CN102251131A - 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
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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, by 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 service requirements.
Ni-based ODS alloy is the potential equivalent material of turbine in blade in the advanced internal combustion turbine and the automobile turbocharger, but Ni-based ODS hardness of alloy height, plasticity is low and formability is poor, be difficult to prepare parts such as complex-shaped blade or turbine by 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 in the internal combustion turbine and moderate, the complex-shaped part of turbine equidimension in the vehicle turbocharger, it has series of advantages such as near-net forming, homogeneous microstructure, performance height, precision height and cost are 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.Pulverize the district to spraying to inject after the formula airflow milling utilizes superonic flow nozzzle that high pressure gas are quickened, 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 by feeding gun by carrying gas, under radiation, convection current, conduction and four kinds of heat transfer mechanism effects of chemistry, heated rapidly and melted, melt granules forms spherical droplets under surface tension effects, and under high thermograde, solidify rapidly, thereby obtain spherical powder.
As seen, can obtain to be fit to the fine particle spherical powder of injection molding process after the mechanical alloy powder is handled by airflow milling refinement and plasma body nodularization, 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, then the mechanical alloying powder is carried out pre-treatment (airflow milling refinement and plasma body nodularization) to obtain the tiny and spheric injection forming powder stock of particle diameter, 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 as shown in Figure 1, concrete processing step is:
1, mechanical alloying: with Co-based alloy powder, Y
2O
3The crude granule pre-mixing of particle and Hf unit is even, then in high-purity Ar atmosphere by high-energy ball milling 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 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 by spray formula airflow milling is carried out dispersion and fining.Control the particle diameter of powder by pilot-gas flow, operating pressure, sorting energy 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.As seen from the 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 by 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, and the nodularization effect of powder is remarkable as can be seen;
4, mixing: it is that mixing 0.5-1.5h makes 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 binding agent mix the back, and wherein the powder loading capacity is 55-65vol%.
Described binding agent adopts cerul multicomponent polymeric system, and the ratio of each constituent element is: 50-70wt% paraffin, 10-20% high density polyethylene(HDPE), 10-20% polypropylene and surplus 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, soaks 5-12h in 45-60 ℃ earlier in organic solvents such as trieline or trichloroethane; 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 ℃ temperature range, 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 the following preparation of quality percentage composition 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 binding agent mix the back and make even feeding in 150 ℃ of mixing 1h on duplicate rows star mixing rolls, wherein binding agent is made up of 63% paraffin, 13% high density polyethylene(HDPE), 17% polypropylene, 7% stearic acid, and the powder loading capacity 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 the following preparation of quality percentage composition 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 binding agent mix the back and make even feeding in 155 ℃ of mixing 1.5h on duplicate rows star mixing rolls, wherein binding agent is made up of 55% paraffin, 20% high density polyethylene(HDPE), 15% polypropylene, 10% stearic acid, and the powder loading capacity 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 the following preparation of quality percentage composition 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 binding agent mix the back and make even feeding in 160 ℃ of mixing 1.5h on duplicate rows star mixing rolls, wherein binding agent is made up of 60% paraffin, 15% high density polyethylene(HDPE), 15% polypropylene, 10% stearic acid, and the powder loading capacity 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 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 altogether with plasma spheroidization powdered preparation γ ' and 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 the following preparation of quality percentage composition 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 binding agent mix the back and make even feeding in 155 ℃ of mixing 2h on duplicate rows star mixing rolls, wherein binding agent is made up of 55% paraffin, 20% high density polyethylene(HDPE), 10% polypropylene, 15% stearic acid, and the powder loading capacity 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 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 by high-energy ball milling
2O
3Particle and Hf element uniform particles are dispersed in the Ni matrix, add 0.5～5wt% 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 binding agent mix the back and carry out the mixing even feeding that obtains in 145-170 ℃ on mixing rolls, binding agent is made up of 50-70wt% paraffin, 10-20% high density polyethylene(HDPE), 10-20% polypropylene and surplus stearic acid, and the powder loading capacity is 55-65vol%; Feeding is 145-165 ℃ in injection temperature, and injection pressure is an injection forming under the condition of 70-90MPa, 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, soaks 8-12h earlier in trieline, 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. according to the described method for preparing the Ni-based ODS alloy of injection forming of claim 1, it is characterized in that: the Co-based alloy powder that adopts in a step is the nickel base superalloy of various standard brands, or according to the non-standard alloying constituent of actual condition design; Powdered alloy adopts element powders to mix, and perhaps adopts high pressure gas atomizing or water atomization to carry out pre-alloyed; Nickel base superalloy is selected from: Nimonic 90, Inconel 718, Inconel 713C, Hastelloy X, GH4195 or GH4195.
3. according to the described 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 described method for preparing the Ni-based ODS alloy of injection forming of claim 1, it is characterized in that: in the sintering process of the hot degreasing of the airflow milling fragmentation of the high-energy ball milling of b step, c step, f step and g step, adopt the argon gas of purity more than 99.999% as protective atmosphere.
5. according to the described 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.
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