外，裂纹敏感性显著降低的同时原料中C含量也较高，高温强度高，在服役温度为1100℃时仍具有优良的性能。
本公开通过各组分含量的相互配合，在高碳含量的镍合金组分下仍能够保持打印后的合金产品不开裂。
采用上述原料成分经3D打印成型的镍基高温合金表面及内部无裂纹，相比于铸锻态GH3230合金，其中的碳化物尺寸明显更小，分布更弥散。
平均碳化物尺寸大小为150-200nm(例如160、170、180、190nm)，碳化物尺寸分布为50nm-4μm(例如包括50-100nm、50-150nm、50-200nm、300nm-4μm、300nm-2μm、500nm-2μm、200nm-3μm等)。
在一种或多种实施方式中，所述镍基高温合金中典型的微观组织结构：碳化物包括一次碳化物，以及二次碳化物；
一次碳化物尺寸为200nm-4μm(例如还可以为200nm-1μm、200nm-2μm、200nm-3μm、300nm-1μm、300nm-2μm、300nm-3μm、300nm-4μm、400nm-1μm、400nm-2μm、400nm-3μm、400nm-4μm、500nm-1μm、500nm-2μm、500nm-3μm、500nm-4μm)，位于枝晶和胞状晶间富集W、Mo元素区域；
二次碳化物尺寸为50-150nm(例如还可以为50-100nm、60-120nm、70-130nm、80-140nm、90-150nm、100-150nm)，部分位于界面，部分位于晶内。
本公开的镍基高温合金是根据在3D打印过程中的适用性以及所存在的打印开裂问题所提出的。合金原料在原始GH3230合金成分基础上通过优化改进使其拥有良好的可焊接性，在激光选区熔融3D打印时几乎不会出现开裂现象，且高温强度高。在一种或多种实施方式中，通过打印过程中各工艺参数之间以及与原料成分间的相互配合，获得致密度高、无裂纹、高温环境下强度高的合金产品。
典型的，本公开的镍基高温合金在高温下(1100℃)的屈服强度大于等于50MPa(例如55MPa、56MPa、58MPa、60MPa)。
屈服强度是采用金属材料拉伸试验方法(GB/T 228.1-2010)测试得到的。
典型的，本公开的镍基高温合金在室温下的断后伸长率大于等于16％。
断后伸长率是采用金属材料拉伸试验方法(GB/T 228.1-2010)测试得到的。
典型的，热等静压前得到的所述镍基高温合金的致密度大于等于99％，热等静压后得到的所述镍基高温合金的致密度大于等于99.95％。
致密度是采用GB/T 3850-2015《致密烧结金属材料与硬质合金密度测定方法》测试得到的。
另一方面，本公开提供了一种镍基高温合金的制造方法，包括以下步骤：利用上述 镍基高温合金中的所述原料并采用3D打印制备得到所述镍基高温合金。
本公开公开的方法选择特定元素组成的材料，通过3D打印获得镍基高温合金。该方法的提出提供了能够获得致密、优良高温性能、无裂纹合金部件的新方式。
在一些实施方式中，3D打印包括激光选区熔融3D打印或电子束熔融3D打印，例如激光选区熔融3D打印。
在一些实施方式中，先将所述原料制备成粒径为15-75μm的粉末再进行所述激光选区熔融3D打印，得到所述镍基高温合金；
在一些实施方式中，包括以下步骤：先将所述原料制备成粒径为15-75μm的粉末再进行所述激光选区熔融3D打印，然后进行热等静压，得到热等静压后致密度>99.95％的镍基高温合金，后经热处理获得所需力学性能。
在一些实施方式中，所述激光选区熔融3D打印过程中的工艺参数包括：
(a)激光功率100-700W；
(b)激光扫描速度600-2000mm/s；
(c)光斑直径40-110μm；
(d)激光间距80-120μm；
(e)铺粉厚度20-80μm。
制造方法中关于各术语的描述与第一方面镍基高温合金中的对应描述内容一致，在此不再赘述。
制造方法获得的镍基高温合金具有与第一方面的镍基高温合金相同的组织形态和性能。相比于铸锻态GH3230合金，利用激光选区熔融3D打印成型的镍基高温合金中碳化物尺寸明显更小，分布更弥散。将本公开镍基高温合金的特定元素组成的材料应用于本公开公开的方法中使得制造的部件不容易开裂，具有优异的性能。
另一方面，本公开提供了一种部件，包括上述镍基高温合金或上述制造方法制造的镍基高温合金。
由此，该部件表面及内部无裂纹，致密度高，高温强度高，满足航空、航天使用需求。
部件典型但非限制性的例如为发动机的进气道、火焰筒、隔热屏等。
另一方面，本公开提供了一种航空、航天发动机、飞行器或燃气轮机，包括上述部件。
可以理解的是，航空、航天发动机、飞行器或燃气轮机具有与本公开镍基高温合金以及部件相同的优势，在此不再赘述。
下面结合具体实施方式，对本公开的一些实施方式作详细说明。在不冲突的情况下，下述的实施例及实施例中的特征可以相互组合。实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。
实施例1
3D打印用镍基高温合金原料包括具有以下质量百分比组分：
C 0.3％，Cr 22％，W 14％，Mo 2％，Fe 0.5％，Al 0.4％，Ti 0.01％，Si 0.02％，Mn 0.01％，B 0.01％，La 0.001％，以及余量的Ni。
将实施例1所述的3D打印用镍基高温合金原料制备成15-75μm的粉末，用激光选区熔融技术(SLM)制备得到高温合金试样，打印过程中使用240W激光功率，1000mm/s激光扫描速度，100μm光斑直径，90μm激光间距，30μm铺粉厚度。
对制备得到的高温合金试样进行金相组织观察及致密度检测。
如图1所示，高温合金试样得到均匀致密无裂纹的金相组织，致密度检测结果为99.2％。
高温合金试样的微观结构如图2所示，晶粒沿沉积方向呈长胞状分布，晶界(包括胞界)上析出大量的碳化物颗粒，晶粒内部还有细小的碳化物均匀分布。高温合金试样中的碳化物主要包括一次碳化物，尺寸较大(200nm-4μm)，为凝固过程中由液相析出，多位于枝晶/胞状晶间富集W、Mo等元素区域；另外还有固相析出的二次碳化物，相对细小(50-150nm)，部分位于界面，也有部分位于晶内。
相对铸锻态合金，3D打印成型的合金中碳化物尺寸明显更小，分布更弥散。平均碳化物尺寸大小为150-200nm，最小的达到几十nm，最大的不超过5μm。
通常情况下碳化物具有比奥氏体基体更高的硬度，特别是在界面连续分布时有可能会降低材料界面的结合力，影响合金的力学性能，在本实施例中，不连续分布的尺寸较小碳化物反而会起到强化作用。
本实施例的3D打印高温合金试样以及利用上述的镍基高温合金的原料采用铸造方法制备得到的铸造合金试样在室温(25℃)及高温下的拉伸性能见下表1：
铸造合金试样的制备方法如下：采用上述的3D打印用镍基高温合金原料的组成进行铸造，具体包括以下步骤：
(1)按成分配比称取高纯度的Co、Al、W、Ti、Ni、Fe、Cr、Mo、C、B、Mn、Si、La等单质材料；
(2)将Co、Ni、Cr等熔点相对较低的元素单质放置在坩埚底部，其上放置W、Mo等难熔元素，Al、Ti、B等元素放入料斗中，以便在熔炼过程中加入；
(3)采用真空感应炉进行熔炼。首先小功率(约120kW)送电加热排除原料上的附着气体，随后大功率(约200kW)快速升温到1500℃以上，保温10分钟，然后降低温度至1300～1400℃左右，保温5分钟，加入料斗中的Al、Ti、B等元素，升温至1500℃以上，保温15分钟后浇铸成高温合金铸锭。
表1
Figure PCTCN2021100852-appb-000002
如表1所示，对比本实施例铸造合金试样和3D打印高温合金试样在室温及高温下的拉伸性能，3D打印高温合金试样的屈服强度在不同温度下均比铸造合金试样要高。
实施例2-4
实施例2-4中3D打印用镍基高温合金原料的各组分质量百分比如表2所示，其他同实施例1。
表2
  C Co W Cr Mo Al Ti Fe B La Mn Si Ni
实施例2 0.08 - 13 20 1 0.2 0.1 3 0.015       余量
实施例3 0.3 - 15 24 3 0.5 - - - 0.004 0.2 0.2 余量
实施例4 0.08 - 14 22 2 0.3 0.1 3 0.013 0.004 0.2 0.2 余量
对比例1-3
对比例1-3中3D打印用镍基高温合金原料的各组分质量百分比如表3所示，其他同实施例1。
表3
Figure PCTCN2021100852-appb-000003
将实施例2-4以及对比例1-3的合金原料制备成15-75μm的粉末，用与实施例1相 同的选区激光熔融技术(SLM)制备得到合金试样(其中，利用对比例3的合金粉末制备得到的合金试样的金相组织图见图3，其金相组织存在大量微裂纹)，各个合金试样在室温(25℃)下的屈服强度见下表4：
表4
Figure PCTCN2021100852-appb-000004
最后应说明的是：以上各实施例仅用以说明本公开的技术方案，而非对其限制；尽管参照前述各实施例对本公开进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分或者全部技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本公开各实施例技术方案的范围。

Claims (17)

  1. 一种镍基高温合金，其特征在于，采用如下原料经3D打印制备得到；
    所述原料包括质量百分比的如下组分：C小于等于0.3％，Co小于5％，W 13-15％，Cr 20-24％，Mo 1-3％，Al 0.2-0.5％，Ti小于0.1％，Fe小于3％，B小于0.015％，La 0.001-0.004％，Mn 0.01-0.2％，Si 0.02-0.2％，以及余量的Ni；
    所述镍基高温合金无裂纹；所述镍基高温合金的组织中平均碳化物尺寸大小为150-200nm，碳化物尺寸分布为50nm-4μm；
    所述镍基高温合金中的碳化物包括一次碳化物，以及二次碳化物；
    一次碳化物尺寸为200nm-4μm，位于枝晶和胞状晶间富集W、Mo元素区域；
    二次碳化物尺寸为50-150nm，部分位于界面，部分位于晶内。
  2. 根据权利要求1所述的镍基高温合金，其特征在于，所述原料包括质量百分比的如下组分：
    C 0.05-0.3％，Co小于5％，W 13-15％，Cr 20-24％，Mo 1-3％，Al 0.2-0.5％，Ti小于0.1％，Fe小于3％，B小于0.015％，La 0.001-0.004％，Mn 0.01-0.1％，Si 0.02-0.1％，以及余量的Ni。
  3. 根据权利要求1所述的镍基高温合金，其特征在于，所述原料包括质量百分比的如下组分：
    C 0.08-0.25％，Co小于5％，W 13-15％，Cr 20-24％，Mo 1-3％，Al 0.2-0.5％，Ti小于0.1％，Fe小于3％，B小于0.015％，La 0.001-0.004％，Mn 0.01-0.06％，Si 0.02-0.06％，以及余量的Ni。
  4. 根据权利要求1所述的镍基高温合金，其特征在于，所述3D打印包括激光选区熔融3D打印或电子束熔融3D打印。
  5. 根据权利要求4所述的镍基高温合金，其特征在于，所述3D打印为激光选区熔融3D打印。
  6. 根据权利要求5所述的镍基高温合金，其特征在于，镍基高温合金采用如下步骤制备得到：先将所述原料制备成粒径为15-75μm的粉末再进行所述激光选区熔融3D打印。
  7. 根据权利要求6所述的镍基高温合金，其特征在于，所述激光选区熔融3D打印后进行热等静压和热处理。
  8. 根据权利要求7所述的镍基高温合金，其特征在于，所述镍基高温合金在1100℃下的屈服强度大于等于50MPa；
    热等静压前得到的所述镍基高温合金的致密度大于等于99％，热等静压后得到的 所述镍基高温合金的致密度大于等于99.95％。
  9. 根据权利要求5-8任一项所述的镍基高温合金，其特征在于，所述激光选区熔融3D打印过程中的工艺参数包括：
    (a)激光功率100-700W；
    (b)激光扫描速度600-2000mm/s；
    (c)光斑直径40-110μm；
    (d)激光间距80-120μm；
    (e)铺粉厚度20-80μm。
  10. 一种镍基高温合金的制造方法，其特征在于，包括以下步骤：
    利用权利要求1-3任一项所述的镍基高温合金中的所述原料并采用3D打印制备得到所述镍基高温合金。
  11. 根据权利要求10所述的制造方法，其特征在于，所述3D打印包括激光选区熔融3D打印或电子束熔融3D打印。
  12. 根据权利要求11所述的制造方法，其特征在于，所述3D打印为激光选区熔融3D打印。
  13. 根据权利要求12所述的制造方法，其特征在于，包括以下步骤：
    先将所述原料制备成粒径为15-75μm的粉末再进行所述激光选区熔融3D打印，得到所述镍基高温合金。
  14. 根据权利要求13所述的制造方法，其特征在于，包括以下步骤：先将所述原料制备成粒径为15-75μm的粉末再进行所述激光选区熔融3D打印，然后进行热等静压和热处理，得到所述镍基高温合金。
  15. 根据权利要求14所述的制造方法，其特征在于，所述激光选区熔融3D打印过程中的工艺参数包括：
    (a)激光功率100-700W；
    (b)激光扫描速度600-2000mm/s；
    (c)光斑直径40-110μm；
    (d)激光间距80-120μm；
    (e)铺粉厚度20-80μm。
  16. 一种部件，其特征在于，所述部件包括权利要求1-9任一项所述的镍基高温合金或权利要求10-15任一项所述的制造方法制造的镍基高温合金。
  17. 一种航空、航天发动机、飞行器或燃气轮机，其特征在于，包括权利要求16所述的部件。
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