WO2015096980A1 - Gamma prime precipitation strengthened nickel-base superalloy for use in powder based additive manufacturing process - Google Patents

Gamma prime precipitation strengthened nickel-base superalloy for use in powder based additive manufacturing process Download PDF

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Publication number
WO2015096980A1
WO2015096980A1 PCT/EP2014/077060 EP2014077060W WO2015096980A1 WO 2015096980 A1 WO2015096980 A1 WO 2015096980A1 EP 2014077060 W EP2014077060 W EP 2014077060W WO 2015096980 A1 WO2015096980 A1 WO 2015096980A1
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powder
lt
mm
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characterized
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PCT/EP2014/077060
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French (fr)
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Roman Engeli
Thomas Etter
Hossein Meidani
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Alstom Technology Ltd
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Priority to EP13199285.1A priority Critical patent/EP2886225B1/en
Priority to EP13199285.1 priority
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Publication of WO2015096980A1 publication Critical patent/WO2015096980A1/en

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00Working by laser beam, e.g. welding, cutting or boring
    • B23K26/34Laser welding for purposes other than joining
    • B23K26/342Build-up welding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER
    • B22F1/00Special treatment of metallic powder, e.g. to facilitate working, to improve properties; Metallic powders per se, e.g. mixtures of particles of different composition
    • B22F1/0003Metallic powders per se; Mixtures of metallic powders; Metallic powders mixed with a lubricating or binding agent
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING 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
    • B22F3/10Sintering only
    • B22F3/105Sintering only by using electric current other than for infra-red radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • B22F3/1055Selective sintering, i.e. stereolithography
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00Working by laser beam, e.g. welding, cutting or boring
    • B23K26/0006Working by laser beam, e.g. welding, cutting or boring taking account of the properties of the material involved
    • 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
    • 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
    • B33Y70/00Materials specially adapted for additive manufacturing
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making alloys
    • C22C1/04Making alloys by powder metallurgy
    • C22C1/0433Nickel- or cobalt-based alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C19/00Alloys based on nickel or cobalt
    • C22C19/03Alloys based on nickel or cobalt based on nickel
    • C22C19/05Alloys based on nickel or cobalt based on nickel with chromium
    • C22C19/051Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
    • C22C19/056Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 10% but less than 20%
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER
    • B22F1/00Special treatment of metallic powder, e.g. to facilitate working, to improve properties; Metallic powders per se, e.g. mixtures of particles of different composition
    • B22F1/0003Metallic powders per se; Mixtures of metallic powders; Metallic powders mixed with a lubricating or binding agent
    • B22F1/0007Metallic powder characterised by its shape or structure, e.g. fibre structure
    • B22F1/0011Metallic powder characterised by size or surface area only
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER
    • B22F2302/00Metal Compound, non-Metallic compound or non-metal composition of the powder or its coating
    • B22F2302/45Others, including non-metals
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER
    • B22F2304/00Physical aspects of the powder
    • B22F2304/10Micron size particles, i.e. above 1 micrometer up to 500 micrometer
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K2103/00Materials to be soldered, welded or cut
    • B23K2103/08Non-ferrous metals or alloys
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Process efficiency
    • Y02P10/25Process efficiency by increasing the energy efficiency of the process
    • Y02P10/29Additive manufacturing
    • Y02P10/295Additive manufacturing of metals

Abstract

The application relates to the technology of producing three-dimensional articles by means of powder-based additive manufacturing, such as selective laser melting (SLM) or electron beam melting (EBM). Especially, it refers to a high oxidation resistant and high gamma-prime (γ') precipitation containing Ni-base super alloy powder on basis of IN738LC with a modified chemical composition. Such powder has the following chemical composition (in wt. -%): 15.7-16.3 Cr, 8.0-9.0 Co, 1.5- 2.0 Mo, 2.4-2.8 W, 1.5-2.0 Ta, 3.2-3.7 Al, 2.2-3.7 Ti, 0.6-1.1 Nb, 0.09-0.13 C, 0.007-0.012 B, 0.004≤Zr<0.03, 0.001≤Si<0.03, remainder Ni and unavoidable residual elements and in addition a powder size distribution between 10 and 100 μm and a spherical morphology. As an advantage nearly crack free three- dimensional articles can be produced with more productive process parameters and without complicated and time consuming variations of the addive manufacturing processes (e.g. pre-heating) and/or post processing (e.g. hot isostatic pressing HIP).

Description

DESCRIPTION

GAMMA PRIME PRECIPITATION STRENGTHENED NICKEL-BASE SUPERALLOY FOR USE IN POWDER BASED ADDITIVE MANUFACTURING

PROCESS

BACKGROUND OF THE INVENTION

The present invention relates to the technology of producing three-dimensional articles by means of powder-based additive manufacturing, such as selective laser melting (SLM) or electron beam melting (EBM). Especially, it refers to a high oxidation resistant and high gamma-prime (γ') precipitation containing Ni-base super alloy powder on basis of IN738LC with a modified chemical composition for manufacturing of nearly crack free components.

PRIOR ART

Gamma-prime (γ') precipitation-strengthened nickel-base superalloys with a combined fraction of Al and Ti of about more than 5 wt.-% are known to be very difficult to weld because of their micro-crack sensitiveness. Micro-cracking during welding of those superalloys, such as IN738LC, MARM-M 247 or CM247LC is attributed to the liquation of precipitates or low-melting eutectics in the heat affected zone (HAZ), ductility dip cracking (DDC) or strain-age cracking in subsequent heat treatment.

In the document: B. Geddes, H. Leon, X. Huang: Superalloys, Alloying and performance, ASM International, 2010, page 71 -72, the authors describe a weldability line for superalloys approximately as [two times Al concentration (in wt.- %) + Ti concentration (in wt. %)] < 6.0, this means that Ni base superalloys with more than 6 wt.- % of [2 times Al (in wt. -%)+ Ti (in wt. -%)] are defined as difficult to weld materials. Solidification and grain boundary liquation cracking occurs during the welding process, whereas post-weld heat treatments often lead to strain age cracking in gamma-prime Ni3(AI,Ti) precipitate strengthened alloys.

Therefore, mainly solid-solution strengthened (e.g. IN625) or gamma-prime strengthened nickel-base superalloys with a low amount of Al and Ti (e.g. IN718) are processed by SLM or EBM so far.

Document DE 10 2009 050 563 A1 describes a Ni-base superalloy for use in additive manufacturing, preferably laser melting, with a defined Ti-content from 0.3 to 1 .2 wt. -% and/or an Al-content from 2.5 to 5.7 wt. -% with a preffered total content of Ti and Al in a range from 2.8 to 5.0 wt. -%.

In a common approach to process difficult to weld gamma-prime precipitation- strengthened nickel-base superalloys, a powder bed is heated to an elevated temperature to reduce residual stresses resulting from the welding process. But, before the finished parts can be removed from the powder bed, it has to be cooled down to ambient temperature. Due to the low heat conductivity of powder beds, the heating up and cooling down of the powder bed requires a lot of time resulting in a significant decrease in productivity of the SLM process. Furthermore expensive heating equipment and isolation as well as adaptation of the process chamber are needed. EP 2 589 449 A1 discloses a SLM process for the production of crack-free and dense three-dimensional articles made of difficult to weld gamma-prime

precipitation-strengthened Nickel- base superalloy wherein the laser power, focus diameter of the focal spot and the scan speed of said focused laser beam are adjusted to obtain heat dissipation welding.

In general, SLM generated articles have different microstructures compared to cast material of the same alloy. This is primary due to powder based layer-by-layer article production and the inherent high cooling rates due to the high energy beam/ material interaction in these processes. Due to the extremely localized melting and the resulting rapid solidification during SLM, segregation of alloying elements and formation of precipitations is considerably reduced, which results in a decreased sensitivity for cracking compared to conventional build-up welding techniques. By using commercially available IN738LC powder for the SLM process

unfortunately microcracks are still present in the manufactured articles. This was for example confirmed in a presentation by Fraunhofer Institute for Laser

Technology (J. Risse, C. Golebiewski, W. Meiners, K. Wissenbach: Influence of process management on crack formation in nickel-based alloy parts (IN738LC) manufactured by SLM, RapidTech, 14./15.05.2013, Erfurt). It was stated there that crack free articles can only be manufactured with an extensive preheating.

However, the applicant has found out that by using IN738LC with adjusted chemistry, SLM allows the near-net shape processing of this difficult to weld material. A high Al and Ti content of gamma-prime (γ') precipitation-strengthened nickel-base superalloys is not the main reason for cracking and that hot cracking susceptibility of SLM processed IN738LC cannot be predicted by classic

weldability charts. SUMMARY OF THE INVENTION

It is an object of the present invention to provide a Nickel-base superalloy powder with high gamma-prime precipitation content for additive manufacturing (SLM, EBM) of three-dimensional articles with a reduced hot cracking tendency and disclose suitable process parameter for manufacturing such an article. The modified composition of the powder according to the present invention is based on known commercially available Inconel 738 (IN738LC) powder with a specification of (in wt. -%): 15.7-16.3 Cr, 8.0-9.0 Co, 1 .5-2.0 Mo, 2.4-2.8 W, 1 .5-2.0 Ta, 3.2-3.7 Al, 2.2-3.7 Ti, 0.6-1 .1 Nb, 0.09-0.13 C, 0.007-0.012 B, 0.03-0.08 Zr, max. 0.3 Si, remainder Ni and unavoidable residual elements (impurities).

This object is realized by a powder composition according to claim 1 with a powder size distribution between 10 and 100 μιτι and a spherical morphology.

The core of the invention is that by a tight control and modification of specific minor/trace elements (0.004<Zr<0.03 wt. -% and 0.001 <Si<0.03 wt. -%) in the IN738LC alloy powder with the above-mentioned powder size distribution and morphology of the powder crack free or at least nearly crack free components can be produced by SLM without preheating. It was found that the known limitation of maximal 0.3 wt. -% Si and maximal 0.08 wt. -% Zr for commercially available IN738LC powder is too high for use of this powder in powder based additive manufacturing, like SLM or EBM. In contrast to the state of the art knowledge not the (Al+Ti) content is limiting the processability, but the minor concentrations of Si and Zr.

In preferred embodiments the Si content of the powder is max. 0.02 wt. -% and/or the Zr content is max. 0.02 wt. -%. The SLM process parameters are chosen such that the Laser area energy density ED during SLM process is according to the invention in the range between 0.5-10 J/mm2. ED is calculated as follows: with PL: Laser Power [W]

Vs: Scan velocity [mm/s]

DB: Laser beam diameter [mm].

According to a preferred embodiment of the invention the Laser area energy density is between 0.8 and 5 J/mm2, preferably between 1 -3.5 J/mm2.

According to another embodiments of the invention the layer thickness of each SLM layer is in the range of 0.01 -0.1 mm, preferably 0.02-0.05 mm and most preferably 0.03-0.04 mm. Then nearly crack free componets, for example gas turbine components, can be produced.

BRIEF DESCRIPTION OF THE DRAWINGS

The present invention is now to be explained more closely by means of different embodiments and with reference to the attached drawings.

Fig. 1 shows the microstructure of a SLM test probe made of standard

IN738LC powder (prior art) with a high density of microcracks;

Fig. 2 shows the microstructure of a SLM test probe made of a modified powder according to a first embodiment of the invention with a reduced density of microcracks compared to Fig. 1 ;

Fig. 3 shows in detail the average crack density for using the prior art powder and for using several embodiments according to the present invention; Fig. 4 shows the crack density dependency on the Zr content in the tested powder and

Fig. 5 shows the crack density dependency on the Si content in the

tested powder.

DETAILED DESCRIPTION OF DIFFERENT EMBODIMENTS OF THE

INVENTION

As described above it was found out that a high Al and Ti content of gamma- prime (γ') precipitation-strengthened nickel-base superalloys is not the main reason for cracking and that hot cracking susceptibility of SLM processed IN738LC powder cannot be predicted by classic weldability charts. In contrast, a tight control of specific minor/trace elements (Zr, Si) is necessary as well as using a powder with a powder size distribution between 10 and 100 μιτι and a spherical morphology.

Fig. 1 shows the microstructure of a SLM test probe (three-dimensional article) made of standard IN738LC powder (commercial available prior art) with a specification of (in wt. -%): 15.7-16.3 Cr, 8.0-9.0 Co, 1 .5-2.0 Mo, 2.4-2.8 W, 1 .5-

2.0 Ta, 3.2-3.7 Al, 2.2-3.7 Ti, 0.6-1 .1 Nb, 0.09-0.13 C, 0.007-0.012 B, 0.03-0.08 Zr, max. 0.3 Si, remainder Ni and unavoidable residual elements (impurities).

IN738LC is high oxidation resistant and has a high content of gamma-prime (γ') precipitations.The details are for Zr content 0.06 wt. -% and for Si content 0.085 wt.- %. It can be seen in Fig. 1 , that the probe according to the prior art has a high density of microcracks.

The core of the invention is that by a tight control and modification of specific minor/trace elements (0.004<Zr<0.03 wt. -% and 0.001 <Si<0.03 wt. -%) in the IN738LC alloy powder with the above-mentioned powder size distribution and morphology of the powder crack free or at least nearly crack free components (three-dimensional articles) can be produced by SLM without preheating. It was found that the known limitation of maximal 0.3 wt. -% Si and 0.08 wt. -% Zr for commercially available IN738LC powder is too high for use of this powder in powder based additive manufacturing, like SLM, EBM. In contrast to the state of the art knowledge not the (Al+Ti) content is limiting the processability, but the minor concentrations of Si and Zr.

Therefore, several Nickel-base powders with a chemical composition of 15.7-16.3 Cr, 8.0-9.0 Co, 1 .5-2.0 Mo, 2.4-2.8 W, 1 .5-2.0 Ta, 3.2-3.7 Al, 2.2-3.7 Ti, 0.6-1 .1 Nb, 0.09-0.13 C, 0.007-0.012 B, 0.004<Zr<0.03, 0.001 <Si<0.03, remainder Ni and unavoidable residual elements and with powder size distribution between 10 and 100 μιτι and a spherical morphology were tested for additive manufacturing of three-dimensional articles. Fig. 2 shows a first embodiment of the invention. The article was produced by SLM with a powder according to the invention, here with Zr< 0.03 wt. -% and Si= 0.0176 wt. -%. During the layer by layer built up of the article the Laser power PL, the scan velocity Vs and the Laser beam diameter of SLM were chosen/applied such that the Laser area energy density ED was in the range between 0.5-10 J/mm2', here in detail ED was 1 .8 J/ mm2. Preferred ranges of the Laser area energy density are 0.8-5 J/mm2, more preferred 1 -3.5 J/mm2.

It can be seen in Fig. 2 that the probe according to the invention has only a very low microcrack density compared to Fig. 1 .

In Fig. 3 is shown in detail the average crack density for using the prior art powder and for using several embodiments according to the present invention. The tight control of the elements Si and Zr considerably reduces hot cracking during SLM or EBM, resulting in defect densities which are by a factor of 6 lower compared to the commercial available IN738LC. Therefore, nearly crack free three-dimensional articles can be produced with more productive process parameters and without complicated and time consuming variations of the addive manufacturing processes (e.g. pre-heating) and/or post processing (e.g. hot isostatic pressing HIP).

Each of the layers applied within the SLM or EBM process have a thickness in the range of 0.01 -0.1 mm, preferably in the range of 0.02-0.05 mm. A more peferred range is 0.03-0.04 mm. In Fig. 4 is shown as an example for different SLM probes made of IN738LC powder the crack density dependency on the Zr content in the tested powder and in Fig. 5 the crack density dependency on the Si content in the tested powder.

Much reduced crack density is received for the disclosed ranges (in wt. -%) of 0.004<Zr<0.03 and 0.001 <Si<0.03. Max. 0.02 wt. -% Zr and/or max 0.02 wt. -% Si are preferred because of the nearly microcrack free microstructure.

Of course, the invention is not limited to the decribed embodiments. For example, it is expected that the disclosed nickel-base superalloy powder is applicable not only for SLM manufacturing process but also for EMB manufacturing process with the described advantages.

Claims

1. Nickel-base superalloy powder with a high gamma-prime precipitation content for additive manufacturing of three-dimensional articles characterized in that the powder has the following chemical composition (in wt. -%): 15.7-16.3 Cr, 8.0-9.0 Co, 1 .5-2.0 Mo, 2.4-2.8 W, 1 .5-2.0 Ta, 3.2-3.7 Al, 2.2-3.7 Ti, 0.6-1 .1 Nb, 0.09-0.13 C, 0.007-0.012 B, 0.004<Zr<0.03, 0.001 <Si<0.03, remainder Ni and unavoidable residual elements and wherein the powder has a powder size distribution between 10 and 100 μιτι and a spherical morphology.
2. Nickel-base superalloy powder according to claim 1 , characterized in that the Si content is max. 0.02 wt. -%.
3. Nickel-base superalloy powder according to claim 1 , characterized in that the Zr content is max. 0.02 wt. -%.
4. SLM process for additive manufacturing of three-dimensional articles with the Nickel-base superalloy powder according to one of claims 1 -3, characterized in that the Laser power PL, the scan velocity Vs and the Laser beam diameter DB during the layer by layer built-up of the article are applied such that the Laser area energy density ED is in the range between 0.5-10 J/mm2.
5. SLM process according to claims 4, characterized in that the Laser area energy density ED is between 0.8 and 5 J/mm2
6. SLM process according to claim 5, characterized in that the Laser area energy density ED is between 1 -3.5 J/mm2.
7. SLM process according to claim 4, characterized in that layers are applied with a thickness of each layer in the range of 0.01 -0.1 mm.
8. SLM process according to claim 7 characterzied in that layers are applied with a thickness of each layer in the range of 0.02-0.05 mm.
9. SLM process according to claim 8 characterzied in that layers are applied with a thickness of each layer in the range of 0.03-0.04 mm.
PCT/EP2014/077060 2013-12-23 2014-12-09 Gamma prime precipitation strengthened nickel-base superalloy for use in powder based additive manufacturing process WO2015096980A1 (en)

Priority Applications (2)

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EP13199285.1A EP2886225B1 (en) 2013-12-23 2013-12-23 Gamma prime precipitation strengthened nickel-base superalloy for use in powder based additive manufacturing process
EP13199285.1 2013-12-23

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CN201480070717.1A CN105828983B (en) 2013-12-23 2014-12-09 γ ' precipitating enhancing nickel based super alloy for the increasing material manufacturing process based on powder
KR1020167019023A KR20160101972A (en) 2013-12-23 2014-12-09 Gamma prime precipitation strengthened nickel-base superalloy for use in powder based additive manufacturing process
US15/107,001 US20170021453A1 (en) 2013-12-23 2014-12-09 Gamma prime precipitation strengthened nickel-base superalloy for use in powder based additive manufacturing process
JP2016542676A JP2017508877A (en) 2013-12-23 2014-12-09 Gamma prime precipitation strengthened nickel base superalloys used in the additive manufacturing process based on powder

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