CN102251131B - Method for preparing injection-molding nickel-base ODS (oxide dispersion strengthened) alloy - Google Patents
Method for preparing injection-molding nickel-base ODS (oxide dispersion strengthened) alloy Download PDFInfo
- Publication number
- CN102251131B CN102251131B CN2011101807442A CN201110180744A CN102251131B CN 102251131 B CN102251131 B CN 102251131B CN 2011101807442 A CN2011101807442 A CN 2011101807442A CN 201110180744 A CN201110180744 A CN 201110180744A CN 102251131 B CN102251131 B CN 102251131B
- Authority
- CN
- China
- Prior art keywords
- powder
- alloy
- injection
- nickel
- base
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 59
- 239000000956 alloy Substances 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000001746 injection moulding Methods 0.000 title claims abstract description 7
- 229910001175 oxide dispersion-strengthened alloy Inorganic materials 0.000 title abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 114
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000002245 particle Substances 0.000 claims abstract description 30
- 238000005238 degreasing Methods 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims abstract description 9
- 230000032683 aging Effects 0.000 claims abstract description 6
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract 3
- 238000002347 injection Methods 0.000 claims description 60
- 239000007924 injection Substances 0.000 claims description 60
- 238000003801 milling Methods 0.000 claims description 29
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 16
- 238000001513 hot isostatic pressing Methods 0.000 claims description 14
- 229920001903 high density polyethylene Polymers 0.000 claims description 12
- 239000004700 high-density polyethylene Substances 0.000 claims description 12
- 238000005551 mechanical alloying Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 9
- 238000005516 engineering process Methods 0.000 claims description 7
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 7
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000011159 matrix material Substances 0.000 claims description 6
- 239000012188 paraffin wax Substances 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 6
- 229910052735 hafnium Inorganic materials 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 4
- 229910000601 superalloy Inorganic materials 0.000 claims description 4
- 238000005275 alloying Methods 0.000 claims description 3
- 238000013461 design Methods 0.000 claims description 3
- 238000007669 thermal treatment Methods 0.000 claims description 3
- 239000000470 constituent Substances 0.000 claims description 2
- 230000007547 defect Effects 0.000 claims description 2
- 238000009689 gas atomisation Methods 0.000 claims description 2
- 229910001026 inconel Inorganic materials 0.000 claims description 2
- 229910000816 inconels 718 Inorganic materials 0.000 claims description 2
- 230000001788 irregular Effects 0.000 claims description 2
- 229910001235 nimonic Inorganic materials 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 238000009692 water atomization Methods 0.000 claims description 2
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 claims 1
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000009826 distribution Methods 0.000 claims 1
- 229910000856 hastalloy Inorganic materials 0.000 claims 1
- 239000004615 ingredient Substances 0.000 claims 1
- 238000004886 process control Methods 0.000 claims 1
- 239000006104 solid solution Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 7
- 230000007246 mechanism Effects 0.000 abstract description 4
- 238000005728 strengthening Methods 0.000 abstract description 3
- 238000010902 jet-milling Methods 0.000 abstract 3
- 238000003723 Smelting Methods 0.000 abstract 1
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 238000005056 compaction Methods 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- 238000007670 refining Methods 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- 239000011812 mixed powder Substances 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 238000009413 insulation Methods 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 229910052804 chromium Inorganic materials 0.000 description 4
- 239000000306 component Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000011863 silicon-based powder Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 238000002203 pretreatment Methods 0.000 description 3
- 101100400378 Mus musculus Marveld2 gene Proteins 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000005563 spheronization Methods 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical compound CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 description 1
- 240000007762 Ficus drupacea Species 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Images
Landscapes
- Powder Metallurgy (AREA)
Abstract
The invention provides a method for preparing a nickel-base ODS (oxide dispersion strengthened) alloy by injection molding, belonging to the technical field of injection molding of powder. The method comprises the following steps: carrying out high-energy ball milling on the raw material powder so that Y2O3 particles are uniformly dispersed in a nickel substrate, refining mechanical alloy powder by jet milling, and carrying out plasma nodularization on the powder which is refined by jet milling; evenly mixing and smelting the powder, which is refined by jet milling and plasma nodularization, and adhesive to obtain a uniform feed material; and carrying out injection molding, two-step degreasing and sintering on the feed material to obtain a sintered blank of which the density is 93-96%, carrying out hot isostatic compaction on the sintered blank so that the sintered blank is completely compact, and finally, carrying solution heat treatment and aging heat treatment to obtain the injection-molding nickel-base ODS alloy. The nickel-base ODS alloy can be prepared into high-precision parts in complex shapes, thereby solving the problem of difficulty in molding of nickel-base ODS alloy. The gamma' phase and the oxide strengthening mechanism are combined to greatly enhance the high-temperature mechanical properties of the nickel-base ODS alloy.
Description
Technical field
The invention belongs to the powder injection forming technical field, providing a kind of especially is feedstock production injection forming nickel-based oxide dispersion-strengthened (Oxide Dispersion Strengthening, ODS) method of alloy with pre-treatment machinery alloying powder.
Background technology
Ni-based ODS alloy still has excellent high temperature creep property, fatigue property and antioxidant property more than 1000 ℃.The middle temperature of nickel-base alloy (700~900 ℃) intensity is lower, through the interpolation formation L1 of elements such as Al, Ti and Nb
2γ ' [the Ni of structure
3(Al, Ti)] precipitated phase can effectively improve medium temperature intensity.Under higher temperature (>1000 ℃), γ ' phase is owing to dissolving loses strengthening effect, and this moment, the dispersion-strengthened mechanism of steady oxide accounted for leading.γ ' phase is a kind of important high-temperature structural material with the Ni-based ODS alloy that dispersed oxide is strengthened mutually altogether, and it can be used as some the crucial high-temperature components in gas turbine engine, aircraft engine and the automobile turbocharger.In gas turbine engine, in order to raise the efficiency, turbine front end inlet temperature increases to about 1500 ℃ by 600-700 ℃ of the initial stage, and this is to the demands for higher performance of high temperature components material (particularly blade material).In automobile-used field, turbocharging technology is to improve automobile engine power, cut down the consumption of energy and automotive industry realizes one of effective means of target for energy-saving and emission-reduction.Turbine is the core component in the automobile turbocharger.At present, turbocharging technology is just progressively popularized to petrol motor, and the exhaust temperature of petrol motor supercharging rear engine is up to 1050 ℃, and common nickel-base alloy can not satisfy request for utilization.
Ni-based ODS alloy is the potential equivalent material of turbine in blade and the automobile turbocharger in the advanced internal combustion turbine; But Ni-based ODS hardness of alloy is high, plasticity is low and formability is poor; Be difficult to prepare parts such as complex-shaped blade or turbine through traditional machine-tooled method, this has seriously restricted applying of Ni-based ODS alloy.Be devoted to the exploitation of Ni-based ODS superalloy and the research of advanced forming technique thereof in the world always.The powder injection forming technology is suitable for preparing high pressure blade and moderate, the complex-shaped part of turbine equidimension in the vehicle turbocharger in the internal combustion turbine; It has that near-net forming, homogeneous microstructure, performance are high, precision is high and series of advantages such as cost is low, can also effectively avoid nonmetal inclusion that cast Ni-base alloy exists, component segregation and defective such as loose.
Mechanical alloying is the requisite technology of preparation injection forming Ni-based ODS powdered alloy raw material, but the mechanical alloy powder is not suitable for carrying out injection forming owing to out-of-shape, powder agglomeration and particle diameter are thick.Therefore, must carry out pre-treatment, to make the powder that particle diameter and shape all are fit to injection forming to the mechanical alloy powder.Utilization can be carried out modification to the particle diameter and the shape of mechanical alloying powder to spray formula airflow milling and radio-frequency plasma spheronization techniques.Inject after utilizing superonic flow nozzzle that high pressure gas are quickened to spray formula airflow milling and pulverize the district, material particles is accelerated and reaches in the collision of nozzle intersection the purpose of pulverizing under the effect of the huge kinetic energy of high-speed gas.The radio-frequency plasma spheronization techniques is that powder particle in irregular shape is sprayed in the plasma furnace through feeding gun by carrying gas; Quilt heats rapidly and melts under radiation, convection current, conduction and four kinds of heat transfer mechanism effects of chemistry; Melt granules forms spherical droplets under surface tension effects; And under high thermograde, solidify rapidly, thereby obtain spherical powder.
It is thus clear that, after handling through airflow milling refinement and plasma body nodularization, the mechanical alloy powder can obtain to be fit to the fine particle spherical powder of injection molding process, and injection forming has successfully solved the difficult problem of Ni-based ODS alloy near-net forming.The development of the Ni-based ODS alloy of injection forming will promote applying of Ni-based ODS alloy greatly.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing the Ni-based ODS alloy of injection forming, be intended to solve the difficult problem of Ni-based ODS alloy near-net forming, have that microstructure is even, performance is high, precision is high, material use efficiency is high and low cost and other advantages.
The present invention at first adopts mechanical alloying prepared oxide dispersion intensifying Co-based alloy powder; Particle diameter is tiny uses powder stock with the spheric injection forming to obtain then the mechanical alloying powder to be carried out pre-treatment (airflow milling refinement and plasma body nodularization); Then pretreated mechanical alloying powder is carried out injection forming, hot isostatic pressing and thermal treatment; Obtain the Ni-based ODS alloy of injection forming at last, preparation technology is as shown in Figure 1, and concrete process step is:
1, mechanical alloying: with Co-based alloy powder, Y
2O
3Particle and the crude granule pre-mixing of Hf unit are even, in high-purity Ar atmosphere, pass through high-energy ball milling then with 0.8-1.5wt%Y
2O
3The Hf element uniform particles of particle and 0.8-3.0wt% is dispersed in the matrix.The rotating speed of ball mill is 380~500 rev/mins, and the ball milling time is 36-72 hour.The pattern of mechanical alloying powder is as shown in Figure 2;
The composition of described Co-based alloy powder is the nickel base superalloy of various standard brands, or according to the non-standard alloy of actual condition design.Nickel base superalloy is selected from: Nimonic 90 (USS), Inconel718 (USS), Inconel 713C (USS), HastelloyX (USS), GH4195 (GB) or GH4195 (GB); Raw material powder adds with the form of element powders, perhaps adopts the pre-alloyed powder of high pressure gas atomizing or water atomization prepared.
2, to spray formula airflow milling: the mechanical alloying powder is handled through spray formula airflow milling is carried out dispersion and fining.Control the particle diameter of powder through pilot-gas flow, WP, sorting ability frequency.Gaseous tension is 3~8MPa, and the separation wheel frequency is 40~60Hz, and the powder diameter after airflow milling is handled is 10-40 μ m.Fig. 3 is the powder morphology figure after spray formula airflow milling is handled.Visible by figure, the obvious refinement of powder after airflow milling is handled, reunion powder disappears;
3, plasma body nodularization: the powder after the airflow milling refinement is carried out plasma spheroidization handle,, make the powder sphericity high as far as possible through parameters such as control powder feeding rate and gas operational throughpuies.Powder feeding rate is 30~200gmin
-1, the plasma output rating is 50~90KW, negative pressure is 7000~12000Pa.Fig. 4 is the SEM shape appearance figure of plasma spheroidization powder, can find out that the nodularization effect of powder is remarkable;
4, mixing: it is that mixing 0.5-1.5h processes even feeding under 30-50 rev/min the condition in 145-170 ℃, rotating speed in duplicate rows star mixing roll that airflow milling refinement powder and plasma spheroidization powder and sticker mix the back, and wherein the powder tonburden is 55-65vol%.
Described sticker adopts cerul multicomponent polymeric system, and the ratio of each constituent element is: 50-70wt% paraffin, 10-20% high density polyethylene(HDPE), 10-20% Vestolen PP 7052 and surplus Triple Pressed Stearic Acid;
5, injection forming: on injection machine, carry out injection forming, obtain the desired shape part.Injection temperature is that 150-175 ℃, injection pressure are 75-125MPa;
6, degreasing: the injection base adopts solvent degreasing and two step of hot degreasing degreasing process, in organic solvents such as trieline or trichloroethane, soaks 5-12h in 45-60 ℃ earlier; In high-purity argon gas atmosphere, carry out hot degreasing then in 25-1100 ℃;
7, sintering: the degreasing base carries out sintering in vacuum atmosphere or high-purity argon gas protective atmosphere, and sintering temperature is 1270-1360 ℃, and soaking time is 1-3h;
8, hot isostatic pressing: sintered blank is carried out hot isostatic pressing in 1000-1200 ℃ TR, and pressure is 100-200MPa, and soaking time is 1-3h, obtains complete fine and close Ni-based ODS alloy;
9, thermal treatment: the goods behind the hot isostatic pressing carry out solution treatment at 1100-1250 ℃, and water-cooled behind the insulation 2-6h then at 650-850 ℃ of ageing treatment 8-24h, finally obtains the Ni-based ODS alloy of injection forming.
Advantage of the present invention is that the particle diameter of the mechanical alloying powder behind airflow milling refinement and the plasma spheroidization is little, sphericity is high, is fit to carry out injection forming.Hot isostatic pressing has further improved comprehensive mechanical performance; Thereby prepare high-performance, high precision, complex-shaped part; Successfully solved the difficult problem of the difficult processing that is shaped of Ni-based ODS alloy, avoided the cast Ni-base alloy problem in addition, the problem includes: problems such as nonmetal inclusion, component segregation and rarefaction defects.Precipitation hardened the combining with oxide dispersion intensifying mechanism of γ ' expanded the mechanical behavior under high temperature of Ni-based ODS alloy significantly.
Description of drawings
Fig. 1 is a process flow sheet of the present invention
Fig. 2 is mechanical alloying powder SEM figure
Fig. 3 is airflow milling refinement powder SEM figure
Fig. 4 is plasma spheroidization powder SEM figure
Fig. 5 (a) is γ ' phase SEM figure in the Ni-based ODS alloy of injection forming
With dispersed oxide TEM figure (b) mutually
Embodiment
Embodiment 1: with the airflow milling fine powder is that feedstock production does not have γ ' and strengthens the Ni-based ODS alloy of injection forming mutually
With the granularity is the Y of 20-30nm
2O
3Particle and high-purity N i powder, Cr powder, Co powder, Mo powder, W powder, Fe powder, Si powder, Hf powder and C powder are raw material, by following quality percentage composition preparation mixed powder: 21%Cr, 1.5%Co, 9%Mo, 0.5%W, 18%Fe, 0.8%Si, 0.09%C, 1%Y
2O
3, 1.2%Hf and surplus Ni.At first mixed powder is carried out high-energy ball milling in high-purity Ar atmosphere and make Y
2O
3Uniform particles is dispersed in the Ni matrix, and drum's speed of rotation is 380 rev/mins, and the ball milling time is 40 hours; The mechanical alloy powder adopts airflow milling to carry out broken thinning processing, and air pressure is 6MPa, and sorting can frequency be 45Hz, obtains the powder of the about 20 μ m of median size; Airflow milling particulate powders and sticker mix the back and on duplicate rows star mixing roll, make even feeding in 150 ℃ of mixing 1h; Wherein sticker is made up of 63% paraffin, 13% high density polyethylene(HDPE), 17% Vestolen PP 7052,7% Triple Pressed Stearic Acid, and the powder tonburden is 56vol.%; Feeding is injection forming on CJ80-E type injection machine, and injection temperature is 155 ℃, and injection pressure is 90MPa; The injection base behind the solution-off 10h, carries out hot degreasing in high-purity argon gas atmosphere in trieline solution, hot skimming temp is 900 ℃; The degreasing base in 1300 ℃ of sintering, is incubated 1h in vacuum atmosphere; Sintered blank is at 1100 ℃ of hot isostatic pressings, and pressure is 100MPa, insulation 2h.The density of the Ni-based ODS alloy of gained injection forming is 98.4%, and the oxide particle median size is 14.5nm.
Embodiment 2: with the plasma spheroidization powder is that feedstock production does not have γ ' and strengthens the Ni-based ODS alloy of injection forming mutually
With the granularity is the Y of 20-30nm
2O
3Particle and high-purity N i powder, Cr powder, Co powder, Mo powder, W powder, Fe powder, Si powder, Hf powder and C powder are raw material, by following quality percentage composition preparation mixed powder: 19%Cr, 2%Co, 8%Mo, 1%W, 19%Fe, 0.6%Si, 0.08%C, 1%Y
2O
3, 1.2%Hf and surplus Ni.At first mixed powder is carried out high-energy ball milling in high-purity Ar atmosphere and make Y
2O
3Uniform particles is dispersed in the Ni matrix, and drum's speed of rotation is 450 rev/mins, and the ball milling time is 48 hours; The mechanical alloy powder adopts airflow milling to carry out broken thinning processing, and air pressure is 8MPa, and sorting can frequency be 50Hz, obtains the powder of the about 30 μ m of median size; Powder after the airflow milling refinement is carried out the plasma body nodularization handle, powder feeding rate is 50gmin
-1, the plasma output rating is 70KW, negative pressure is 7000Pa in the chamber; Powder after the nodularization and sticker mix the back and on duplicate rows star mixing roll, make even feeding in 155 ℃ of mixing 1.5h; Wherein sticker is made up of 55% paraffin, 20% high density polyethylene(HDPE), 15% Vestolen PP 7052,10% Triple Pressed Stearic Acid, and the powder tonburden is 64vol.%; Feeding is injection forming on CJ80-E type injection machine, and injection temperature is 160 ℃, and injection pressure is 90MPa; The injection base behind the solution-off 12h, carries out hot degreasing in high-purity argon gas atmosphere in trieline solution, hot skimming temp is 1000 ℃; The degreasing base in 1320 ℃ of sintering, is incubated 2h in high-purity argon gas atmosphere; Sintered blank is at 1150 ℃ of hot isostatic pressings, and pressure is 150MPa, insulation 2h.The density of the Ni-based ODS alloy of gained injection forming is 99.1%, and the oxide particle median size is 11.1nm.
Embodiment 3: prepare γ ' with the airflow milling fine powder and be total to the Ni-based ODS alloy of intensified type injection forming with oxide compound
With the granularity is the Y of 20-30nm
2O
3Particle and high-purity N i powder, Cr powder, Nb powder, Mo powder, Ti powder, Al powder, Fe powder, Si powder, Hf powder and C powder are raw material, by following quality percentage composition preparation mixed powder: 18%Cr, 5%Nb, 3%Mo, 0.4%Al, 1%Ti, 19%Fe, 0.3%Si, 0.36%C, 1%Y
2O
3, 1.2%Hf and surplus Ni.At first mixed powder is carried out high-energy ball milling in high-purity Ar atmosphere and make Y
2O
3Uniform particles is dispersed in the Ni matrix, and drum's speed of rotation is 400 rev/mins, and the ball milling time is 60 hours; The mechanical alloy powder adopts airflow milling to carry out broken thinning processing, and air pressure is 5MPa, and sorting can frequency be 40Hz, obtains the powder of the about 35 μ m of median size; Airflow milling particulate powders and sticker mix the back and on duplicate rows star mixing roll, make even feeding in 160 ℃ of mixing 1.5h; Wherein sticker is made up of 60% paraffin, 15% high density polyethylene(HDPE), 15% Vestolen PP 7052,10% Triple Pressed Stearic Acid, and the powder tonburden is 57vol.%; Feeding is injection forming on CJ80-E type injection machine, and injection temperature is 160 ℃, and injection pressure is 90MPa; The injection base behind the solution-off 8h, carries out hot degreasing in high-purity argon gas atmosphere in trieline solution, hot skimming temp is 1100 ℃; The degreasing base in 1340 ℃ of sintering, is incubated 1h in vacuum atmosphere; Sintered blank is at 1100 ℃ of hot isostatic pressings, and pressure is 200MPa, insulation 2h; The hot isostatic pressing sample is at 1250 ℃ of solution treatment 2h, then at 700 ℃ of ageing treatment 12h.The density of the Ni-based ODS alloy of gained injection forming is 99.2%, and the volume(tric)fraction of γ ' phase is 45%, and particle diameter is 100nm, and the oxide particle median size is 12.8nm.
Embodiment 4: strengthen the Ni-based ODS alloy of injection forming with plasma spheroidization powdered preparation γ ' altogether with oxide compound
With the granularity is the Y of 20-30nm
2O
3Particle and high-purity N i powder, Cr powder, Nb powder, Mo powder, Ti powder, Al powder, Fe powder, Si powder, Hf powder and C powder are raw material, by following quality percentage composition preparation mixed powder: 16%Cr, 16%Co, 1.9%Ti, 0.85%Al, 2%Fe, 0.7%Si, 0.065%C, 1%Y
2O
3, 1.2%Hf and surplus Ni.At first mixed powder is carried out high-energy ball milling in high-purity Ar atmosphere and make Y
2O
3Uniform particles is dispersed in the Ni matrix, and drum's speed of rotation is 400 rev/mins, and the ball milling time is 48 hours; The mechanical alloy powder adopts airflow milling to carry out broken thinning processing, and air pressure is 7MPa, and sorting can frequency be 55Hz, obtains the powder of the about 19 μ m of median size; Powder after the airflow milling refinement is carried out the plasma body nodularization handle, powder feeding rate is 60gmin
-1, the plasma output rating is 80KW, negative pressure is 6000Pa in the chamber; Powder after the nodularization and sticker mix the back and on duplicate rows star mixing roll, make even feeding in 155 ℃ of mixing 2h; Wherein sticker is made up of 55% paraffin, 20% high density polyethylene(HDPE), 10% Vestolen PP 7052,15% Triple Pressed Stearic Acid, and the powder tonburden is 65vol.%; Feeding is injection forming on CJ80-E type injection machine, and injection temperature is 160 ℃, and injection pressure is 90MPa; The injection base behind the solution-off 10h, carries out hot degreasing in high-purity argon gas atmosphere in trieline solution, hot skimming temp is 1000 ℃; The degreasing base in 1290 ℃ of sintering, is incubated 2h in vacuum or high-purity argon gas atmosphere; Sintered blank is at 1200 ℃ of hot isostatic pressings, and pressure is 150MPa, insulation 2h; The hot isostatic pressing sample is at 1200 ℃ of solution treatment 3h, then at 750 ℃ of ageing treatment 10h.The density of the Ni-based ODS alloy of gained injection forming is 99.1%, and the volume(tric)fraction of γ ' phase is 45%, and particle diameter is 100nm, and the oxide particle median size is 8.8nm.
Claims (5)
1. method for preparing the Ni-based ODS alloy of injection forming is characterized in that:
A, design of alloy, the interpolation massfraction is 0.8~1.5% Y in the nickel-base alloy basic ingredient
2O
3As the dispersed oxide phase, add massfraction and be 0.8~3.0% Hf element as disperse phase refinement element, and with alloying constituent uniform mixing in proportion;
B, high-energy ball milling make Y through high-energy ball milling
2O
3Particle and Hf element uniform particles are dispersed in the Ni matrix, add 0.5~5wt% Triple Pressed Stearic Acid as process control agent, and drum's speed of rotation is 380~500 rev/mins, and the ball milling time is 36~72 hours;
C, airflow milling refinement are adopted spray formula airflow milling are carried out the mechanical alloying powder broken refinement and obtained the fine grain size powder, and gaseous tension is that 3~8MPa, separation wheel frequency are 40~60Hz;
D, plasma spheroidization, employing plasma spheroidization make the irregular powder after the airflow milling refinement change sphere into, and powder feeding rate is 30~200gmin
-1, the plasma output rating is 50~90kW, negative pressure is 7000~12000Pa;
E, mixing and injection forming; Airflow milling refinement powder and plasma spheroidization powder and sticker mix the back and on mixing roll, carry out the mixing even feeding that obtains in 145-170 ℃; Sticker is made up of 50-70wt% paraffin, 10-20% high density polyethylene(HDPE), 10-20% Vestolen PP 7052 and surplus Triple Pressed Stearic Acid, and the powder tonburden is 55-65vol%; Feeding is 145-165 ℃ in injection temperature, and injection pressure is that the condition injected of 70-90MPa is shaped, and obtains zero defect injection base;
The injection base that f, step e obtain adopts the technology of " the solution-off heating is taken off " to carry out degreasing, in trieline, soaks 8-12h earlier, carries out hot degreasing at 25-1100 ℃ then, time 8-12h;
The degreasing base that g, sintering, step f obtain is at 1270-1360 ℃ of sintering 1-3h, and the sintered blank density that obtains reaches 93-95%;
The sintered blank that h, hot isostatic pressing, step g obtain makes sintered blank fine and close entirely at 1000~1200 ℃, 100-200MPa hot isostatic pressing 1-3h;
I, thermal treatment, the goods behind the hot isostatic pressing adopt solid solution to optimize γ ' particle diameter and size distribution mutually with ageing treatment, at 1100-1250 ℃ of solution treatment 2-6h, at 650-850 ℃ of ageing treatment 8-24h, finally obtain the Ni-based ODS alloy of injection forming.
2. based on the said method for preparing the Ni-based ODS alloy of injection moulding of claim 1; It is characterized in that: the Co-based alloy powder that adopts in a step is the nickel base superalloy that is selected from the various standard brands of Nimonic 90, Inconel 718, Inconel 713C, Hastelloy X, GH4195 or GH4195, or based on the non-standard alloying component of actual condition design; Alloy powder adopts element powders to mix, and perhaps adopts high pressure gas atomizing or water atomization to carry out pre-alloyed.
3. according to the said method for preparing the Ni-based ODS alloy of injection forming of claim 1, it is characterized in that: add Y in a step
2O
3Particle diameter be 20-30nm.
4. according to the said method for preparing the Ni-based ODS alloy of injection forming of claim 1, it is characterized in that: the airflow milling in the high-energy ball milling of b step, c step is broken, adopt the argon gas of purity more than 99.999% as protective atmosphere in the sintering process of the hot degreasing of f step and g step.
5. according to the said method for preparing the Ni-based ODS alloy of injection forming of claim 1, it is characterized in that: the powder diameter after airflow milling is handled in the c step is 10-40 μ m.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN2011101807442A CN102251131B (en) | 2011-06-30 | 2011-06-30 | Method for preparing injection-molding nickel-base ODS (oxide dispersion strengthened) alloy |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN2011101807442A CN102251131B (en) | 2011-06-30 | 2011-06-30 | Method for preparing injection-molding nickel-base ODS (oxide dispersion strengthened) alloy |
Publications (2)
Publication Number | Publication Date |
---|---|
CN102251131A CN102251131A (en) | 2011-11-23 |
CN102251131B true CN102251131B (en) | 2012-11-28 |
Family
ID=44978696
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN2011101807442A Expired - Fee Related CN102251131B (en) | 2011-06-30 | 2011-06-30 | Method for preparing injection-molding nickel-base ODS (oxide dispersion strengthened) alloy |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN102251131B (en) |
Families Citing this family (25)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103060591B (en) * | 2013-01-08 | 2014-08-13 | 北京科技大学 | Method for near-net shaping of porous Ni-based ODS (oxide dispersion strengthening) alloy |
CN103008657A (en) * | 2013-01-13 | 2013-04-03 | 北京科技大学 | Method for preparing oxide dispersion strengthened alloy by rapid forming |
CN103122420B (en) * | 2013-02-28 | 2015-01-07 | 北京科技大学 | Method for preparing porous nickel-based ODS ( Oxide Dispersion Strengthened) alloy |
CN103121105B (en) * | 2013-03-19 | 2015-04-01 | 北京科技大学 | Method for preparing micro spherical niobium (Nb)-wolfram (W)-molybdenum (Mo)-zirconium (Zr) alloy powder |
CN103551573B (en) * | 2013-10-22 | 2015-06-17 | 中国科学院金属研究所 | Previous particle boundary precipitation preventable high-temperature alloy powder hot isostatic pressing process |
CN103834831B (en) * | 2014-03-11 | 2016-03-30 | 武汉理工大学 | In crystal grain, nano yttrium oxide disperse strengthens nickel-base composite material and preparation method thereof |
CN106536781B (en) | 2014-07-23 | 2018-04-13 | 株式会社Ihi | The manufacture method of Ni alloy parts |
CN104263998B (en) * | 2014-09-18 | 2016-06-22 | 中国华能集团公司 | A kind of Technology for Heating Processing of ni-fe-cr-boron system high temperature alloy |
CN105821359B (en) * | 2016-04-11 | 2018-03-09 | 西安欧中材料科技有限公司 | A kind of Technology for Heating Processing of high-ductility nickel-base alloy |
CN107052345A (en) * | 2016-12-28 | 2017-08-18 | 江苏精研科技股份有限公司 | Copper alloy injection molding process |
CN106834870B (en) * | 2017-02-15 | 2018-05-11 | 江苏省海洋资源开发研究院(连云港) | Ni-Al2O3Composite material near-net-shape method |
CN107127348A (en) * | 2017-06-15 | 2017-09-05 | 北京康普锡威科技有限公司 | A kind of preparation method of MIM metal dusts |
CN107775005B (en) * | 2017-11-29 | 2019-08-02 | 安徽恒利增材制造科技有限公司 | A kind of injection molding method of high-strength aluminum alloy turbine wheel |
CN108161275B (en) * | 2018-01-08 | 2021-02-02 | 河北工业大学 | Nickel-based alloy weld structure grain refinement method and application thereof |
CN108461748B (en) * | 2018-03-23 | 2020-09-15 | 格林美(无锡)能源材料有限公司 | Lithium ion battery single crystal anode material and preparation method thereof |
CN108611507B (en) * | 2018-04-25 | 2020-06-05 | 北京航空航天大学 | Hot isostatic pressing near-net forming method based on powder reprocessing |
FR3080786A1 (en) * | 2018-05-03 | 2019-11-08 | Commissariat A L'energie Atomique Et Aux Energies Alternatives | ODS ALLOY POWDER AND PROCESS FOR PRODUCING THE SAME BY PLASMA PROCESSING |
CN110014145B (en) * | 2019-04-18 | 2020-10-23 | 北京科技大学 | Preparation method of spherical ferrite-based powder |
CN110343908A (en) * | 2019-08-30 | 2019-10-18 | 江苏奇纳新材料科技有限公司 | The hip moulding and heat treatment process of IN718 alloy powder and its alloy |
CN111926207B (en) * | 2020-08-27 | 2021-12-14 | 北京科技大学 | Method for preparing nickel-based alloy |
CN112632716A (en) * | 2020-11-17 | 2021-04-09 | 北京科技大学 | Defect visualization analysis method for preparing turbine through powder injection molding and preparation method of titanium-aluminum alloy turbine |
CN112453413B (en) * | 2020-11-20 | 2023-05-12 | 中科南京绿色制造产业创新研究院 | Preparation method of oxide dispersion strengthening steel spherical powder for 3D printing |
CN114015908B (en) * | 2021-09-28 | 2022-09-06 | 深圳艾利门特科技有限公司 | Nickel-phosphorus alloy and preparation method and application thereof |
CN114058895B (en) * | 2021-11-16 | 2023-01-17 | 陕西宝锐金属有限公司 | Double nozzle spray forming Y 2 O 3 Process for particle reinforced Monel 400 alloy plate |
CN117020204A (en) * | 2023-08-22 | 2023-11-10 | 钢研昊普科技有限公司 | 20CrNiMo bearing piece and preparation method and application thereof |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1814379A (en) * | 2006-03-07 | 2006-08-09 | 北京科技大学 | Method for preparing Al2O3 dispersion-strengthened Ni Al base composite material |
CN101948970A (en) * | 2010-10-13 | 2011-01-19 | 北京科技大学 | Mechanical alloying method for preparing strengthened dispersion alloy of nickel-based oxide |
CN101979691A (en) * | 2010-10-13 | 2011-02-23 | 北京科技大学 | Method for preparing oxide dispersion strengthened cobalt-based super alloy |
-
2011
- 2011-06-30 CN CN2011101807442A patent/CN102251131B/en not_active Expired - Fee Related
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1814379A (en) * | 2006-03-07 | 2006-08-09 | 北京科技大学 | Method for preparing Al2O3 dispersion-strengthened Ni Al base composite material |
CN101948970A (en) * | 2010-10-13 | 2011-01-19 | 北京科技大学 | Mechanical alloying method for preparing strengthened dispersion alloy of nickel-based oxide |
CN101979691A (en) * | 2010-10-13 | 2011-02-23 | 北京科技大学 | Method for preparing oxide dispersion strengthened cobalt-based super alloy |
Non-Patent Citations (2)
Title |
---|
《球磨时间对镍基ODS合金拉伸性能的影响》;陈嵩等;《材料科学与工艺》;20100831;第18卷(第4期);第486-488页 * |
陈嵩等.《球磨时间对镍基ODS合金拉伸性能的影响》.《材料科学与工艺》.2010,第18卷(第4期),第486-488页. |
Also Published As
Publication number | Publication date |
---|---|
CN102251131A (en) | 2011-11-23 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN102251131B (en) | Method for preparing injection-molding nickel-base ODS (oxide dispersion strengthened) alloy | |
CN103240412B (en) | Method for preparing powder super-alloy by near net shape | |
CN101716686B (en) | Short-flow preparation method of micro-sized spherical titanium powder | |
CN102554242B (en) | Method for manufacturing micro-fine spherical titanium powder | |
CN103240418A (en) | Near-net shaping method for charging turbine with hollow internal structure | |
CN103233182B (en) | Forming method for nanometer beta' phase element and nanometer oxide composite reinforced Fe-based ODS alloy | |
CN102925780B (en) | Titanium alumel material and preparation technology thereof | |
CN101948970A (en) | Mechanical alloying method for preparing strengthened dispersion alloy of nickel-based oxide | |
CN107096924A (en) | The preparation method and product of a kind of spherical metal base rare earth nano composite powder available for 3 D-printing | |
CN102127713B (en) | Oxide dispersion-strengthening ferrite steel with bicrystal structure and production method thereof | |
CN104004942B (en) | TiC particle-reinforced nickel-based composite material and preparation method thereof | |
CN105274445A (en) | Oxide-dispersion-strengthened low-activation steel and preparation method thereof | |
CN110014145B (en) | Preparation method of spherical ferrite-based powder | |
CN105397085B (en) | A kind of method that discharge plasma sintering prepares Ni-base P/M Superalloy | |
CN110576185A (en) | Nanocrystalline high-entropy alloy powder and preparation method thereof | |
CN102211193B (en) | Manufacture process of changeable geometrical cross-section turbocharger nozzle blade | |
CN113458402A (en) | Method for preparing high-temperature alloy powder by using nickel-based high-temperature alloy powder return material | |
CN102286694A (en) | Oxidation-resistant iron-based high-temperature alloy and preparation method thereof | |
CN103056378A (en) | Preparation method for sphere-like tungsten powder | |
CN111266571B (en) | Adhesive, TiAl alloy turbine injection molding preparation method and product | |
CN110039062B (en) | Method for preparing spherical nickel-based powder | |
CN102765941A (en) | Ceramic powder turbocharger nozzle ring installation disk and manufacturing method of ceramic powder turbocharger nozzle ring installation disk | |
CN109877312A (en) | A kind of preparation method of spherical shape ferrite base ODS alloy powder | |
CN105039793A (en) | Nano-featured enhanced aluminum-based composite and preparing method thereof | |
CN102690977A (en) | Method for preparing gamma' phase strengthened cobalt-based ODS alloy by using solution method |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20121128 |