CN110337500A - Ni base superalloy and its manufacturing method - Google Patents
Ni base superalloy and its manufacturing method Download PDFInfo
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- CN110337500A CN110337500A CN201880006208.0A CN201880006208A CN110337500A CN 110337500 A CN110337500 A CN 110337500A CN 201880006208 A CN201880006208 A CN 201880006208A CN 110337500 A CN110337500 A CN 110337500A
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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
- C22C19/056—Alloys 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%
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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
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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
- C22C19/007—Alloys based on nickel or cobalt with a light metal (alkali metal Li, Na, K, Rb, Cs; earth alkali metal Be, Mg, Ca, Sr, Ba, Al Ga, Ge, Ti) or B, Si, Zr, Hf, Sc, Y, lanthanides, actinides, as the next major constituent
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- 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%
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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
- C22C19/057—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being less 10%
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- 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
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Abstract
It is 35 moles of % or more at being grouped as that Ni base superalloy of the invention, which has the Equilibrium Precipitation amount of the γ ' phase at 700 DEG C, and having maximum gauge in section structure is 75nm crystal grain below.The method for manufacturing the Ni base superalloy is also provided.This method comprises: preparatory process, prepares have the blank at the Ni base superalloy being grouped as that the Equilibrium Precipitation amount of the γ ' phase at 700 DEG C is 35 moles of % or more;And manufacturing procedure, multiple plastic processing is carried out to the blank with 500 DEG C of temperature below and makes accumulative working modulus for 30% or more.Further, a kind of method manufacturing Ni base superalloy is also provided, prepare have this at be grouped as, hardness is 500HV or more, in section structure have maximum gauge be 75nm crystal grain below alloy material, plastic processing is carried out to the alloy material with 500 DEG C of temperature below, obtains the alloy that hardness is 500HV or more.
Description
Technical field
The present invention relates to Ni base superalloy and its manufacturing methods.
Background technique
As the heat-resistant part of the gas turbine for aircraft engine, power generation, for example, largely using INCONEL (note
Volume trade mark) Ni base superalloy as 718 alloys.High performance and low energy consumption with gas turbine, seek to have
The heat-resistant part of high heat resisting temperature.In order to improve the heat resistance (elevated temperature strength) of Ni base superalloy, it is most useful that
Increase as with Ni3Al is the γ ' phase (being also denoted as " γ ' " phase below) of the precipitation strength phase of the intermetallic compound mainly formed
Amount.Also, Ni base superalloy also contains Al, Ti, Nb that element is generated as γ ', so as to so that Ni base is super heat-resisting
The elevated temperature strength of alloy further increases.From now in order to meet high-fire resistance, high intensity, seek the more Ni bases of amount of γ ' phase
Superalloy.
However, it is known that increase of the Ni base superalloy with γ ' phase, hot worked deformation drag becomes larger and difficult processing.
In particular, in γ ' when being γ ' moles of rate of 35~40 moles of % or more, processability is especially low for the quantitative change of phase.For example, INCONEL
γ ' is mutually especially more in the alloys such as (registered trademark) 713C alloy, IN939, IN100, Mar-M247, it is impossible to which plastic processing is led to
Casting (as-cast) is directly used in frequently as casting alloy.
As the motion for improving the thermoplasticity processing property of such Ni base superalloy, described in patent document 1
There to be the Ni hyper-base heat-resisting alloy ingot casting that γ ' moles of rate is 40 moles of % composition described above with 5% or more working modulus and deficiency
30% is cold worked, the manufacturing method being then heat-treated with the temperature more than γ ' solid solubility temperature.This method is added by cold
The combination of work process and heat treatment procedure is so as to the superalloy application hot-working of Ni base and capable of obtaining 90% or more
Recrystallization rate.
In addition, repairing the heat-resistant part of the Ni base superalloy more than the amount of above-mentioned γ ' phase in recent years or utilizing three-dimensional
The demand for making the heat-resistant part itself increases.As appearance blank at this time, the filament of Ni base superalloy is needed.This is thin
The component shape that line can also be processed into spring etc. carry out using.The line footpath (diameter) of the filament of Ni base superalloy is for example,
5mm is hereinafter, further thin in this way for 3mm or less.Such filament is for example 10mm " wire rod " conduct below preparing line footpath
Intermediate carries out plastic processing to carry out production being effective to the wire rod." wire rod " as the intermediate is as long as can be with
Utilize plastic processing, so that it may effectively manufacture the filament of Ni base superalloy.
The manufacturing method of filament as such superalloy, motion have the foudry line for being 5mm or more with line footpath to be
Original material by these casting line tyings and carries out hot extrusion, the gimmick then separated (patent document 2).
Existing patent document
Patent document
Patent document 1: International Publication No. 2016/129485
Patent document 2: No. 4777710 specifications of U.S. Patent No.
Summary of the invention
Problems to be solved by the invention
As described above, Ni base superalloy increases with the amount of γ ' phase, thermoplasticity processing property is reduced.Patent document 2
Gimmick is effective to the manufacture for the filament that predetermined component forms, but is only applicable to this at being grouped as, after being for the amount of γ ' phase
When the Ni base superalloy of " the 35 moles of % or more " that states, it is extremely difficult that they, which are thermoformed into filament,.
In addition, the gimmick of patent document 2 there are complex procedures, manufacturing cost is big the problems such as.
The method of patent document 1 is effective to the hot worked Ni base superalloy of application.But, it is therefore desirable to working modulus
5% or more and ingot casting is cold worked less than 30%, is then heat-treated.
Present invention aims to with previous entirely different new skill, it is super to provide the excellent Ni base of plastic processing
Heat-resisting alloy and its manufacturing method.It is of the invention it is other be designed to provide even if without hot-working, also can be to process greatly
The Ni base superalloy and its manufacturing method of rate progress plastic processing.Do not implement other midways that are designed to provide of the invention
Heat treatment and the Ni base superalloy and its manufacturing method that plastic processing can be carried out with big working modulus.Of the invention is other
It is designed to provide the wire rod of manufacture Ni base superalloy, the new method of filament.
The solution to the problem
A viewpoint according to the present invention, providing the Equilibrium Precipitation amount with the γ ' phase at 700 DEG C is 35 moles of % or more
At being grouped as, in section structure be the Ni base superalloy of 75nm crystal grain below with maximum gauge.
According to a specific example, which preferably has the hardness of 500HV or more.
In addition, according to a specific example, it is 1 μm preferably every2In section structure there are 5 or more the maximum gauges be 75nm
Crystal grain below.
According to a specific example, preferably the Ni base superalloy includes C:0~0.25%, Cr:8.0 in terms of quality %
~25.0%, Al:0.5~8.0%, Ti:0.4~7.0%, Co:0~28.0%, Mo:0~8%, W:0~6.0%, Nb:0~
4.0%, Ta:0~3.0%, Fe:0~10.0%, V:0~1.2%, Hf:0~1.0%, B:0~0.300%, Zr:0~
0.300%, surplus is Ni and impurity.
According to a specific example, which preferably there is the Equilibrium Precipitation amount of the γ ' phase at 700 DEG C to be
40 moles of % or more at being grouped as.
According to a specific example, preferably the Ni base superalloy include in mass C:0~0.03%, Cr:8.0~
22.0%, Al:2.0~8.0%, Ti:0.4~7.0%, Co:0~28.0%, Mo:2.0~7.0%, W:0~6.0%, Nb:0
~4.0%, Ta:0~3.0%, Fe:0~10.0%, V:0~1.2%, Hf:0~1.0%, B:0~0.300%, Zr:0~
0.300%, surplus is Ni and impurity.
Other viewpoints according to the present invention provide the method for manufacturing above-mentioned Ni base superalloy.The manufacturing method includes:
Preparatory process prepares the blank with the Ni base superalloy of mentioned component composition;With
Manufacturing procedure carries out multiple plastic processing to the blank with 500 DEG C of temperature below, so that accumulative working modulus is
30% or more.
According to a specific example, which has the shape of bar, adds up the multiple plasticity that working modulus is 30% or more
It is processed as making the processing of the reduced cross-sectional area of the bar.
The plastic processing preferably includes the process compressed from the periphery of bar towards axle center.
According to a specific example, without heat treatment between preferably multiple plastic processing.
Other viewpoints according to the present invention, providing manufacture (or processing), there is the Equilibrium Precipitation amount of γ ' phase at 700 DEG C to be
The method at the Ni base superalloy being grouped as of 35 moles of % or more.This method comprises:
Preparatory process, prepare hardness be 500HV or more, in section structure have maximum gauge be 75nm crystal grain below
Alloy material;With
Manufacturing procedure carries out plastic processing to alloy material with 500 DEG C of temperature below, and obtaining hardness is 500HV or more
Alloy.
It is preferably repeated multiple times to carry out above-mentioned manufacturing procedure according to a specific example.
Additionally, it is preferred that without heat treatment between the multiple manufacturing procedure.
It is 1 μm preferably every for alloy material and aforementioned alloy according to a specific example2In section structure there are 5 with
Upper maximum gauge is 75nm crystal grain below.
According to a specific example, which preferably there is the Equilibrium Precipitation amount of the γ ' phase at 700 DEG C to be
40 moles of % or more at being grouped as.
Further, the Ni base superalloy preferably have above-mentioned record at being grouped as.
Show by referring to the explanation and appended attached drawing of non-limiting specific example below advantages of the present invention,
Feature and detailed content.
Detailed description of the invention
Fig. 1 is the electron backscatter diffraction for indicating the section microscopic structure of Ni base superalloy of example No.1-2 of the present invention
(EBSD) as an example figure.
Fig. 2 is an example for indicating the EBSD picture of the section microscopic structure of Ni base superalloy of example No.1-4 of the present invention
The figure of son.
Fig. 3 is an example for indicating the EBSD picture of the section microscopic structure of Ni base superalloy of example No.1-5 of the present invention
The figure of son.
Fig. 4 is an example for indicating the EBSD picture of the section microscopic structure of Ni base superalloy of example No.1-7 of the present invention
The figure of son.
Fig. 5 is an example for indicating the EBSD picture of the section microscopic structure of Ni base superalloy of example No.1-9 of the present invention
The figure of son.
Fig. 6 is an example for indicating the EBSD picture of the section microscopic structure of Ni base superalloy of comparative example No.1-1
Figure.
Specific embodiment
The present invention can provide plastic processing excellent Ni base using the new method for being not based on previous thermoplasticity processing
It is really innovated as superalloy.
Present inventors studied γ ' plastic processing of Ni base superalloy more than the amount of phase.Its result specifies, makes
" nanocrystal " is generated in the tissue of Ni base superalloy to improve the plastic processing of Ni base superalloy tremendously
The phenomenon that.Further, it was found that the generation of the nanocrystal can be reached using " the cold plasticity processing " of rated condition, to complete this
Invention.
It is 35 moles of %'s or more that Ni base superalloy of the invention, which has the Equilibrium Precipitation amount of the γ ' phase at 700 DEG C,
At being grouped as, having maximum gauge in section structure is 75nm crystal grain below.It is that 75nm is below with the maximum gauge
The Ni base superalloy of crystal grain has excellent plastic processing.Also, for the plastic processing, Ni base of the invention is super
The cold plasticity processability of heat-resisting alloy is especially excellent.
Herein, the amount of the γ ' phase of Ni base superalloy can use the numerical value such as " volume fraction " of the γ ' phase, " the area ratio "
Index expression.The index expression of the amount of γ ' the phase numerical value of " γ ' moles of rate " in this specification.γ ' moles of rate refers to Ni base
The Equilibrium Precipitation amount of γ ' phase that superalloy can be precipitated in thermodynamic equilibrium state, stable.It is indicated with " mole rate "
The value of the Equilibrium Precipitation amount of γ ' phase is determined by what Ni base superalloy had at being grouped as.Mole % of the Equilibrium Precipitation amount
Value can use calculation of thermodynamic equilibrium parsing find out.The parsing of calculation of thermodynamic equilibrium can pass through various thermodynamical equilibriums
Software for calculation precision is good and easily finds out.
γ ' moles of rate of Ni base superalloy is set as " the Equilibrium Precipitation amount at 700 DEG C " in the present invention.Ni base is super
The elevated temperature strength of heat-resisting alloy can use the Equilibrium Precipitation amount evaluation of the γ ' phase in tissue, and the elevated temperature strength is bigger, and thermoplasticity adds
Work becomes more difficult.The Equilibrium Precipitation amount of γ ' phase in tissue generally becomes smaller in general 700 DEG C of following temperature dependences, becomes
Less constant, therefore on the basis of value when above-mentioned " 700 DEG C ".
As described above, γ ' moles of rate of usually Ni base superalloy is bigger, it is thermoformed more difficult.But according to
The present invention increases γ ' moles of rate, and the cold plasticity processability raising with Ni base superalloy has very big relationship.The present invention
Ni base superalloy due in its section structure have " nanocrystal ", can improve by leaps and bounds cold plasticity processing
Property.The nanocrystal is easiest to the phase interface of austenite phase (Gamma (γ)) and γ ' phase of the matrix from Ni base superalloy
It generates.Therefore, γ ' moles of rate for increasing Ni base superalloy is related to the increase of above-mentioned phase interface, facilitates nanocrystal
Generation.Also, until the generation of above-mentioned nanocrystal is promoted when γ ' moles of rate reaches 35% level.More preferably
The Equilibrium Precipitation amount of γ ' phase is 40 moles of % or more at being grouped as at 700 DEG C.The Equilibrium Precipitation of further preferred γ ' phase
Amount is 50 moles of % or more, is even more preferably 60 moles of % or more.The Equilibrium Precipitation amount of particularly preferred γ ' phase is rubbed for 63
You are % or more, more preferably 66 moles of % or more, is still more preferably 68 moles of % or more.To at 700 DEG C γ ' phase put down
There is no particular limitation for the upper limit for the amount of precipitation that weighs, and 75 moles of % or so are real.
The Ni base for the precipitation strength type that Equilibrium Precipitation amount as the γ ' phase at 700 DEG C is 35 moles of % or more is super heat-resisting
Alloy, preferably have for example includes C:0~0.25%, Cr:8.0~25.0%, Al:0.5~8.0%, Ti:0.4 in mass
~7.0%, Co:0~28.0%, Mo:0~8%, W:0~6.0%, Nb:0~4.0%, Ta:0~3.0%, Fe:0~
10.0%, V:0~1.2%, Hf:0~1.0%, B:0~0.300%, Zr:0~0.300%, surplus are the group of Ni and impurity
At.
Alternatively, Ni base superalloy preferably has in mass comprising C:0~0.03%, Cr:8.0~22.0%, Al:
2.0~8.0%, Ti:0.4~7.0%, Co:0~28.0%, Mo:2.0~7.0%, W:0~6.0%, Nb:0~4.0%,
Ta:0~3.0%, Fe:0~10.0%, V:0~1.2%, Hf:0~1.0%, B:0~0.300%, Zr:0~0.300%, it is remaining
Amount is the composition of Ni and impurity.
Hereinafter, being said to each ingredient of a mode as Ni base superalloy of the invention preferably formed
Bright (being " quality % " at the unit being grouped as).
Carbon (C)
Contained element of the C as the castability for improving Ni base superalloy in the past.Also, the Ni especially more than γ ' phasor
Base superalloy is typically used as cast member since plastic processing is difficult, is added with a certain amount of C.The C of the addition is being cast
It makes in tissue and is remained in the form of carbide, a part forms coarse eutectic carbide.Also, carbide coarse in this way exists
When carrying out plastic processing to Ni base superalloy, when especially carrying out plastic processing at room temperature, becomes the starting point of crackle and split
The progress path of line generates adverse effect to the plastic processing of Ni base superalloy.
Therefore, for being surpassed using providing the Ni base superalloy more than γ ' phasor as the excellent Ni base of plastic processing
Heat-resisting alloy material and not as the present invention for the purpose of cast member, the reduction of the C in the Ni base superalloy is very heavy
It wants.Also, on the other hand, there is " nanocrystal " in section structure in Ni base superalloy of the invention, so as to
Improve cold plasticity processability by leaps and bounds, therefore can permit the C content for example with the content in cast member with degree.The present invention
The case where preferred C content be set as 0.25% or less.More preferably successively it is set as 0.1% or less, 0.03% or less.Further
Preferably 0.025% hereinafter, be even more preferably 0.02% or less.Particularly preferably less than 0.02%.
For Ni base superalloy of the invention, C is constraint element, and preferred administration is lower.Also, can not also
In the case where adding C (inevitable impurity level), the lower limit of C can be set as to 0 mass %.In general, even if not add C
Ni base superalloy, analyze its at being grouped as when, be able to confirm that such as 0.001% or so C content.
Chromium (Cr)
Cr is the element for improving oxidative resistance, corrosion resistance.But the excessive Cr that contains then forms the equal embrittlement of σ (Sigma)
Phase reduces hot-workability when intensity, preparation blank.Therefore, Cr is for example preferably set to 8.0~25.0%.More preferably 8.0
~22.0%.Preferred lower limit is 9.0%, more preferably 9.5%.Further preferably 10.0%.Additionally, it is preferred that the upper limit be
18.0%, more preferably 16.0%.Further preferably 14.0%.Particularly preferably 12.5%.
Molybdenum (Mo)
Mo facilitates the solution strengthening of matrix, improves the effect of elevated temperature strength.But Mo, which becomes excessive, then forms gold
Compound phase between category and damage elevated temperature strength.Therefore, Mo is preferably that 0~8% (can not also add (inevitable water impurity
It is flat)).More preferably 2.0~7.0%.Further preferred lower limit is 2.5%, more preferably 3.0%.Further preferably
3.5%.In addition, the further preferred upper limit is 6.0%, more preferably 5.0%.
Aluminium (Al)
Al forms the γ ' (Ni as hardening constituent3Al) phase is the essential elements for improving elevated temperature strength.But excessively addition
The reason of making hot-workability when preparing blank reduce, become the faults in material such as the crackle in processing.Therefore, Al is preferably 0.5
~8.0%.More preferably 2.0~8.0%.Further preferred lower limit is 2.5%, more preferably 3.0%.Further preferably
4.0%, it is still more preferably 4.5%.Particularly preferably 5.1%.In addition, the further preferred upper limit is 7.5%, more preferably
It is 7.0%.Further preferably 6.5%.
It should be noted that, in order to ensure preparing hot-workability when blank, reducing Cr due to the relationship with above-mentioned Cr
Content when, can permit the content that the Al of partial response is reduced with it.Also, such as it is set as 13.5% in the upper limit of Cr
When, the lower limit of the content of Al is preferably set to 3.5%.
Titanium (Ti)
Ti and Al is similarly formed γ ' phase, for the element for making the solution strengthening of γ ' phase, improving elevated temperature strength.But excessively add
Add, γ ' mutually becomes unstable at high temperature and incurs the coarsening under high temperature, and forms harmful η (eta) phase, damages standard
Hot-workability when standby blank.Therefore, Ti is for example preferably 0.4~7.0%.In view of generating element, Ni matrix with other γ '
Balance then Ti preferred lower limit be 0.6%, more preferably 0.7%.Further preferably 0.8%.Additionally, it is preferred that the upper limit
It is 6.5%, more preferably 6.0%.Further preferably 4.0%, particularly preferably 2.0%.
Hereinafter, being illustrated to any ingredient that can be added in Ni base superalloy of the invention.
Cobalt (Co)
Co improves the stability of tissue, even if largely containing Ti as intensified element, can also maintain heat when preparing blank
Processability.On the other hand, Co is expensive, therefore cost increase.Therefore, Co by with other element combinations, for example, can be with
One of the arbitrary element that 28.0% range below contains.Preferred lower limit when adding Co can be set as 8.0%.More preferably
It is 10.0%.In addition, the preferred upper limit of Co is set as 18.0%.More preferably 16.0%.It should be noted that can pass through
With γ ' generate element, Ni matrix balance and Co is set as no added horizontal (the inevitable impurity level of raw material), this
The lower limit of Co is considered as 0% in the case of kind.
Tungsten (W)
W and Mo are again it is facilitate one of selection element of the solution strengthening of matrix.But W excessively then formed it is harmful
Intermetallic compound phase and damage elevated temperature strength, therefore for example the upper limit is set as 6.0%.The preferred upper limit is 5.5%, more preferably
It is 5.0%.It can be 1.0% by the lower limit set of W to more reliably play the effect of above-mentioned W.In addition, being added by compound
Add W and Mo, can further play solid solution strengthening effect.The addition of W preferably 0.8% or more when compound addition.It needs to illustrate
, W can be set as no added horizontal (the inevitable impurity level of raw material), this feelings and sufficiently adding Mo
The lower limit of W is considered as 0% under condition.
Niobium (Nb)
Nb is same as Al, Ti, to form γ ' phase, makes one of the solution strengthening of γ ' phase, the selection element for improving elevated temperature strength.
But excessively addition Nb forms harmful δ (delta) phase, damages hot-workability when preparing blank.Therefore, the upper limit example of Nb
Such as it is set as 4.0%.The preferred upper limit is 3.5%, more preferably 2.5%.It should be noted that in order to more reliably play
The lower limit set of Nb is 1.0% by the effect for stating Nb.It is preferred that can be set as 2.0%.Element can be generated by other γ '
Addition and Nb is set as no added horizontal (inevitable impurity level), the lower limit of Nb is considered as 0% in this case.
Tantalum (Ta)
Ta is same as Al, Ti, forms γ ' phase, to make one of the solution strengthening of γ ' phase, the selection element for improving elevated temperature strength.
But then γ ' mutually becomes unstable at high temperature and incurs the coarsening under high temperature excessively addition Ta, and forms harmful η
(eta) phase damages hot-workability when preparing blank.Therefore, the upper limit of Ta is for example set as 3.0%.Preferably 2.5% with
Under.It should be noted that being 0.3% by the lower limit set of Ta to more reliably play the effect of above-mentioned Ta.It can pass through
The γ ' such as Ti, Nb generate the balance of element addition and matrix and Ta are set as no added horizontal (inevitable water impurity
It is flat), the lower limit of Ta is considered as 0% in this case.
Iron (Fe)
Fe is the substitution as Ni, Co of high price and one of the selection element used, and the reduction for cost of alloy is that have
Effect.The effect in order to obtain, deciding whether to be added by the combination with other elements is advisable.But excessively contain Fe
The equal brittle phase of σ (Sigma) is then formed, hot-workability when intensity, preparation blank is reduced.Therefore, the upper limit of Fe is for example set
It is 10.0%.The preferred upper limit is 9.0%, more preferably 8.0%.It on the other hand, can be by generating element, Ni base with γ '
The balance of matter and Fe is set as no added horizontal (inevitable impurity level), the lower limit of Fe is considered as in this case
0%.
Vanadium (V)
V is useful one of the selection element of intercrystalline strengthening that solution strengthening to matrix, carbide generate.But the mistake of V
Degree addition will lead to the generation of the unstable phase of manufacturing process high temperature, will lead to bad to manufacturing and mechanical behavior under high temperature generation
It influences.Therefore, the upper limit of V is for example set as 1.2%.The preferred upper limit is 1.0%, more preferably 0.8%.It needs to illustrate
Being, in order to more reliably play the effect of above-mentioned V, can be 0.5% by the lower limit set of V.Can by with its in alloy
The balance of its alloying element and V is set as no added horizontal (inevitable impurity level), in this case by the lower limit of V
It is considered as 0%.
Hafnium (Hf)
Hf be the oxidative resistance of alloy is improved, selection element that intercrystalline strengthening brought by carbide generates is useful it
One.But the excessive addition of Hf will lead to the generation of manufacturing process oxide, the generation of the unstable phase of high temperature, cause to manufacturing
Adverse effect is generated with mechanical behavior under high temperature.Therefore, the upper limit of Hf is for example set as 1.0%.It should be noted that in order to more really
The effect of above-mentioned Hf is played on the spot, can be 0.1% by the lower limit set of Hf.Can by with other alloying elements in alloy
Balance and Hf is set as no added horizontal (inevitable impurity level), the lower limit of Hf is considered as 0% in this case.
Boron (B)
B is the element for improving grain-boundary strength, improving creep strength, ductility.On the other hand, the effect that B reduces fusing point is big,
In addition, forming hot-workability when coarse boride then hinders preparation blank, therefore such as control is to be no more than 0.300%
It is good.The preferred upper limit is 0.200%, more preferably 0.100%.Further preferably 0.050%, particularly preferably 0.020%.
It should be noted that said effect is preferably minimum in order to obtain contains 0.001%.Preferred lower limit is 0.003%, further
Preferably 0.005%.Particularly preferably 0.010%.B can be set as and the balance with other alloying elements in alloy
No added level (inevitable impurity level), is considered as 0% for the lower limit of B in this case.
Zirconium (Zr)
Zr is same as B to be had the effect of improving grain-boundary strength.On the other hand, Zr excessively then will lead to the drop of fusing point really
It is low, hinder hot-workability when elevated temperature strength, preparation blank.Therefore, the upper limit of Zr is for example set as 0.300%.On preferred
It is limited to 0.250%, more preferably 0.200%.Further preferably 0.100%, particularly preferably 0.050%.It needs to illustrate
It is that said effect is preferably minimum in order to obtain contains 0.001%.Preferred lower limit is 0.005%, further preferably
0.010%.Zr can be set as no added horizontal (inevitably miscellaneous and the balance with other alloying elements in alloy
Matter is horizontal), the lower limit of Zr is considered as 0% in this case.
Surplus other than element described above is Ni, also may include inevitable impurity.
Ni base superalloy of the invention is that 75nm is below " nanocrystalline due to having maximum gauge in its section structure
Grain ", therefore the plastic processing under cool condition can be improved by leaps and bounds.Not yet abundant clearly mechanism.However, it is believed that institute as above
The phase interface for stating γ phase and γ ' phase facilitates the generation of nanocrystal.Also, the nanocrystal of the generation is with plastic processing rate
And its quantity also increases and it generates Grain Boundary Sliding or Crystal Rotation to realize the plastic deformation of Ni base superalloy, with
Previous is compared based on the generation of dislocation with the plastic deformation that the crystal of proliferation slides, and there are the different possibility of the mechanism of its deformation
Property.As a fact for implying the possibility, the present inventor's confirmation, which has, is carrying out aftermentioned cool condition to Ni base superalloy
Under plastic processing when, nanocrystal once generation, then by further progress plastic processing (make plastic processing rate increase
Add) and increase the quantity of nanocrystal, but it (also includes the feelings of several increases that the hardness of alloy does not increase with plastic processing rate
Condition) but " substantially certain " (for example, for above-mentioned γ ' moles of rate be 35 moles of % or more Ni base superalloy when be 500HV
More than).The phenomenon implies the rising of dislocation density caused by without generating plastic processing.
The size for so facilitating the nanocrystal of the raising of plastic processing is the section structure of Ni base superalloy
In " maximum gauge be 75nm or less ".Also, the maximum gauge be the such crystal grain of 75nm or less size can be different from
Toward the size of crystal grain seen in common technique.At this point, above-mentioned section structure can be from along its length when being, for example, wire rod
It takes in the section (that is, section of the central axis comprising wire rod) of bisection.And the section for example can be respectively from the table of wire rod
The position in face, from the surface of wire rod to central axis go deep into the position (D is line footpath) of 1/4D and the central axis of wire rod position cut
It takes in face.Also, one of these respective sections, or both more than section structure confirmation there are above-mentioned nanocrystals
?.
It should be noted that when even the shape other than wire rod is also halved with above-mentioned same observation along its length
Section.
There is in Ni base superalloy section structure of the invention receiving for " maximum gauge being 75nm or less " as described above
Rice crystal grain.Maximum gauge in the section structure is 75nm nanocrystal below preferably at every 1 μm2There are 5 in section structure
More than a.Increased by nanocrystal, the medium for playing the role of plastic deformation increases, and plastic processing further increases.Into one
Step is preferably, and maximum gauge is 75nm crystal grain below at every 1 μm2There are 10 or more in section structure, it is more preferably the presence of
50 or more, further preferably there are 100 or more.And still more preferably it is followed successively by 200 or more, 300 or more.On
The total number of the nanocrystal confirmed in the gross section tissue that a number density for the nanocrystal stated can will be observed that is removed
It is averagely found out with the whole field areas observed.
It should be noted that being 75nm nanocrystal below, maximum gauge for the maximum gauge in section structure
Lower limit do not need special setting.Also, the maximum gauge in section structure is the presence or absence of 75nm nanocrystal below, a
Numerical example such as can use the confirmation of EBSD picture.Also, it is set as scanning step from by the determination condition of EBSD: 0.01 μm, by crystal grain
It is defined as when 15 ° of misorientation or more of crystal boundary among identifiable crystal grain, extraction maximum gauge is that 75nm is below nanocrystalline
Grain counts.Also, the presence or absence of the nanocrystal that maximum gauge is about 25nm or more as an example, can be confirmed and number.
Such Ni base superalloy preferably has the hardness of 500HV or more.
By observing Ni base superalloy of the invention above since the plastic processing under cool condition is excellent,
It can be as " cold plasticity processing purposes ".
In addition, Ni base superalloy of the invention can be used as the " line for carrying out the intermediate shape of cold plasticity processing
Material (wire material) ".Wire rod refers to that its line footpath (diameter) is the such material of such as 10mm or less, 8mm or less, 6mm or less
Material, the final material thin in this way for 5mm or less, 4mm or less, 3mm or less, 2mm or less.Also, wire rod refers to that its length is opposite
In the line footpath of above-mentioned wire rod be, for example, 10 times or more, 50 times or more, 100 times or more materials long in this way.
In addition, Ni base superalloy of the invention can be used as the final product shape processed using above-mentioned cold plasticity
" filament (the wire product) " of shape.Filament refer to its line footpath (diameter) be, for example, 5mm or less, 4mm or less, 3mm or less this
The material of sample, the final material thinner in this way for 2mm or less, 1mm or less.Also, filament refers to its length relative to above-mentioned thin
The line footpath of line is, for example, 50 times or more, 100 times or more, 300 times or more materials longer in this way.
Then, illustrate to obtain with mentioned component composition, having maximum gauge in section structure is 75nm crystalline substance below
The manufacturing method of the Ni base superalloy of the invention of grain.The manufacturing method includes: preparatory process, prepares have mentioned component
The blank (raw material) of the Ni base superalloy of composition;And manufacturing procedure, with 500 DEG C of temperature below to the blank
Multiple plastic processing is carried out, so that accumulative working modulus is 30% or more.By improving " working modulus " of the compression process, Ni is found
" nanocrystal " can be formed in base superalloy materials microstructure.
Illustrate the manufacturing method.
The blank of Ni base superalloy is also possible to make the smelting process of ingot casting by the way that melt to be poured into mold
Obtained material.Also, the manufacture for ingot casting, for example, can be suitable for by vacuum melting and vacuum induction melting, electroslag remelting
Etc. conventional methods combination etc. carry out.In addition, blank can be the material obtained using powder metallurgic method.Also, to above-mentioned casting
Ingot, the alloy block made of powder metallurgic method implement hot-working, machining as needed, can be processed into defined shape,
For example, the blank of the shape of billet (billet), bar (bar material).
Then, it carries out adding up the plastic processing that working modulus is 30% or more at 500 DEG C of temperature below.The present invention and previous
" utilizing heat " plastic processing it is different, by " cold " plastic processing, can be generated in the tissue of Ni base superalloy
Nanocrystal and obtain the excellent Ni base superalloy of plastic processing.In order to reach the purpose, above by cold plasticity
Processing needs that the low temperature region restored or recrystallized does not occur in the plastic processing.Therefore, in plastic processing preferably not
It is heat-treated.Heat treatment described herein refers in the heat treatment for restoring or recrystallizing the such high-temperature region of generation, example
Such as it is heated to the heat treatment of the temperature more than 500 DEG C.
Above-mentioned plastic processing temperature of the invention is set as " 500 DEG C or less " and is important.Preferably 300 DEG C hereinafter, more
Preferably 100 DEG C hereinafter, further preferably 50 DEG C or less (for example, room temperature).
The manufacture of known Ni base superalloy described above can be applied to wire-form, plate, band etc..And
It is known at this point, Ni base superalloy of the invention is wire rod, plate (sheet material), band (strip
It material can also be filament, thin plate (sheet product), strip (strip except intermediate shape)
Product final product shape).The relationship of plate (thin plate), band (strip), size can be by above-mentioned wire rod (filament)
When line footpath replace with plate thickness or with thickness.
Especially when the blank of Ni base superalloy is bar, in order to form above-mentioned nanocrystal, bar situation can
Bar processing is carried out to compress sectional area.At this point, as being starting material, to the bar with " bar " of Ni base superalloy
The mode of plastic processing is carried out, " the length direction of compression and bar that can assign uniform pressure in bar is preferably implemented
The processing of the sectional area in vertical section ".Also, plasticity compression sectional area (stick diameter) is carried out to the blank of the bar, is stretched
The processing of length.Especially when obtaining the wire rod of Ni base superalloy, comparison wire rod sectional area (diameter) big " bar " into
Row plastic processing is effective to make.Accumulative working modulus is carried out from the periphery of bar towards axle center with 500 DEG C of temperature below
For 30% or more plastic processing, the sectional area of bar is compressed.As processing so, there are swaged forging (swaging), boxlike roller
Die wire drawing, orifice type dies wire drawing etc..
On the other hand, rolling processing can be used for the manufacture of plate, the band of Ni base superalloy etc..
For the formation of nanocrystal, the accumulative working modulus of above-mentioned plastic processing up to " 30% or more " in the present invention.It is tired
Counting working modulus is preferably 40% or more, this makes above-mentioned nanocrystal at every 1 μm2The number generated in section structure is such as 10
More than a, therefore it is preferred that.
Also, accumulative working modulus is more preferably 60% or more, for this number for generating above-mentioned nanocrystal
Such as 50 or more, therefore it is preferred that.It more preferably 70% or more, is more preferably 80% or more, this keeps above-mentioned nanocrystal raw
At number be such as 100 or more, therefore it is preferred that.It is still more preferably 90% or more, particularly preferably 97% or more, these
The number that accumulative working modulus successively generates above-mentioned nanocrystal such as 200 or more, 300 or more, therefore it is preferred that.
Herein, working modulus is indicated when bar is carried out swaged forging, mold wire drawing by sectional shrinkage.Sectional shrinkage
With the sectional area A of the bar before plastic processing0With the sectional area A of wire rod, filament after plastic processing1Relational expression calculate.
[(A0-A1)/A0] × 100 (%) (1)
On the other hand, when carrying out rolling processing, working modulus is indicated with reduction ratio.Reduction ratio is by the base before plastic processing
The thickness of material is set as t0, plate by after plastic processing, band, thin plate, strip thickness be set as t1When formula calculate.
[(t0-t1)/t0] × 100 (%) (2)
Accumulative working modulus indicate repeatedly to carry out plastic processing or the blank to final machining object when through multi-pass plus
Work rate.
The mechanism that nanocrystal generates in tissue is not yet completely clear.But in order to sufficiently generate nanocrystal, test is true
Fixed above-mentioned working modulus subsistence level is 30% or so (referring to embodiment).That is, the bar to above-mentioned Ni base superalloy carries out
Cold plasticity processing observes nanocrystal initially preferentially in the phase of γ phase and γ ' phase when it adds up working modulus and reaches about 30%
Interface generates.Also, the Ni base superalloy (for example, bar (wire rod)) for once generating the nanocrystal is further applied
The quantity for adding cold plasticity to process then nanocrystal increases, which makes Ni base superalloy (for example, bar (line
Material)) plastic processing further increase.Also, by repeating the plastic processing (by the increase of accumulative working modulus), Ni
The plastic processing of base superalloy (for example, bar (wire rod)) more improves, be confirmed as can with plastic processing midway not into
Row heat treatment, add up under cool condition working modulus reach 97% or more plastic processing is such, " room temperature is superplastic " plasticity adds
The phenomenon that work.
The plastic processing of the working modulus of above-mentioned " 30% an or more " not instead of plastic processing is completed, until tissue
During middle formation nanocrystal, for example, in order to inhibit alloy to crack, the completion of plastic processing several times such as flaw is preferred.It will
" big strain " plastic processing several times of 30% or more working modulus is imparted in blank, to effectively make the strain in base
Suitably disperse in material, Grain Boundary Sliding, the Crystal Rotation of above-mentioned nanocrystal are uniformly generated in blank.As a result, base can be made
The generation for uniformly and equably forming nanocrystal in material and crackle, flaw in the plastic processing can also being inhibited etc..Point
When multiple plastic processing, do not need to be heat-treated during each plastic processing.Also, to above-mentioned 30% or more working modulus
The upper limit do not set especially, such as according to intermediate, shape of final product etc. can be suitable for setting.If also, preparing
Aftermentioned alloy material, according to its specification etc., for example, it can be set to being numerical value as 50%, 45%, 40%, 35%.
In addition, making the working modulus (sectional shrinkage) in certain arbitrary plastic processing (passage) when plastic processing several times
Processing efficiency can be improved greater than the working modulus (sectional shrinkage) in its previous plastic processing (passage).It can also be gradually
Increase the working modulus (sectional shrinkage) of each plastic processing (passage).
For " passage " in the present invention, can by above-mentioned swaged forging, mold wire drawing, roll in the plastic processing of these types
Using (or a pair of) mold, roller plastic processing when be denoted as " 1 passage ".
Especially when the blank of Ni base superalloy is bar, for the formation of nanocrystal, it is believed that in above-mentioned plasticity
In processing, applies uniform and impartial pressure in bar and be important.Also, it therefore towards axle center is pressed from the periphery of bar
The plastic processing of the sectional area of contracting bar is effective.At this point, not needing to limit plastic processing mode.Wherein, add to through plasticity
The complete cycle of the bar of work is equably applied stressed plastic processing mode and is advantageous.As the concrete example, swaged forging can be enumerated
Processing.Swaged forging processing is to make to surround multiple molds rotation of the complete cycle of bar on one side, forges the outer peripheral surface of bar on one side, therefore right
The generation of nanocrystal is preferred.In addition it is also possible to using other plastic processings such as boxlike roller die wire drawing, orifice type dies wire drawings.
Situation of the invention, can carrying out the heating of the blank (such as bar) before above-mentioned plastic processing, to be maintained at γ ' solid
The temperature Th of solubility temperature (solvus temperature) Ts or more is simultaneously cooling to be heat-treated.By carrying out the heat treatment, blank can be made
Tissue in γ ' phase is equably precipitated again.It becomes easy to form nanocrystal in the tissue after plastic processing as a result,.Think this
It is because the phase interface of γ phase and γ ' phase that Ni base superalloy has becomes uniformly, to promote the shape of nanocrystal
At.
It is preferably 10 DEG C higher than solvus temperature Ts or more of high temperature that above-mentioned heating, which keeps temperature Th,.Also, it does not need to set
Heating keeps the upper limit of temperature Th.Heating keeps temperature Th theoretically to start melting less than the blank of Ni base superalloy
Temperature (solidus temperature).Kept for the retention time of the bar after temperature Th be preferably set to 2 hours in addition, reaching above-mentioned heating
More than.It and was real for 10 hours or less.Preferably 7 hours or less.More preferably 4 hours or less.As a result, at grouping
Also effective (equal thermal effect) at homogenization.
Other specific examples according to the present invention, providing manufacture has the side of Ni base superalloy of mentioned component composition
Method.This method comprises: preparatory process, preparing has maximum gauge in the section structure that hardness is 500HV or more be 75nm or less
Crystal grain alloy material (alloy material);And manufacturing procedure, aforementioned blank is moulded with 500 DEG C of temperature below
Property process and obtain hardness be 500HV or more alloy.It herein, is above description as the alloy material of the starting material of processing
Ni base superalloy of the invention, for example, above explained wire rod, plate, band.It is below with 500 DEG C in the present invention
It is super heat-resisting with the Ni base that maximum gauge is 75nm crystal grain below in the section structure that temperature is 500HV or more to above-mentioned hardness
When plastic processing is repeated in alloy, it is found that the nanocrystal in the section structure of its midway gradually increases (lasting to be formed), dimension
The phenomenon that holding plastic processing.At this point, the hardness of alloy maintains 500HV or more, or slightly increase.It is of the invention as a result, " to cut
With nanocrystal in covering weave " plastic processing of Ni base superalloy in the early stage is excellent and its excellent plasticity adds
Work also maintains down in next plastic processing.Also, the Ni base superalloy of whole plastic processings is completed in section
Also there is nanocrystal in tissue, the filament, thin plate, strip of final product shape can be made into.
Ni base superalloy after plastic processing is γ phase and γ ' hands down, and extending direction is elongated to filum.But
After plastic processing is at defined size, shape, when being supplied in the form of final product, as needed, it is possible to implement heat treatment is to make
At desired equiaxed crystal tissue.By the heat treatment, for example, hardness can be adjusted to less than 500HV, it easily will most
Whole product, which is bent or cuts into, meets transport form, the form using form.
It is processed by the manufacturing method, such as only by cold plasticity, by the intermediates shape such as above-mentioned wire rod, plate, band
The material of shape can also provide the Ni base until various forms of the material of final products shape such as filament, thin plate, strips
Superalloy.
Embodiment 1
The melt prepared using vacuum melting is cast, the columned Ni base of production diameter 100mm, quality 10kg
The ingot casting of superalloy A.Ni base superalloy A's is shown in table 1 at (quality %) is grouped as.Above-mentioned casting is also showed that in table 1
" γ ' moles of rate " of ingot and " γ ' solid solubility temperature (solvus temperature) Ts ".These values use commercially available thermodynamic balance calculation software
" JMatPro (Version 8.0.1, Sente Software Ltd. company manufacture) " calculates.In the calculation of thermodynamic equilibrium
The content for each element that input table 1 is enumerated in software finds out above-mentioned " γ ' moles of rate " and " γ ' solid solubility temperature Ts ".To the Ni base
The ingot casting of superalloy A is implemented to keep Th:1200 DEG C of temperature, retention time: heat treatment in 8 hours, after furnace is cold, along the ingot casting
The parallel direction of length direction take the bar of diameter 6.0mm, length 60mm, using the bar as the base for being used for plastic processing
Material.The hardness of the bar is 320HV." swaged forging processing 1 " (table that working modulus is 31% is carried out to the bar under room temperature (25 DEG C)
Processing documented by 2 alloy 1-2), make the wire rod (line footpath 5.0mm) of the Ni base superalloy of example 1 of the present invention.The present invention
The wire rod of the Ni base superalloy of example 1 makes in which can keep good surface state.Also, the Ni base of example 1 of the present invention is super
The hardness of the wire rod of heat-resisting alloy is 595HV.It should be noted that working modulus is found out by above explained formula (1).
[table 1]
It * include inevitable impurity.
Fig. 1 is the figure for indicating the EBSD picture of the section microscopic structure of the wire rod of alloy No.1-2 of example of the present invention.The section
Microscopic structure is to go deep into the position of 1/4D from the surface of wire rod to central axis along the section that the length direction of wire rod is halved
The tissue (line footpath of D expression wire rod) that the section of (position A) is taken.Also, the determination condition of EBSD is using scanning electron
Subsidiary EBSD measures system " OIM Version 5.3.1 (TSL in microscope " ULTRA55 (manufacture of Zeiss company) "
The manufacture of Solution company) ", be set as multiplying power: 10000 times, scanning step: 0.01 μm, the definition of crystal grain is by 15 ° of misorientation
It is used as crystal boundary above.At this point, the maximum gauge (maximum length) of the nanocrystal confirmed in EBSD picture, small about 25nm,
Confirm the presence or absence of nanocrystal of maximum gauge of the value or more and number.According to Fig. 1, the line of the alloy No.1-2 of example of the present invention
It is 75nm nanocrystal below (for example, having dark point in circle encirclement) that material has maximum gauge in its section is knitted.Along conjunction
In the section that the length direction of the wire rod of golden No.1-2 is halved, section and wire rod from the position (position B) on the surface of wire rod
The section of position (position C) of central axis take tissue, parsed as described above using EBSD.Also, respectively from position
It sets A, B, C and takes the section structure amounted at 6 at 2, be with counting maximum gauge in Fig. 1 same field of view area (2 3 μm of μ m)
The sum of 75nm nanocrystal below is divided by (6 μm of total visual field area2× 6) per unit area of above-mentioned nanocrystal is found out
A number density be " 8/μm2”。
On the other hand, swaged forging processing being carried out to alloy No.1-1 under room temperature (25 DEG C), the line footpath after processing is 5.5mm,
Working modulus (sectional shrinkage) is 16.0%.The section microscopic structure is observed according to main points same as alloy No.1-2,
As a result as shown in fig. 6, not observing that maximum gauge is 75nm nanocrystal below.In addition, hardness is also 480HV.
The wire rod of the alloy No.1-2 of example of the present invention is carried out shown in table 2 while successively accumulating under room temperature (25 DEG C)
Working modulus " swaged forging processing 3~10 ", make respectively from bar keep accumulative working modulus increased from alloy No.1-3 to
The wire rod of the Ni base superalloy of alloy No.1-10.It should be noted that between each swaged forging processing without heat at
Reason.It is made with can keeping good surface state from alloy No.1-3 to the wire rod of alloy No.1-10.Also, these lines
It is 75nm nanocrystal below (particle that black is seen in figure) that material also has maximum gauge in its section structure.Fig. 2~
Fig. 5 successively indicates the EBSD of the section microscopic structure of alloy No.1-4, No.1-5, No.1-7, No.1-9 of example of the present invention respectively
Picture.The section microscopic structure takes the determination condition of position and EBSD identical as the main points of Fig. 1.And it to these wire rods, presses
The per unit area for the 75nm nanocrystal below having in its section structure is measured according to main points identical as alloy No.1-1
A number density.In addition, also measuring the hardness of wire rod.Result by these measurement results together with example 1 of the present invention is shown in table 2.
[table 2]
According to the result of table 2 it is found that further applying cold plasticity to the Ni base superalloy for once generating nanocrystal
Processing, so that the number of nanocrystal increases.But the number of nanocrystal increases, and the hardness of Ni base superalloy is not
Increase with plastic processing rate and is constant.Therefore, using swaged forging processing can carry out in cold conditions plastic processing until
Line footpath is the wire rod of the example No.1-10 of the present invention of 1.0mm.Starting material is made (that is, hard as the wire rod of alloy No.1-2
Degree be 500HV or more section structure in have maximum gauge be 75nm crystal grain below alloy material) when, can carry out from
The accumulative working modulus that the wire rod of the alloy material rises is 96%, is then 97% if the accumulative working modulus from initial pieces of bar stock
Cold plasticity processing.Further, the wire rod of the alloy No.1-10 of example of the present invention is the plastic processing in above-mentioned big accumulative working modulus
It later can be with the state of the plastic processing under further progress cool condition.I.e. it is found that alloy after the processing of example of the present invention
Hardness unrelated with working modulus is constant (595HV~605HV), thus once being formed maximum gauge be 75nm crystal grain below and
The alloy material of hardness with 500HV or more can continue to be cold worked.
Embodiment 2
The melt prepared using vacuum melting is cast, the columned Ni base of production diameter 100mm, quality 10kg
The ingot casting of superalloy B.Ni base superalloy B's is shown in table 3 at being grouped as (quality %)." γ ' moles shown in table 3
Rate " and " γ ' solid solubility temperature Ts " also using commercially available thermodynamic balance calculation software " JMatPro (Version 8.0.1,
Sente Software Ltd. company manufacture) it calculates.The ingot casting of Ni base superalloy B is implemented to keep temperature Th:
1250 DEG C, retention time: heat treatment in 8 hours after furnace is cold, takes diameter along the direction parallel with the length direction of the ingot casting
The bar of 6.0mm, length 60mm, using the bar as the blank for being used for plastic processing.The hardness of the bar is 381HV.With reality
It applies example 1 and swaged forging processing is successively equally carried out to the bar, make the wire rod of alloy No.2-1~No.2-6.
[table 3]
It * include inevitable impurity.
According to the result of table 4, line footpath of the wire rod of alloy No.2-1 after swaged forging processing is 5.5mm, and working modulus (is received in section
Shrinkage) it is 16.0%.Do not observe that maximum gauge is 75nm nanocrystal below in the section microscopic structure.In addition, hardness
It also is 494HV.
On the other hand, the working modulus (sectional shrinkage) of the wire rod of alloy No.2-2~No.2-6 is 30% or more, is existed
Observe that maximum gauge is 75nm nanocrystal below in its section structure, with the increase of working modulus, of nanocrystal
Number density also increases.The hardness of these alloys is 500HV or more, but different from the result of embodiment 1, with the increasing of working modulus
Add, discovery hardness has the tendency being slightly increased.The wire rod of further processing is the hardness of 600HV or more.
[table 4]
Embodiment 3
The melt prepared using vacuum melting is cast, the columned Ni base of production diameter 100mm, quality 10kg
The ingot casting of superalloy C.Ni base superalloy C's is shown in table 5 at being grouped as (quality %)." γ ' moles shown in table 5
Rate " and " γ ' solid solubility temperature Ts " also using commercially available thermodynamic balance calculation software " JMatPro (Version 8.0.1,
Sente Software Ltd. company manufacture) it calculates.The ingot casting of Ni base superalloy C is implemented to keep temperature Th:
Heat treatment in 1200 DEG C × retention time: 8 hours after furnace is cold, takes diameter along the direction parallel with the length direction of the ingot casting
The bar of 6.0mm, length 60mm, using the bar as the blank for being used for plastic processing.The hardness of the bar is 389HV.With reality
It applies example 1 and swaged forging processing is successively equally carried out to the bar, make the wire rod of alloy No.3-1~No.3-10.
[table 5]
* comprising can not to avoid impurity.
According to the result of table 6, line footpath of the wire rod of alloy No.3-1 after swaged forging processing is 5.5mm, and working modulus (is received in section
Shrinkage) it is 16.0%.Do not observe that maximum gauge is 75nm nanocrystal below in the section microscopic structure.In addition, hardness
It also is 468HV.
The working modulus (sectional shrinkage) of the wire rod of alloy No.3-2~No.3-10 is 30% or more, in its section group
Observe that maximum gauge is 75nm nanocrystal below in knitting, with the increase of working modulus, a number density of nanocrystal
Increase.The hardness of these alloys is 500HV or more, but similarly to Example 1, and unrelated with working modulus is constant (524HV
~542HV).
[table 6]
Embodiment 4
With the wire rod (line footpath 1.5mm) of the alloy No.1-9 of embodiment 1 be starting material, under room temperature (25 DEG C) to its into
The orifice type dies wire drawing of 4 passage of row, halfway through alloy No.4-1 (line footpath 1.35mm), 4-2 (line footpath 1.20mm), 4-3 (line
Diameter 1.05mm) wire rod, the final wire rod (line footpath 0.95mm) for making alloy No.4-4.Can carry out without problems processing until
Wire rod of the diameter less than 1mm.It should be noted that without heat treatment between each passage.Working modulus passes through above explained formula (1)
It finds out.
Midway between above-mentioned 4 passage, the hardness of alloy No.4-1,4-2,4-3 are followed successively by 593HV, 602HV, 598HV.
Also, any wire rod observes that maximum gauge is 75nm nanocrystal below in its section structure, with working modulus
Increase, a number density of nanocrystal also increases.Also, as shown in table 7, the conjunction that the mold wire drawing of 4 passages terminates
The wire rod of golden No.4-4 is in its section structure, and every 1 μm2Observe that 620 maximum gauges are 75nm nanocrystal below, firmly
Degree is 593HV.Also, the hardness of the wire rod of alloy No.4-1~4-4 is 500HV or more, similarly to Example 1, with processing
Unrelated rate is constant (593HV~602HV).
[table 7]
More than, the plastic processing of the Ni base superalloy of each embodiment is excellent, and the Ni base of example of the present invention is super heat-resisting
Alloy carries out cold plasticity processing, so that confirmation can be processed into the wire rod of any line footpath.The present embodiment manufactures wire rod, but
These wire rods can of course be processed into the filament of final product shape.Also, the plasticity of Ni base superalloy of the invention adds
Work is excellent, it may thus be appreciated that can also be with plastic processing at the shape other than wire rod, filament.
Claims (17)
1. a kind of Ni base superalloy has the ingredient that the Equilibrium Precipitation amount of the γ ' phase at 700 DEG C is 35 moles of % or more
Composition, having maximum gauge in section structure is 75nm crystal grain below.
2. Ni base superalloy according to claim 1, wherein the Ni base superalloy has 500HV or more
Hardness.
3. Ni base superalloy according to claim 1 or 2, wherein at every 1 μm2There are 5 or more in section structure
The maximum gauge is 75nm crystal grain below.
4. Ni base superalloy described in any one of claim 1 to 3, wherein the Ni base superalloy with
Quality % is counted
C:0~0.25%,
Cr:8.0~25.0%,
Al:0.5~8.0%,
Ti:0.4~7.0%,
Co:0~28.0%,
Mo:0~8%,
W:0~6.0%,
Nb:0~4.0%,
Ta:0~3.0%,
Fe:0~10.0%,
V:0~1.2%,
Hf:0~1.0%,
B:0~0.300%,
Zr:0~0.300%,
Surplus is Ni and impurity.
5. Ni base superalloy according to any one of claims 1 to 4 has the balance of the γ ' phase at 700 DEG C
Amount of precipitation is 40 moles of % or more at being grouped as.
6. Ni base superalloy according to any one of claims 1 to 5, wherein the Ni base superalloy with
Quality % is counted
C:0~0.03%,
Cr:8.0~22.0%,
Al:2.0~8.0%,
Ti:0.4~7.0%,
Co:0~28.0%,
Mo:2.0~7.0%,
W:0~6.0%,
Nb:0~4.0%,
Ta:0~3.0%,
Fe:0~10.0%,
V:0~1.2%,
Hf:0~1.0%,
B:0~0.300%,
Zr:0~0.300%,
Surplus is Ni and impurity.
7. the method for Ni base superalloy described in a kind of any one of manufacturing claims 1~6 comprising:
Preparatory process prepares have the blank at the Ni base superalloy being grouped as;With
Manufacturing procedure carries out multiple plastic processing to the blank with 500 DEG C of temperature below, so that accumulative working modulus is 30%
More than.
8. the blank has the shape of bar according to the method described in claim 7, wherein,
The multiple plastic processing that the accumulative working modulus is 30% or more is to make the processing of the reduced cross-sectional area of the bar.
9. according to the method described in claim 8, wherein, the plastic processing include from the periphery of the bar towards axle center into
The process of row compression.
10. the method according to any one of claim 7~9, wherein without heat between the multiple plastic processing
Processing.
11. it is the super at the Ni base being grouped as of 35 moles of % or more that a kind of manufacture, which has the Equilibrium Precipitation amount of the γ ' phase at 700 DEG C,
The method of heat-resisting alloy comprising:
Preparatory process prepares hardness and is 500HV or more, there is maximum gauge to be the conjunction of 75nm crystal grain below in section structure
Golden material;With
Manufacturing procedure carries out plastic processing to the alloy material with 500 DEG C of temperature below, and obtaining hardness is 500HV or more
Alloy.
12. according to the method for claim 11, wherein repeated multiple times to carry out the manufacturing procedure.
13. according to the method for claim 12, wherein without heat treatment between the multiple manufacturing procedure.
14. method described in any one of 1~13 according to claim 1, wherein in the alloy material and the alloy,
At every 1 μm2It there are 5 maximum gauges described above is 75nm crystal grain below in section structure.
15. method described in any one of 1~14 according to claim 1, wherein the Ni base superalloy is in terms of quality %
Include
C:0~0.25%,
Cr:8.0~25.0%,
Al:0.5~8.0%,
Ti:0.4~7.0%,
Co:0~28.0%,
Mo:0~8%,
W:0~6.0%,
Nb:0~4.0%,
Ta:0~3.0%,
Fe:0~10.0%,
V:0~1.2%,
Hf:0~1.0%,
B:0~0.300%,
Zr:0~0.300%,
Surplus is Ni and impurity.
16. method described in any one of 1~15 according to claim 1, wherein have the Equilibrium Precipitation of the γ ' phase at 700 DEG C
Amount is 40 moles of % or more at being grouped as.
17. method described in any one of 1~16 according to claim 1, wherein the Ni base superalloy is in terms of quality %
Include
C:0~0.03%,
Cr:8.0~22.0%,
Al:2.0~8.0%,
Ti:0.4~7.0%,
Co:0~28.0%,
Mo:2.0~7.0%,
W:0~6.0%,
Nb:0~4.0%,
Ta:0~3.0%,
Fe:0~10.0%,
V:1.2% or less,
Hf:0~1.0%,
B:0~0.300%,
Zr:0~0.300%,
Surplus is Ni and impurity.
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EP (1) | EP3587606A4 (en) |
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Also Published As
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JPWO2018155446A1 (en) | 2019-02-28 |
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EP3587606A4 (en) | 2020-08-12 |
JP6422045B1 (en) | 2018-11-14 |
EP3587606A1 (en) | 2020-01-01 |
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