CN109789457A - Ni base superalloy squeezes out the manufacturing method of material and Ni base superalloy squeezes out material - Google Patents
Ni base superalloy squeezes out the manufacturing method of material and Ni base superalloy squeezes out material Download PDFInfo
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- CN109789457A CN109789457A CN201780060401.8A CN201780060401A CN109789457A CN 109789457 A CN109789457 A CN 109789457A CN 201780060401 A CN201780060401 A CN 201780060401A CN 109789457 A CN109789457 A CN 109789457A
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- 229910000601 superalloy Inorganic materials 0.000 title claims abstract description 83
- 239000000463 material Substances 0.000 title claims abstract description 69
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 238000001125 extrusion Methods 0.000 claims abstract description 69
- 238000001556 precipitation Methods 0.000 claims abstract description 62
- 238000005266 casting Methods 0.000 claims abstract description 38
- 239000013078 crystal Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 230000008569 process Effects 0.000 claims abstract description 12
- 239000000155 melt Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 abstract description 22
- 230000000694 effects Effects 0.000 description 19
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 13
- 239000012535 impurity Substances 0.000 description 12
- 239000002994 raw material Substances 0.000 description 9
- 238000005728 strengthening Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 238000004364 calculation method Methods 0.000 description 6
- 206010037660 Pyrexia Diseases 0.000 description 5
- 208000037656 Respiratory Sounds Diseases 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 5
- 239000000956 alloy Substances 0.000 description 5
- 238000001953 recrystallisation Methods 0.000 description 5
- 229910052721 tungsten Inorganic materials 0.000 description 5
- 229910000765 intermetallic Inorganic materials 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000007711 solidification Methods 0.000 description 4
- 230000008023 solidification Effects 0.000 description 4
- 229910052715 tantalum Inorganic materials 0.000 description 4
- 229910052720 vanadium Inorganic materials 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 230000008602 contraction Effects 0.000 description 3
- 238000001887 electron backscatter diffraction Methods 0.000 description 3
- 229910052735 hafnium Inorganic materials 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- 229910010038 TiAl Inorganic materials 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 206010011376 Crepitations Diseases 0.000 description 1
- 229910001005 Ni3Al Inorganic materials 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 240000005373 Panax quinquefolius Species 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000000116 mitigating effect Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000005482 strain hardening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C23/00—Extruding metal; Impact extrusion
- B21C23/002—Extruding materials of special alloys so far as the composition of the alloy requires or permits special extruding methods of sequences
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C23/00—Extruding metal; Impact extrusion
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C23/00—Extruding metal; Impact extrusion
- B21C23/21—Presses specially adapted for extruding metal
- B21C23/212—Details
-
- 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
-
- 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%
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Extrusion Of Metal (AREA)
- Forging (AREA)
Abstract
The Ni base superalloy that the present invention provides the precipitation strength type more than γ ' phase squeezes out the manufacturing method of material and Ni base superalloy squeezes out material.A kind of Ni base superalloy squeezes out the manufacturing method of material, it includes the 1st process, using by the Equilibrium Precipitation amount for the γ ' phase having at 700 DEG C be 40 moles of % or more precipitation strength type Ni base superalloy at be grouped as melt casting obtained from ingot casting as blank, by the blank heating to the hot processing temperature for being set as 1030 DEG C of γ ' phase solid solubility temperatures more than or lower than above-mentioned Ni base superalloy;With the 2nd process, the blank that will warm up above-mentioned hot processing temperature is inserted into ingot-containing tube, compressing force is applied to blank from the one end of the ingot-containing tube, blank is squeezed out from the hole of the mold for the another side for being set to ingot-containing tube with the extruded velocity of 10~300mm/s, obtains the extrusion material of Ni base superalloy.It is formed in addition, Ni base superalloy squeezes out material with mentioned component, the average crystal grain diameter in section structure is calculated as 20 μm or less with equivalent circle diameter.
Description
Technical field
The manufacturing method of material is squeezed out the present invention relates to Ni base superalloy and Ni base superalloy squeezes out material.
Background technique
So far, (high using heat resistance in the material of the component parts of aircraft engine, power generation gas turbine etc.
Warm intensity) excellent " precipitation strength type " Ni base superalloy.The Ni base superalloy of precipitation strength type is to utilize work
For by Ni3Al、Ni3Ti、Ni3(TiAl) " the gamma of the precipitation strength phase of the intermetallic compound typically indicated such as
Prime (γ ') phase (hereinafter also referred to as " γ ' phase ".) " alloy of the reinforcing of Lai Shixian Ni base superalloy.Moreover, in order to
The heat resistance of the Ni base superalloy of the precipitation strength type is further increased, it is effective for increasing the amount of above-mentioned γ ' phase.
A part of such component parts is made by " squeezing out (extrusion) ".Extrusion refers to following method: example
Such as, the blank that will warm up hot processing temperature is inserted into ingot-containing tube, applies from the one end of the ingot-containing tube to above-mentioned blank and compresses
Power squeezes out blank from the hole of the mold for the another side for being set to ingot-containing tube, obtains squeezing out material.Moreover, as precipitation strength
The Ni base superalloy of type squeezes out the manufacturing method of material, proposes to the Ni base superalloy with precipitation strength type
" ingot casting (ingot bar) " obtained from being cast at the melt being grouped as is blank, is squeezed out to the blank made of the ingot casting
Method (patent document 1).
Existing technical literature
Patent document
Patent document 1: Japanese Unexamined Patent Application 63-125649 bulletin
Summary of the invention
Problems to be solved by the invention
In the case where the Ni base superalloy for making precipitation strength type squeezes out material, firstly, if γ ' phase transformation in blank
More, then the deformation drag of blank is got higher, so that the extrusion molding (hot-workability) of blank can significantly reduce.Moreover, the blank
When for the Ni base superalloy with precipitation strength type at " ingot casting " being grouped as, segregation when casting solidification, which is inclined to, to be become
By force, many brittlement phases can thus be generated in blank, when extrusion cracks since the crystal boundary of the cast sturcture, and blank squeezes
Mouldability further decreases out.
The object of the present invention is to provide with the ingredient of the Ni base superalloy with the precipitation strength type more than γ ' phase
The ingot casting of composition is that the Ni base superalloy of blank squeezes out the manufacturing method of material and Ni base superalloy squeezes out material.
The solution to the problem
The present invention is the manufacturing method that a kind of Ni base superalloy squeezes out material, includes the 1st process, and Ni base is super resistance to
The blank heating of thermalloy is to hot processing temperature;With the 2nd process, the blank that will warm up above-mentioned hot processing temperature is inserted into Sheng ingot
Cylinder applies compressing force to blank from the one end of the ingot-containing tube, from the hole of the mold of the another side for being set to ingot-containing tube by base
Material squeezes out, and obtains the extrusion material of Ni base superalloy,
The blank of above-mentioned Ni base superalloy is ingot casting obtained from casting melt, and the melt has at 700 DEG C
γ ' phase Equilibrium Precipitation amount be 40 moles of % or more precipitation strength type Ni base superalloy at being grouped as,
Above-mentioned hot processing temperature is set as to the γ ' Xiang Gu of 1030 DEG C of blanks more than or lower than above-mentioned Ni base superalloy
The temperature of solubility temperature, and extruded velocity when squeezing out above-mentioned blank is set as 10~300mm/s.
In addition, the present invention is that a kind of Ni base superalloy squeezes out material, the Equilibrium Precipitation with the γ ' phase at 700 DEG C
Amount is the Ni base superalloy of the precipitation strength type of 40 moles of % or more at being grouped as, and the average crystal grain in section structure is straight
Diameter is calculated as 20 μm or less with equivalent circle diameter.
The effect of invention
In accordance with the invention it is possible to make the Ni base superalloy with the precipitation strength type more than γ ' phase at being grouped as
Extrusion material.Moreover, being capable of providing the extrusion material of the Ni base superalloy with mentioned component composition.
Detailed description of the invention
Fig. 1 is that the section of " contraction flow region of blank " when showing the extrusion molding of example of the present invention, near die hole is macro
See the photo instead of attached drawing of an example of tissue.
Fig. 2 is the electron backscatter diffraction (EBSD) for showing the section microscopic structure of extrusion material of example production through the invention
The figure of an example of image.
Fig. 3 is the Ni base for showing the precipitation strength type for being 40 moles of % or more to the Equilibrium Precipitation amount of the γ ' phase at 700 DEG C
The figure of an example of the relationship of rate of straining and sectional shrinkage when superalloy implementation high temperature tension test.
Specific embodiment
The manufacturing method that Ni base superalloy of the invention squeezes out material is to utilize the side of following so-called " directly extruding "
Method: compressing force is applied to blank from the one end of the ingot-containing tube inserted with blank, from the mould for the another side for being set to ingot-containing tube
The hole of tool squeezes out blank.Moreover, in the present invention, there is precipitation strength type more than γ ' phase in order to directly extrude production by this
Ni base superalloy at the extrusion material being grouped as, there is feature below.
(1) the above-mentioned blank that Ni base superalloy of the invention squeezes out the manufacturing method of material will have at 700 DEG C
The Equilibrium Precipitation amount of γ ' phase is the Ni base superalloy of the precipitation strength type of " 40 moles of % or more " into the melt being grouped as
" ingot casting " obtained from casting.It should be noted that ingot casting, will the ingot casting squeeze out obtained from extrusion material also have at 700 DEG C
γ ' phase Equilibrium Precipitation amount be " 40 moles of % or more " precipitation strength type Ni base superalloy at being grouped as.
For the Ni base superalloy of precipitation strength type, tissue is mainly solid-solution in made of Ni matrix as alloying component
γ phase with as by Ni3(TiAl) etc. the γ ' of the precipitation strength phase of the intermetallic compound typically indicated is mutually constituted.In this way
The hot-working of Ni base superalloy usually play this in the solid solubility temperature (γ ' phase solid solubility temperature) being mutually dissolved from above-mentioned γ '
The temperature region (such as 900 DEG C~1200 DEG C) in the section until the solidus temperature of Ni base superalloy carries out.The heat adds
In working hour, if above-mentioned γ ' phase is more, deformation drag is got higher, so that the hot-workability of Ni base superalloy reduces.
At this point, the amount of above-mentioned γ ' phase changes according to the temperature of heating Ni base superalloy.Moreover, with temperature
Start temperature (γ ' phase solid solubility temperature) reduction is mutually precipitated from γ ' for degree, and the Equilibrium Precipitation amount of γ ' phase is (steady in thermodynamic equilibrium state
The amount of precipitation of fixed γ ' phase) increase since minimum value, usually becoming smaller in substantially 700 DEG C of following temperature dependences (is substantially permanent
Definite value).Therefore, the Equilibrium Precipitation amount of the γ ' phase of Ni base superalloy can be by the basis of value when above-mentioned " 700 DEG C "
Come hold its whole γ ' phase amount of precipitation tendency.
Moreover, in the extrusion molding of Ni base superalloy, blank more than the above-mentioned γ ' phase specifically has 700
The Equilibrium Precipitation amount of γ ' phase at DEG C is the Ni base superalloy of the precipitation strength type of 40 moles of % or more at being grouped as
In the case where blank, be mutually not easy to disappear in above-mentioned temperature region γ ', more than γ ' phase solid solubility temperature at a temperature of be extruded into
Type is difficult.The present invention carries out extrusion molding to this blank for being difficult to carry out hot worked Ni base superalloy.
In the blank of the wanted extrusion molding of the present invention, the Equilibrium Precipitation amount of the γ ' phase at above-mentioned 700 DEG C is preferably 50 to rub
You are % or more.Moreover, more preferably 60 moles of % or more.It should be noted that not needing the upper limit that the value is especially arranged.But
It is that 75 moles of % or so are real.
Moreover, in the Ni base superalloy of precipitation strength type of the invention, by " mole % " above-mentioned γ ' phase indicated
The value of Equilibrium Precipitation amount is that can be had by the Ni base superalloy at being grouped as the value determined.The Equilibrium Precipitation amount
The value of " mole % " can be by being found out based on the parsing of calculation of thermodynamic equilibrium.Moreover, based on calculation of thermodynamic equilibrium
In the case where parsing, by using various thermodynamic balance calculation softwares, can precision it is good and easily find out.
Equilibrium Precipitation amount as the γ ' phase at above-mentioned 700 DEG C is the Ni base of the precipitation strength type of " 40 moles of % or more "
Superalloy, for example, can enumerate in terms of quality % C:0.001~0.25%, Cr:8.0~22.0%, Mo:2.0~
7.0%, Al:2.0~8.0%, Ti:0.4~7.0%, surplus are the basic at being grouped as (hereinafter, for " matter of Ni and impurity
The such statement of % " is measured, " % " is abbreviated as).In addition, it is above-mentioned it is basic at being grouped as in, as needed can also be containing being selected from
Co:28.0% or less, W:6.0% or less, Nb:4.0% or less, Ta:3.0% or less, Fe:10.0% or less, V:1.2% with
Under, the one kind or two or more element material in Hf:1.0% or less, B:0.300% or less, Zr:0.30% or less.As this
The Ni base superalloy of sample, such as (UDIMET is Special Metals Corporation by Alloy713C, UDIMET720
Registered trademark), IN100 be representative.
For the mentioned component composition of illustration, the effect of each element is illustrated.
<C:0.001~0.25%>
C has the effect of the castability for improving Ni base superalloy, the intensity for improving crystal boundary.But if C becomes more,
It can be precipitated in the form of coarse eutectic carbide in the final solidification portion of casting ingot casting.Eutectic carbide quantity with C
The increase of amount and while increase, carbide is also thicker big.When coarse carbide increases, the crackle of plastic processing can be become
Starting point, the deteriorated ductility of plastic processing.Therefore, the content of C is preferably set to 0.001~0.25%.More preferably it is set as 0.10%
Below, further preferably it is set as 0.05% or less.Particularly preferably it is set as 0.02% or less.In addition, be more preferably set as 0.003% with
It is upper, further preferred to be set as 0.005% or more.Particularly preferably it is set as 0.008% or more.
<Cr:8.0~22.0%>
Cr is the element for improving oxidative resistance, corrosion resistance.But if excessive contain Cr, it will form the equal embrittlement of σ
Phase reduces intensity, hot-workability.Therefore, the content of Cr is preferably set to 8.0~22.0%.More preferably 9.0% or more, into
One step is preferably 9.5% or more.Particularly preferably 10.0% or more.In addition, more preferably 18.0% or less, further preferably
16.0% or less.Particularly preferably 14.0% or less.
<Mo:2.0~7.0%>
Mo has the effect of facilitating the solution strengthening of matrix, improves elevated temperature strength.But it if Mo is excessive, will form
Intermetallic compound phase is to damage elevated temperature strength.Therefore, the content of Mo is preferably set to 2.0~7.0%.More preferably 2.5%
It above, is more preferably 3.0% or more.Particularly preferably 3.5% or more.In addition, more preferably 6.0% or less, further
Preferably 5.5% or less.Particularly preferably 5.0% or less.
<Al:2.0~8.0%>
Al is to form γ ' mutually thus the element for improving elevated temperature strength.But excessively containing for Al can be such that hot-workability drops
The reason of low, as faults in material such as the crackles squeezed out in processing.Therefore, the content of Al is preferably set to 2.0~8.0%.It is more excellent
It is selected as 2.5% or more, further preferably 3.5% or more.Particularly preferably 4.5% or more.In addition, more preferably 7.5% with
Under, further preferably 7.0% or less.Particularly preferably 6.5% or less.
<Ti:0.4~7.0%>
Ti and Al is similarly the element to form γ ' phase, the solution strengthening of γ ' phase is improved to elevated temperature strength.But if
Excessively contain Ti, then will form harmful η (eta) mutually to damage hot-workability.Therefore, the content of Ti be preferably set to 0.4~
7.0%.It more preferably 0.45% or more, is more preferably 0.5% or more.In addition, more preferably 5.0% or less, further
Preferably 3.0% or less.Particularly preferably 1.0% or less.
<Co:28.0% or less>
Co is the stability for improving tissue, and the choosing of hot-workability can be maintained containing a large amount of Ti as intensified element
One of selecting property element.On the other hand, due to Co valuableness, cost increase.Therefore, even if Co's contains containing in the case where Co
Amount is it is also preferred that be set as 28.0% or less.It more preferably 18.0% or less, is more preferably 16.0% or less.Particularly preferably
13.0% or less.Moreover, in the case where Co can be set as to no added grade (the inevitable impurity levels of raw material), it will
The lower limit of Co is set as 0%.Furthermore, it is possible to be set as Co less than 1.0%.
It should be noted that obtaining by containing in the case where Co bring said effect, the content of Co is preferably set to 1.0%
More than.It more preferably 3.0% or more, is more preferably 8.0% or more.Particularly preferably 10.0% or more.
<W:6.0% or less>
W is to facilitate one of selective element of solution strengthening of matrix in the same manner as Mo.On the other hand, if W is excessive
It will form harmful intermetallic compound phase, so that elevated temperature strength deteriorates.Therefore, even if containing in the case where W, the content of W
It is preferably set to 6.0% or less.It more preferably 5.5% or less, is more preferably 5.0% or less.Particularly preferably 4.5% with
Under.Moreover, the lower limit of W is set in the case where W can be set as to no added grade (the inevitable impurity levels of raw material)
It is 0%.Furthermore, it is possible to be set as W less than 1.0%, and then can be set to less than 0.8%.
It should be noted that obtain W by containing in the case where bring said effect, the content of W be preferably set to 1.0% with
On.Moreover, by compound containing W and Mo, thus effective to the performance of above-mentioned solution strengthening.With Mo compound containing containing W sometimes
Amount is preferably set to 0.8% or more.
<Nb:4.0% or less>
Nb is the selective element to form γ ' phase, the solution strengthening of γ ' phase is improved to elevated temperature strength in the same manner as Al, Ti
One of.But excessively containing for Nb will form harmful δ (delta) phase, deteriorate hot-workability.Therefore, even if containing Nb's
In the case of, the content of Nb is it is also preferred that be set as 4.0% or less.It more preferably 3.5% or less, is more preferably 3.0% or less.It is special
It You Xuanwei 2.5% or less.Moreover, in the feelings that Nb can be set as to no added grade (the inevitable impurity levels of raw material)
Under condition, the lower limit of Nb is set as 0%.Furthermore, it is possible to be set as Nb less than 0.5%.
It should be noted that obtaining by containing in the case where Nb bring said effect, the content of Nb is preferably set to 0.5%
More than.It more preferably 1.0% or more, is more preferably 1.5% or more.Particularly preferably 2.0% or more.
<Ta:3.0% or less>
Ta is the selective element to form γ ' phase, the solution strengthening of γ ' phase is improved to elevated temperature strength in the same manner as Al, Ti
One of.But the excessive addition of Ta makes γ ' mutually become the unstable coarsening so as to cause under high temperature, and shape at high temperature
At harmful η (eta) phase, deteriorate hot-workability.Therefore, even if the content of Ta is it is also preferred that be set as containing in the case where Ta
3.0% or less.It more preferably 2.5% or less, is more preferably 2.0% or less.Particularly preferably 1.5% or less.Moreover,
In the case that Ta can be set as to no added grade (the inevitable impurity levels of raw material), the lower limit of Ta is set as 0%.And
And Ta can be set as less than 0.3%.
It should be noted that obtaining by containing in the case where Ta bring said effect, the content of Ta is preferably set to 0.3%
More than.It more preferably 0.5% or more, is more preferably 0.7% or more.Particularly preferably 1.0% or more.
<Fe:10.0% or less>
Fe is that can replace expensive Ni, Co and contain, to one of reduction effective as selective element of cost of alloy.
But if excessively containing Fe, the equal brittle phase of σ will form to make intensity, hot-workability reduce.Therefore, even if containing
In the case where Fe, the content of Fe is it is also preferred that be set as 10.0% or less.More preferably 8.0% or less, be more preferably 6.0% with
Under.Particularly preferably 3.0% or less.Moreover, Fe can be set as to no added grade (inevitable impurity of raw material etc.
Grade) in the case where, the lower limit of Fe is set as 0%.Furthermore, it is possible to be set as Fe less than 0.1%.
It should be noted that in the case where obtaining by containing Fe bring said effect, instead of the Fe of the content of Ni, Co
Content be for example preferably set to 0.1% or more.It more preferably 0.4% or more, is more preferably 0.6% or more.Particularly preferably
It is 0.8% or more.
<V:1.2% or less>
V is useful one of the selective element of solution strengthening, the brought intercrystalline strengthening of carbide generation to matrix.But
It is that the excessive addition of V will lead to the generation of the unstable phase of high temperature in manufacturing process, is brought to manufacturing and mechanical behavior under high temperature
Adverse effect.Therefore, even if the content of V is it is also preferred that be set as 1.2% or less containing in the case where V.More preferably 1.0% or less,
Further preferably 0.8% or less.Particularly preferably 0.7% or less.Moreover, V can be set as no added grade (raw material
Inevitable impurity levels) in the case where, the lower limit of V is set as 0%.Furthermore, it is possible to be set as V less than 0.1%.
It should be noted that obtain by containing in the case where V bring said effect, the content of V be preferably set to 0.1% with
On.It more preferably 0.2% or more, is more preferably 0.3% or more.Particularly preferably 0.5% or more.
<Hf:1.0% or less>
Hf be the oxidative resistance of alloy is improved, selective element that intercrystalline strengthening brought by carbide generates is useful it
One.But the oxide that the excessive addition of Hf will lead to manufacturing process generates, the generation of the unstable phase of high temperature, to manufacturing and
Mechanical behavior under high temperature brings adverse effect.Therefore, even if the content of Hf is it is also preferred that be set as 1.0% or less containing in the case where Hf.
It more preferably 0.7% or less, is more preferably 0.5% or less.Particularly preferably 0.3% or less.Moreover, that Hf can be set
In the case where for no added grade (the inevitable impurity levels of raw material), the lower limit of Hf is set as 0%.Furthermore, it is possible to will
Hf is set as less than 0.02%.
It should be noted that obtaining by containing in the case where Hf bring said effect, the content of Hf is preferably set to
0.02% or more.It more preferably 0.05% or more, is more preferably 0.1% or more.Especially excellent is to select 0.15% or more.
<B:0.300% or less>
B is that one of can be improved grain-boundary strength, improve creep strength, the selective element of ductility.On the other hand, the mistake of B
The addition of degree can be such that the fusing point of alloy is greatly reduced, in addition, the formation of coarse boride will lead to processability deterioration.Therefore,
Even if the content of B is preferably also 0.300% or less in the case where containing B.More preferably 0.100% or less, further preferably
It is 0.050% or less.Particularly preferably 0.020% or less.Moreover, B can be set as to no added grade, (raw material can not be kept away
The impurity levels exempted from) in the case where, the lower limit of B is set as 0%.Furthermore, it is possible to be set as B less than 0.001%.
It should be noted that obtaining by containing in the case where B bring said effect, the content of B is preferably set to 0.001%
More than.It more preferably 0.003% or more, is more preferably 0.005% or more.Particularly preferably 0.007% or more.
<Zr:0.30% or less>
Zr is one of the selective element improve with grain-boundary strength in the same manner as B.But if excessively contain
Zr then will lead to the reduction of the fusing point of alloy, so that elevated temperature strength, hot-workability deteriorate.Therefore, even if the case where containing Zr
Under, the content of Zr is it is also preferred that be set as 0.30% or less.It more preferably 0.25% or less, is more preferably 0.20% or less.It is special
It You Xuanwei 0.15% or less.Moreover, Zr can be set as to no added grade (the inevitable impurity levels of raw material)
In the case of, the lower limit of Zr is set as 0%.Furthermore, it is possible to be set as Zr less than 0.001%.
It should be noted that obtaining by containing in the case where Zr bring said effect, the content of Zr is preferably set to
0.001% or more.It more preferably 0.005% or more, is more preferably 0.01% or more.Particularly preferably 0.03% or more.
Moreover, the blank of extrusion molding is to be by the Equilibrium Precipitation amount for the γ ' phase having at above-mentioned 700 DEG C in the present invention
The Ni base superalloy of the precipitation strength type of " 40 moles of % or more " at be grouped as melt casting obtained from " ingot casting ".
That is, with mentioned component composition ingot casting have the tendency that being segregated in its casting solidification it is strong, can in cast sturcture after solidification
Form a large amount of brittlement phases.In the past, it when this ingot casting for foring a large amount of brittlement phases being carried out extrusion molding to it as blank, squeezes
Intercrystalline fracture of the blank in molding from its cast sturcture out, it is difficult to obtain the extrusion material for the recrystallized structure for having fine.This
The manufacturing method that the Ni base superalloy of invention squeezes out material can be with this Ni base superalloy for being difficult to extrusion molding
Ingot casting is blank, realizes the extrusion molding of the blank.
(2) Ni base superalloy of the invention squeezes out in the manufacturing method of material, will become the heat of the blank of above-mentioned ingot casting
Processing temperature is set as the temperature of " γ ' the phase solid solubility temperature " of the blank of " 1030 DEG C or more " and " being lower than " above-mentioned Ni base superalloy
Degree.
The precipitation that the Equilibrium Precipitation amount of γ ' phase in the case where the blank of extrusion molding has 700 DEG C is 40 moles of % or more
The Ni base superalloy of enhanced type at being grouped as and in the case where by casting obtained ingot casting, in the past, the blank
Extrusion molding be difficult.But the inventors discovered that, the extrusion molding of above-mentioned blank is not the only change by blank
This simple property that the size of form drag can " directly " be evaluated.
That is, in the extrusion molding of blank, if its hot processing temperature is reduced from γ ' phase solid solubility temperature, base at the same time
The amount of precipitation of γ ' phase in material is also significantly increased.As a result, will not sufficiently be generated if the deformation drag of blank dramatically increases
Fever is processed by the deformation bring of blank, especially near the die hole that blank is shunk (contraction flow region of blank), meeting exists
" temperature is uneven " is generated in blank, the deformation drag with blank itself interacts greatly, will increase the plastic deformation of blank
Inhomogeneity.Then, it is as a result difficult to obtain the extrusion material with fine recrystallized structure.
Result, it is believed that in the present case, for improving the extrusion molding of above-mentioned blank, not only from subtracting
The angle of the opinion of its small deformation drag is studied and processes such opinion of generating heat caused by the deformation from utilizing
It is effective that angle, which also carries out research,.Moreover, for the deformation drag for the blank that can sufficiently obtain processing fever, it can be because
Above-mentioned hot processing temperature and very sensitively react, therefore the management of the hot processing temperature is important.Moreover, of the invention
In the case where, by the way that above-mentioned hot processing temperature to be set as to " 1030 DEG C or more ", above-mentioned processing fever can be effectively utilized, even if
There are γ in blank ' phase under conditions of (that is, lower than γ ' phase solid solubility temperature hot processing temperature under), also can be improved blank
Synthesis extrusion molding.About above-mentioned hot processing temperature, preferably 1050 DEG C or more.More preferably 1080 DEG C or more.Into one
Preferably 1100 DEG C or more of step.Particularly preferably 1130 DEG C or more.
On the other hand, if above-mentioned hot processing temperature rises towards γ ' phase solid solubility temperature, the precipitation of the γ ' phase in blank
Amount reduces (solid solution), so that the deformation drag of blank becomes smaller.Then, which can play the extrusion molding for improving blank
Effect.
But if above-mentioned hot processing temperature rises to γ ' phase solid solubility temperature, the growth for weighing crystal grain is significant, becomes coarse
Recrystallized structure, squeeze out material become brittleness.Moreover, it is important that if above-mentioned hot processing temperature is more than γ ' phase solid solubility temperature,
Then the Equilibrium Precipitation amount of the γ ' phase at 700 DEG C is 40 moles of % or more into the Ni base superalloy being grouped as
In the case of, from above-mentioned γ ' phase solid solubility temperature, into the very narrow temperature region solidus temperature, blank can become
The state of " zero ductility ", extrusion molding become difficult.Therefore, in the present invention, by the way that above-mentioned hot processing temperature is set as " being lower than "
The temperature of " γ ' the phase solid solubility temperature " of the blank of above-mentioned Ni base superalloy, to utilize institute's band in above-mentioned processing fever
On the basis of the extrusion molding of the blank come improves, the tissue for squeezing out material can be made to become fine recrystallized structure.For
Above-mentioned hot processing temperature, preferably 1180 DEG C or less.More preferably 1170 DEG C or less.Further preferably 1150 DEG C or less.
It should be noted that in the blank of the Ni base superalloy of precipitation strength type according to the present invention, it is above-mentioned
γ ' phase solid solubility temperature is that can be had by the Ni base superalloy at being grouped as the value determined.At this point, above-mentioned γ ' Xiang Gu
Solubility temperature can be by being found out based on the parsing of calculation of thermodynamic equilibrium.Moreover, being solved based on calculation of thermodynamic equilibrium
In the case where analysis, by using various thermodynamic balance calculation softwares, can precision it is good and easily find out.
(3) manufacturing method that Ni base superalloy of the invention squeezes out material will squeeze the blank for becoming above-mentioned ingot casting
Extruded velocity when out is set as " 10~300mm/s ".
The blank of extrusion molding has the precipitation that the Equilibrium Precipitation amount of the γ ' phase at 700 DEG C is 40 moles of % or more strong
The Ni base superalloy of change type at being grouped as, moreover, for the ingot casting as obtained from casting, in order to improve
The extrusion molding of such blank, it is also important for adjusting " extruded velocity " when its extrusion molding.
Fig. 3 be using Alloy713C (the Equilibrium Precipitation amount of the γ ' phase at 700 DEG C: 69 moles of %, γ ' phase solid solubility temperature:
1185 DEG C) when, the stretch test result at its 1150 DEG C.In the temperature region lower than γ ' phase solid solubility temperature, " receive in section
The value of shrinkage " increases as " rate of straining " increases, it is known that it is super resistance to the Ni base for improving precipitation strength type to improve process velocity
The mouldability of thermalloy is effective.Furthermore, it is believed that effective phenomenon is also the same in extrusion molding, that is, precipitation strength type
Ni base superalloy " ductility " lower than its γ ' phase solid solubility temperature temperature region in can because increase " extruded velocity "
And it improves.Then, in the present case, which is set as the quick value of " 10mm/s or more ".It should be noted that
The movement speed of " bar " when the extruded velocity can be set to the extrusion billet in extrusion molding.If extruded velocity is less than 10mm/
S then has the ductility of blank at this time to reduce to squeeze out the worry that material cracks.For above-mentioned extruded velocity, preferably
12mm/s or more.More preferably 14mm/s or more.
To increasing, the mechanism speculate that extruded velocity improves the ductility of blank is as follows.I.e., it is believed that Ni base superalloy
In γ ' meet the dynamic recrystallization hindered in its hot-working, so that Ni base superalloy be hindered successfully to deform.Therefore,
The Equilibrium Precipitation amount of γ ' phase at 700 DEG C is that the Ni base superalloy of 40 moles of % or more needs importing to make in hot-working
It can be realized the degree that the dynamic recrystallization smoothly deformed generates, higher " strain energy ".And think, in hot-working,
By improving above-mentioned " rate of straining (extruded velocity) ", the above-mentioned strain energy being fed in Ni base superalloy is become difficult to
Release, so that enough dynamic recrystallizations are generated, so that Ni base superalloy is smoothly deformed into possibility.
On the other hand, in the present case, above-mentioned extruded velocity is set as " 300mm/s or less ".It is squeezed out by increasing
Speed is conducive to the ductility for improving blank.But extruded velocity is when reaching certain numerical value, the degree meeting that blank ductility improves
Slow down, effect saturation.In addition, if considering the ability of extrusion device, the upper limit of above-mentioned extruded velocity (movement speed of bar)
It is real for 300mm/s or so.For above-mentioned extruded velocity, preferably 280mm/s or less.More preferably 260mm/s or less.
Even in addition, the extruded velocity is that can also obtain effect of the invention in 100mm/s or less, 90mm/s situation below.
(4) preferably, in the manufacturing method that Ni base superalloy of the invention squeezes out material, above-mentioned blank is to casting
Blank made of ingot is heat-treated.
In the present case, even if the ingot casting that " will keep the state after just casting to melt " is as blank,
By above-mentioned method, it is also able to achieve the extrusion molding of the blank.Moreover, by after just being cast to melt to the holding
State ingot casting be heat-treated after, be made into blank, the segregation in blank can be mitigated, extrusion molding can be made more
Excellent blank.The temperature range of above-mentioned heat treatment is preferably set to the model near γ ' the phase solid solubility temperature of Ni base superalloy
It encloses.Moreover, being preferably set to the temperature range of " 1170~1250 DEG C " as concrete example.More preferably it is set as 1240 DEG C or less.Into one
Step is preferably set to 1230 DEG C or less.
If above-mentioned heat treatment temperature is too low, the mitigation effect being segregated becomes smaller.In addition, the case where carrying out above-mentioned heat treatment
Under, if its heat treatment temperature is got higher, such as substantially be more than above-mentioned γ ' phase solid solubility temperature, then casting when formed γ phase it is thick
Big crystal grain can further growth.Moreover, the embrittlement of grain boundaries in blank can be promoted.Speculate generate the embrittlement of grain boundaries the reason of be because
For microelement crystal boundary segregation.
It should be noted that heat treatment time can be according to the common homogeneous heat treatment (soaking carried out to various ingot bars
Process it) sets.For example, can be set to 3~30 hours heat treatment times.It can be preferably set to 10 hours or more heat
Handle the time.
When for the present invention, by being set as above-mentioned hot processing temperature and extruded velocity, even if to keep just casting melt
State supply after making has the Ni base for the precipitation strength type that the Equilibrium Precipitation amount of the γ ' phase at 700 DEG C is 40 moles of % or more
Superalloy at the blank being grouped as, be also able to carry out extrusion molding.Moreover, for above-mentioned blank, in section structure
Even if average crystal grain diameter be 6.3mm or more in terms of equivalent circle diameter and then reach the coarse diameter (reality of 7mm or more
Middle 30mm or so is the upper limit), also it is able to carry out extrusion molding.
Moreover, for example, fine recrystallized structure can be made in the extrusion material made by above-mentioned extrusion molding.Such as
The average crystal grain diameter that can be made in the section structure for squeezing out material is calculated as 20 μm with equivalent circle diameter and below fine ties again
Crystalline substance tissue (2 μm or so are lower limit in reality).In turn, can be made with equivalent circle diameter be calculated as 15 μm or less, 10 μm it is below
Fine recrystallized structure.Furthermore it is possible to which the average crystal grain diameter in the section structure for squeezing out material is fine to such as blank
Horizontal and then 1/1000th levels below below of 1/400th of average crystal grain diameter in section structure.
Section structure for measuring above-mentioned average crystal grain diameter can be in blank and extrusion material the two from along extrusion
The position of the central axis in the section (that is, section of the central axis comprising blank or the length direction for squeezing out material) when direction is cut in half
It sets and takes.It is then possible to according to the equivalent circle diameter of each crystal grain confirmed in the section taken from the position of the central axis
Find out above-mentioned average crystal grain diameter.
Extrusion ratio (sectional area of blank/extrusion material sectional area) when extrusion molding can be set to be extruded into common
The extrusion ratio applied in type.For example, extrusion ratio can be set as 2~40.Moreover, the extrusion ratio can be 30 hereinafter, can also be with
It is 20 or less.The extrusion material obtained in this way is for example with the form of wire rod.In addition, for the wire rod, such as the diameter in section is
1.4~20mm.Moreover, further hot-working, cold working are carried out to it by using such extrusion material as starting material,
It is 1~3mm metal wire thin in this way so as to make the diameter in such as section.
Embodiment
It is cast with defined at the melt being grouped as to what is prepared by vacuum melting, makes diameter 110mm
The ingot casting of × length 120mm.Then, which is put into heat-treatment furnace, implemented in air atmosphere 1200 DEG C × 20 hours
After heat treatment, it is cold to carry out furnace.Then, the ingot casting machinery after the heat treatment is processed into diameter 82mm × length 105mm ruler
The blank of extrusion is made in very little shape.It should be noted that also having been made by method same as described above for measuring section
The blank of average crystal grain diameter in tissue.Then, with chlorination iron liquid to the position of the central axis of the length direction of the blank
Section is corroded, with the section after its corrosion of 10 times of multiplying power of optical microphotograph sem observations.Then, to the 50mm of the observation ×
The crystal grain confirmed in the visual field area of 40mm has carried out image analysis, and as a result the average crystal grain diameter in its section structure is with circle
Equivalent diameter is calculated as 10mm or so.
Above-mentioned melt is shown in table 1 at (that is, blank at be grouped as) is grouped as.It should be noted that Co, W, Ta,
V, Hf is impurity element, therefore meets Co≤28.0%, W≤6.0%, Ta≤3.0%, V≤1.2%, Hf≤1.0%.In addition,
For these melts at being grouped as, thermodynamic balance calculation software " JMatPro (Version8.0.1, Sente are used
Software Ltd. corporation) " find out the Equilibrium Precipitation amount and γ ' phase solid solubility temperature of γ ' phase at 700 DEG C.It will be listed by table 1
The content of each element of act is input in the thermodynamic balance calculation software and is calculated, as a result in table 1 at being grouped as
In range, the Equilibrium Precipitation amount of the γ ' phase at 700 DEG C is 66~67 moles of %, and γ ' phase solid solubility temperature is 1185~1188 DEG C.
[table 1]
※ includes impurity (Co≤28.0%, W≤6.0%, Ta≤3.0%, V≤1.2%, Hf≤1.0%)
Above-mentioned blank is put into heating furnace, defined hot processing temperature (the 1st process) is heated to.It then, will be above-mentioned
Blank after being kept for 2 hours under hot processing temperature takes out from heating furnace, is encased in the ingot-containing tube of extrusion device, implements to be based on
Defined extruded velocity (movement speed of bar) directly extrudes (the 2nd process).At this point, by blank from heating furnace taking-up after 3
Start above-mentioned directly extrude within second.Then, the extrusion material of production is evaluated, confirm is in the outside or inside for squeezing out material
It is no not generate " crackle ".Result is shown in table 2 together with extrusion condition.
[table 2]
According to table 2, the precipitation strength type for being 40 moles of % or more to the Equilibrium Precipitation amount with the γ ' phase at 700 DEG C
Ni base superalloy carries out squeezing based on hot processing temperature and extruded velocity of the invention at the blank (ingot casting) being grouped as
Extrusion material No.1~4 obtained from forming out do not crack.Moreover, squeezing out material No.1~4 has fine recrystallized structure.
In contrast, extrusion material No.5 more than above-mentioned γ ' phase solid solubility temperature a height of for hot processing temperature, is being extruded into
Blank state loss of ductility when type and produce crackle.In addition, the extrusion material No.6 small for extruded velocity is also the same, squeezing
Out form when blank state loss of ductility and produce crackle.Moreover, the dynamic recrystallization for squeezing out material No.6 does not carry out sufficiently,
There is non-recrystallization tissue.
Fig. 1 show squeeze out material No.4 extrusion molding when blank contraction flow region section macrostructure.In Fig. 1, it is known that
The crystal grain diameter of the position of blank before deflation is the blank of the coarse cast sturcture 1 of substantially 10mm or so after shrinking
The change in location of (squeezing out material) is fine recrystallized structure 2.In addition, Fig. 2 shows the section microscopic structures for squeezing out material No.4
EBSD image.It should be noted that the determination condition of EBSD are as follows: scanning step: being set as 0.1 μm, the definition for crystal grain will
15 ° of misorientation or more are set as crystal boundary.In addition, the section microscopic structure is obtained from being cut in half along the length direction for squeezing out material
Microscopic structure at the position of central axis in section.Moreover, being counted according in the visual field area of Fig. 2 (200 150 μm of μ m)
Crystal grain, the extrusions material No.4 of example production is about 2.1 μm micro- with average grain diameter in terms of equivalent circle diameter through the invention
Thin recrystallized structure.Moreover, it is also the same in extrusion material No.1~3 of hot processing temperature when squeezing out than squeezing out material No.4 high,
By the measuring method of average crystal grain diameter same as described above, having the average crystal grain diameter in terms of equivalent circle diameter is 20 μm
Fine recrystallized structure below.
It should be noted that for squeezing out material No.1, the low value of the hot processing temperature " 1025 DEG C " when making its extrusion is removed
Other than this, implements the extrusion based on the same terms, make another extrusion material.As a result, in the case where another extrusion material, blank
Deformation drag dramatically increase, nor can obtain adequately process fever, the recrystallized structure for having fine cannot be obtained
Extrusion material.
Description of symbols
1 cast sturcture
2 recrystallized structures
Claims (2)
1. a kind of Ni base superalloy squeeze out the manufacturing method of material comprising:
1st process, by the blank heating of Ni base superalloy to hot processing temperature;With
2nd process, the blank that will warm up the hot processing temperature are inserted into ingot-containing tube, from the one end of the ingot-containing tube to institute
It states blank and applies compressing force, the blank is squeezed out from the hole of the mold for the another side for being set to the ingot-containing tube, obtains Ni
The extrusion material of base superalloy,
The blank of the Ni base superalloy is ingot casting obtained from casting melt, and the melt has the γ ' at 700 DEG C
The Equilibrium Precipitation amount of phase is the Ni base superalloy of the precipitation strength type of 40 moles of % or more at being grouped as,
The γ ' that the hot processing temperature is set as 1030 DEG C of blanks more than or lower than the Ni base superalloy is mutually dissolved temperature
The temperature of degree, and extruded velocity when squeezing out the blank is set as 10~300mm/s.
2. a kind of Ni base superalloy squeezes out material, which is characterized in that the Equilibrium Precipitation amount with the γ ' phase at 700 DEG C is 40
The Ni base superalloy of the precipitation strength type of mole % or more at being grouped as,
Average crystal grain diameter in section structure is calculated as 20 μm or less with equivalent circle diameter.
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PCT/JP2017/020143 WO2018061317A1 (en) | 2016-09-30 | 2017-05-30 | Method of manufacturing ni-based super heat resistant alloy extruded material, and ni-based super heat resistant alloy extruded material |
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US (1) | US20190232349A1 (en) |
EP (1) | EP3520915A4 (en) |
JP (1) | JP6660042B2 (en) |
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WO2020031579A1 (en) * | 2018-08-07 | 2020-02-13 | 日立金属株式会社 | Method for producing ni-based super-heat-resisting alloy, and ni-based super-heat-resisting alloy |
CN112813294B (en) * | 2020-12-30 | 2022-03-08 | 北京钢研高纳科技股份有限公司 | High-strength high-elasticity Ni-Cr-Co-W-based alloy wire and preparation method thereof |
JP2022160167A (en) * | 2021-04-06 | 2022-10-19 | 大同特殊鋼株式会社 | Heat resistant alloy member, material used therefor and method for manufacturing them |
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2017
- 2017-05-30 JP JP2018541895A patent/JP6660042B2/en not_active Expired - Fee Related
- 2017-05-30 WO PCT/JP2017/020143 patent/WO2018061317A1/en unknown
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US20190232349A1 (en) | 2019-08-01 |
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EP3520915A1 (en) | 2019-08-07 |
EP3520915A4 (en) | 2020-06-10 |
WO2018061317A1 (en) | 2018-04-05 |
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