CN105397085B - A kind of method that discharge plasma sintering prepares Ni-base P/M Superalloy - Google Patents
A kind of method that discharge plasma sintering prepares Ni-base P/M Superalloy Download PDFInfo
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- CN105397085B CN105397085B CN201510672555.5A CN201510672555A CN105397085B CN 105397085 B CN105397085 B CN 105397085B CN 201510672555 A CN201510672555 A CN 201510672555A CN 105397085 B CN105397085 B CN 105397085B
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Abstract
The invention discloses a kind of method that discharge plasma sintering prepares Ni-base P/M Superalloy, belong to powdered metallurgical material field.Shaping is sintered to atomization Ni-base Superalloy Powder using discharge plasma sintering process, solid solution and Ageing Treatment is then carried out, obtains Ni-base P/M Superalloy.The present invention proposes that discharge plasma sintering process prepares Ni-base P/M Superalloy, realizes that powder Fast Sintering shapes, can effectively suppress crystal grain and grow up, the alloy of preparation has tiny, uniform equiaxed grain structure；It is connected by powder surface-discharge activation with quick diffusion, suppresses powder particle complex boundary carbide, the formation of oxide, eliminates primary granule border；This method process route is simple, and preparation time is short, and the second phase size is tiny, be evenly distributed, good mechanical performance.
Description
Technical field
The present invention relates to a kind of method that discharge plasma sintering prepares Ni-base P/M Superalloy, belong to powder metallurgy material
Material field.
Background technology
Ni-base P/M Superalloy has tiny crystal grain, even tissue, without gross segregation, alloying level be high, surrender is strong
The features such as degree height and excellent fatigue behaviour, be the preferred material for manufacturing advanced engine thermal end pieces.
The preparation of Ni-base P/M Superalloy mainly includes two technology paths, and one is the countries such as America and Europe, main to use " argon
Aerosolization the hot extrusion of (AA) powder (HEX) shaping+isothermal forging (ITF) " preparation technology；Two be the countries such as Russia, is mainly adopted
With " the direct high temperature insostatic pressing (HIP) of plasma rotating electrode (PREP) powder (As-HIP) shaping " preparation technology.
P＆WA companies of the U.S. are prepared for first in 1972 using argon gas powder by atomization+hot extrusion+isothermal forging process
IN100 powder metallurgy superalloys, 11 kinds of parts such as compressor disc and the turbine disk as F100 engines, 1976 using directly heat
Isostatic pressing process have developed the LC Astroloy powder turbine disks, for JT8D-17R and TF-30 engines.A frame in 1980
After TF/A-18 aircraft low-pressure turbines disk rupture accident equipped with F404 engines, the U.S. is carried out to the manufacturing process of powder disk
Adjustment, the powder turbine disk is prepared using high temperature insostatic pressing (HIP)/hot extrusion+isothermal forging process.
China starts to carry out the research of powder metallurgy superalloy in 1970s, and two kinds of techniques are prepared with powder metallurgy conjunction
Gold has all carried out the research work of correlation.Chinese patent CN102392147A, discloses a kind of superfine crystal nickel-based powder metallurgy and closes
Golden preparation method, prepares superalloy powder using plasma rotating electrode process or Powder In Argon Atomization, is obtained through Powder hot isostatic pressure
Dense powder high temperature alloy blank is obtained, then blank is coated with non-metallic insulation material, then the ingot blank coated is forged and pressed
The upset quasi- isothermal forging being combined with local deformation control, obtains biscuit.Finally, the biscuit of forging is subjected to recrystallization annealing
Processing, obtains the tiny powder metallurgy superalloy biscuit of even tissue, crystal grain.There is provided one kind by Chinese patent CN104493167A
The thermal extrusion moulding method of powder metallurgy superalloy annular element, will load hot extrusion annular bag using argon gas atomization superalloy powder
Set, high temperature insostatic pressing (HIP) obtains ingot blank first, and large extrusion ratio (10~20) hot extrusion is then carried out to ingot blank, and machining removes out jacket
Material obtains powder metallurgy superalloy.
Ni-base P/M Superalloy technological process is prepared using high temperature insostatic pressing (HIP) or hot extrusion+isothermal forging shaping at present to answer
Miscellaneous, time-consuming, prepares cost high.Powder metallurgy superalloy is prepared using high temperature insostatic pressing (HIP) shaping, because soaking time is longer so that brilliant
Grain is easily grown up, and the oxygen of powder adsorption is easily reacted with the active element in alloy, and oxygen is formed on powder particle border
Compound, causes primary granule border occur, drops low-alloyed mechanical property.
For above-mentioned problem, this patent proposes that discharge plasma sintering process prepares Ni-base P/M Superalloy.
The content of the invention
It is an object of the invention to provide a kind of method that discharge plasma sintering prepares Ni-base P/M Superalloy.
The method that a kind of discharge plasma sintering of the present invention prepares Ni-base P/M Superalloy, using nickel-base high-temperature powder as original
Material, through solid solution and Ageing Treatment after being shaped by discharge plasma sintering, obtains Ni-base P/M Superalloy.
The method that a kind of discharge plasma sintering of the present invention prepares Ni-base P/M Superalloy, the nickel-base high-temperature powder is
Argon gas is atomized Ni-base Superalloy Powder.
The method that a kind of discharge plasma sintering of the present invention prepares Ni-base P/M Superalloy, the nickel-base high-temperature powder
Granularity is less than or equal to 75 μm.
The method that a kind of discharge plasma sintering of the present invention prepares Ni-base P/M Superalloy, discharge plasma sintering shaping
Technological parameter be：1000~1200 DEG C of temperature, 40~100MPa of pressure；5~20min of soaking time.
The method that a kind of discharge plasma sintering of the present invention prepares Ni-base P/M Superalloy, the temperature of the solution treatment
For 1000~1250 DEG C, 1~2h of soaking time.
The method that a kind of discharge plasma sintering of the present invention prepares Ni-base P/M Superalloy, the temperature of Ageing Treatment is
700~900 DEG C, 4~10h of soaking time.
Advantages and positive effects of the present invention：
The present invention proposes to prepare Ni-base P/M Superalloy using discharge plasma sintering, with advantages below and positive effect
Really：
First, discharge plasma sintering prepares Ni-base P/M Superalloy, and the shaping of powder Fast Sintering, effectively suppression can be achieved
Combinations grain grow up, the alloy of preparation has tiny, uniform equiaxed grain structure.
Second, Ni-base P/M Superalloy is prepared using discharge plasma sintering, passes through powder particle surface discharge activation
It is connected with quick diffusion, being rapidly heated and the combination of powder metallurgical interface for powder surface can be achieved, suppresses powder particle border and answers
The formation of miscellaneous carbide, oxide, eliminates primary granule border.
3rd, Ni-base P/M Superalloy is prepared using discharge plasma sintering, process route is simple, and preparation time is short,
Second phase size is tiny, be evenly distributed, good mechanical performance.
In summary, the present invention is a kind of quick method for preparing Ni-base P/M Superalloy, and this method can be controlled effectively
Crystal grain grows up, eliminates primary granule border, improves mechanical property.
Brief description of the drawings
Accompanying drawing 1 is comparative example 1 atomized powder, 1150 DEG C of large extrusion ratios (10：1) nickel-base high-temperature of hot-pressed preparation is closed
Microscopic structure ESEM (SEM) figure of gold；
Accompanying drawing 2 is the [document of comparative example 2：Zhao Junpu, Tao Yu, Yuan Shouqian, wait original in powder metallurgy high-temperature alloys
Grain border (PPB) problem [J] powder metallurgy industries, 2010 (04)：43-49] atomized powder high temperature insostatic pressing (HIP) shaping prepare it is Ni-based
The microscopic structure of high temperature alloy.
Accompanying drawing 3 is micro- group of nickel base superalloy prepared by 1 atomized powder of embodiment, 1150 DEG C of plasma agglomeration shapings
Knit ESEM (SEM) figure.
Accompanying drawing 4 is the aobvious of Ni-base P/M Superalloy prepared by 1 atomized powder of embodiment, 1150 DEG C of plasma agglomeration shapings
Micro-assembly robot.Compared with alloy prepared by the high temperature insostatic pressing (HIP) of accompanying drawing 2, primary granule border is substantially eliminated.
It can be seen that the grain size number of gained nickel base superalloy is ASTM9 grades from accompanying drawing 1, crystal grain is thicker.
In accompanying drawing 2,1,2,3 represent the border of primary granule respectively.As can be seen that the atomized powder of comparative example 2 from accompanying drawing 2
The microscopic structure of nickel base superalloy prepared by high temperature insostatic pressing (HIP) shaping is observed that obvious primary granule border, such as 1,2,3
It is shown.
As can be seen that the second distributed mutually of the gained finished product of embodiment 1 is uniform from accompanying drawing 3, crystal grain is tiny, uniform, crystal grain
It is ASTM10 grades to spend rank, and the alloy grain compared to the hot-pressed preparation shown in accompanying drawing 1 is more tiny, uniform.
It can be seen that its primary granule border in the finished product prepared by embodiment 1 from accompanying drawing 4 substantially to disappear, with accompanying drawing 2
After contrast, this sign just becomes apparent.
Embodiment
The invention will be further described with specific comparative example and embodiment below in conjunction with the accompanying drawings.
Comparative example 1：
Argon gas is atomized into Ni-based pre-alloyed powder, and (composition is Ni-20.6Co-13Cr-3.8Mo-2.1W-3.4Al-3.9Ti-
2.4Ta-0.9Nb (wt%)) load steel capsule, vacuumize degasification, sealing；Hot-pressed in 1150 DEG C of progress, extrusion ratio is
10：1, obtain nickel-base alloy bar；Finally in 1180 DEG C of solid solutions 1h, 815 DEG C of timeliness 8h, nickel base superalloy is obtained.
The room-temperature mechanical property of alloy is：Fracture strength 1197MPa, yield strength 827MPa, elongation percentage 4.94%, density
8.1787g/cm3.The microscopic structure of alloy is shown in accompanying drawing 1, and grain size number is ASTM9 grades.
Comparative example 2：[Zhao Junpu, Tao Yu, Yuan Shouqian wait the primary granule border in powder metallurgy high-temperature alloys to document
(PPB) problem [J] powder metallurgy industries, 2010 (04)：43-49]
Argon gas is atomized into Ni-based pre-alloyed powder, and (composition is Ni-13Co-16Cr-4Mo-4W-2.2Al-3.7Ti-0.8Nb
(wt%)) load steel capsule, vacuumize degasification, sealing；High temperature insostatic pressing (HIP) shaping is carried out in 1180 DEG C/130MPa, the time is 3h, is obtained
Obtain nickel-base alloy blank.The microscopic structure of alloy is shown in accompanying drawing 2, occurs in that obvious primary granule border.
Comparative example 3
Argon gas is atomized into Ni-based pre-alloyed powder, and (composition is Ni-20.6Co-13Cr-3.8Mo-2.1W-3.4Al-3.9Ti-
2.4Ta-0.9Nb (wt%)) plasma agglomeration is carried out in 900 DEG C/40MPa, 20min is incubated, solution treatment is then carried out：900
DEG C/3h, then carry out Ageing Treatment：700 DEG C/8h, obtain nickel base superalloy.
The room-temperature mechanical property of alloy is：Fracture strength 57MPa, material is changed into fragility；Density 7.0g/cm3。
Embodiment 1：
Argon gas is atomized into Ni-based pre-alloyed powder, and (composition is Ni-20.6Co-13Cr-3.8Mo-2.1W-3.4Al-3.9Ti-
2.4Ta-0.9Nb (wt%)) plasma agglomeration is carried out in 1150 DEG C/40MPa, 5min is incubated, blank is prepared；Then carry out
Solution treatment：1180 DEG C/1h, Ageing Treatment：815 DEG C/8h, obtain nickel base superalloy.
The room-temperature mechanical property of alloy is：Fracture strength 1273MPa；Yield strength 906MPa；Elongation percentage 10.65%；It is close
Spend 8.1735g/cm3.The microscopic structure of alloy is shown in accompanying drawing 3,4, and grain size number is ASTM10 grades, and primary granule border is obtained substantially
To elimination.
Embodiment 2：
Argon gas is atomized into Ni-based pre-alloyed powder, and (composition is Ni-20.6Co-13Cr-3.8Mo-2.1W-3.4Al-3.9Ti-
2.4Ta-0.9Nb (wt%)) plasma agglomeration is carried out in 1100 DEG C/60MPa, 10min is incubated, blank is prepared；Then enter
Row solution treatment：1115 DEG C/1h+1170 DEG C/3h, Ageing Treatment：845 DEG C/8h+760 DEG C/8h, obtain nickel base superalloy.
Claims (3)
1. a kind of method that discharge plasma sintering prepares Ni-base P/M Superalloy, it is characterized in that：Using nickel-base high-temperature powder as
Raw material, through solution treatment and Ageing Treatment after being molded by discharge plasma sintering, obtains Ni-base P/M Superalloy；
Discharge plasma sintering shaping technological parameter be：1000~1200 DEG C of temperature, 40~100MPa of pressure, soaking time 5
~20min；
The temperature of the solution treatment is 1000~1250 DEG C, 1~2h of soaking time；
The temperature of Ageing Treatment is 700~900 DEG C, 4~10h of soaking time.
2. the method that discharge plasma sintering according to claim 1 prepares Ni-base P/M Superalloy, it is characterised in that：
The nickel-base high-temperature powder is that argon gas is atomized Ni-base Superalloy Powder.
3. the method that discharge plasma sintering according to claim 1 prepares Ni-base P/M Superalloy, it is characterised in that：
The granularity of the nickel-base high-temperature powder is less than or equal to 75 μm.
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| RU2816973C1 (en) * | 2023-02-20 | 2024-04-08 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Юго-Западный государственный университет" (ЮЗ ГУ) | Method of producing heat-resistant nickel alloy from powders obtained by electroerosion dispersion of “жс6у” alloy wastes in lighting kerosene |
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