CN103240412B - Method for preparing powder super-alloy by near net shape - Google Patents
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Abstract
Disclosed is a method for preparing powder super-alloy by a near net shape. Firstly, high-purity intermediate alloy powder is prepared by the aid of vacuum melting and air jet pulverization technology. Secondly, the intermediate alloy powder and fine particle diameter metal powder (such as carbonyl nickel powder, carbonyl iron powder, reduction tungsten powder and reduction molybdenum powder) are mixed in a high-energy ball mill with protective atmosphere to obtain mixed powder. The mixed powder and paraffin base binders are uniformly premixed, feedstock with a uniform rheological performance is obtained by mixing and is formed on an injection forming machine to obtain a blank in a complicated shape. The binders are removed from the blank in the complicated shape by the aid of solvent degreasing and hot degreasing technologies, the degreased blank is sintered in the vacuum atmosphere, the sintered blank is further compacted by the aid of unjacketed hot isostatic pressure, and finally, a super-alloy part in the complicated shape is obtained by the aid of solid solution and aging treatment. Raw material powder cost and technological energy consumption are remarkably reduced, and prepared super-alloy is almost fully compact, uniform in structure and excellent in comprehensive mechanical property.
Description
Technical field
The invention belongs to Powder Injection Molding Technology field, provide especially a kind of nearly end form to prepare the method for powder superalloy.
Background technology
Powder superalloy has good elevated temperature strength and anti-oxidant corrosion resistance, and excellent antifatigue and creep-resistant property, fracture property and structure stability are many modern national defense equipments and the irreplaceable critical material of the development of the national economy.The alloying level of powder superalloy is high, conventional cast product often exist serious component segregation and tissue odds even, its performance can not be brought into play completely.Compare with cast superalloy, powder superalloy have structural constituent evenly, without advantages such as gross segregations, its combination property is more excellent.When preparing powder superalloy part, traditional handicraft generally uses " atomized alloy powder-high temperature insostatic pressing (HIP) (hot extrusion)-isothermal forging-machining " technique, when manufacturing complex-shaped parts (particularly small complex part), toward contact, need more machining processes, utilization rate of raw materials is low, and, superalloy machinability is poor, part manufacturing cost is very high, and this has limited the extensive use of powder superalloy.Powder injection forming has aspect the small parts of 3 D complex shape and has unique advantage in preparation in batches, such as the hot-end component in locomotive engine turbocharger (as charging turbine, adjusting vane etc.), and the less high temperature parts such as high pressure blade, cellular turbine seal, locking nut and adjusting rod of the size in aero-engine.Yet up to this point, injection moulding powder metallurgy superalloy product does not obtain industrial applications widely yet, its reason mainly contains two: the one, and product sintering densification difficulty, required sintering temperature is higher, and sintering warpage is often larger, and finished product rate is low; The 2nd, powder injection forming often needs the attritive powder (particle mean size ~ 10 μ m) of selecting granularity less, and the productive rate that existing alloy powder production technology is produced attritive powder is low, manufacturing cost is high, and particularly the source of the fine superalloy powder of high-quality (low oxygen content, few nonmetal inclusion) is extremely limited.The present invention, from reducing the angle of material powder cost, carries out alloying by adding fine intermediate alloy powder, and adopts injection molding technology preparation to have the superalloy part of complicated shape.
Summary of the invention
The object of the present invention is to provide a kind of method that adopts injection molding technology to prepare complicated shape superalloy part.The mixed-powder of intermediate alloy powder and fine pure metal powder (as carbonyl nickel powder, carbonyl iron dust, reduction tungsten powder, reduction molybdenum powder etc.) of take is raw material, by the chemical composition gradient increasing between Specific Surface Area Measurement and distortion of lattice, raising powder, improve the driving gesture of sintering process Atom migration, reduce sintering temperature, sintering process can be carried out under the condition that there is no liquid phase or only have a small amount of liquid phase to occur.The method contributes to solve product sintering warpage problem, can also significantly reduce material powder cost and process energy consumption.
First the present invention adopts vacuum melting and airflow pulverization to prepare high cleanliness intermediate alloy powder; then in thering is the high energy ball mill of protective atmosphere, fine grain metal dust (carbonyl nickel powder, carbonyl iron dust, super-fine cobalt powder, reduction tungsten powder, reduction molybdenum powder etc.) is mixed with intermediate alloy powder, obtain distributed components, there is suitable apparent density and mobility and have compared with the mixed-powder of macrolattice distortion.Then, mixed-powder and the premixed of paraffinic base binding agent is even, and mixed-powder obtains the uniform feeding of rheological property after mixing, and feeding is shaped on injection machine, obtains required complicated shape base substrate.Adopt the method for solvent degreasing+hot degreasing to remove binding agent, degreasing blank is sintering in vacuum atmosphere, and sintered blank adopts cladless HIP further densified, finally carry out solid solution and Ageing Treatment, obtain complicated shape superalloy part, as shown in Figure 1, concrete technology step has preparation technology:
1, material powder preparation: according to the kind of alloying element in target superalloy and content design intermediate alloy, the content of matrix element in intermediate alloy (Fe, Ni or Co) is 25-40wt.%, all the other are active element (as Cr, Ti, Al, Ta, Nb, Zr, Hf, B, Re and C), and the mass ratio of various active elements is consistent with the mass ratio of each element in target superalloy.Intermediate alloy carries out melting in vacuum induction melting furnace, obtains intermediate alloy ingot casting.Then, intermediate alloy ladle barrow is whittled into chip, and chip is broken into fine grained on high speed disintegrator.Fine grained is further by air-flow crushing refinement, and gas pressure is 3 ~ 8MPa, and separation wheel frequency is 40 ~ 60Hz, obtains the intermediate alloy powder of average grain diameter≤10 μ m.In high-purity Ar atmosphere (99.999%), fine grain (2-10 μ m) metal dust (as carbonyl nickel powder, carbonyl iron dust, super-fine cobalt powder, reduction tungsten powder, reduction molybdenum powder etc.) is carried out to high-energy ball milling with intermediate alloy powder, obtain mixed-powder;
The iron-base superalloy that described target superalloy is various standard brands (such as K213, GH2036, GH2038 or GH2132 etc.), nickel base superalloy (such as K418, Ren é 104, GH4049 or GH4169 etc.), cobalt base superalloy (Mar-M509, FSX-414, Mar-M302 or Haynes25 etc.), or according to the non-standard alloy of actual condition design;
2, mixing: it is that under the condition of turn/min of 30-50, mixing 60-120min makes the uniform feeding of rheological property in 135-150 ℃, rotating speed that particle diameter is less than to the mixed-powder of 20 μ m and paraffinic base binding agent in double-planet mixing roll, and wherein powder loading is 60-64vol%;
In described paraffinic base binding agent, the content of each constituent element is: 15-30wt.% low density polyethylene (LDPE), 10-15wt.% polypropylene, 5-7wt.% stearic acid and surplus paraffin;
2, injection moulding: direct injection moulding on injection machine, injection temperature is that 135-150 ℃, injection pressure are 70-110MPa, obtains complicated shape base substrate;
3, degreasing: adopt solvent degreasing and hot degreasing two step degreasing process, first solution-off 6-12h in trichloro-ethylene; Then in high-purity argon gas atmosphere, carry out hot degreasing and presintering.Degreasing process is: the heating rate with 2 ℃/min is heated to 250 ℃ of insulation 2h, then the heating rate with 3 ℃/min is heated to 420 ℃ of insulation 1h, heating rate with 5 ℃/min is heated to 500 ℃ of insulation 0.5h again, finally, at 650-750 ℃ of presintering 1-1.5h, obtains degreasing blank;
4, sintering: degreasing blank carries out sintering in vacuum atmosphere, vacuum is 1 * 10
-4pa, sintering temperature is 1180-1240 ℃, temperature retention time is 60-180min, obtains sintered blank;
5, cladless HIP: sintered blank is carried out cladless HIP in the temperature range of 1150-1200 ℃, pressure is 100-200MPa, temperature retention time is 60-120min, obtains full densification (density is greater than 99%) base substrate;
6, heat treatment: full dense green is carried out solution treatment at 1150-1200 ℃, water-cooled after insulation 1-2h, then carries out Ageing Treatment at 650-700 ℃, finally obtains complicated shape superalloy.
The present invention makes intermediate alloy in advance alloy with high activity element (as Cr, Ti, Al, Ta, Nb, Zr, Hf, B, Re and C), then with the form of intermediate alloy, rather than the form of individual element is added in material, be not subject to the restriction of the conditions such as alloying element is oxidizable, can effectively avoid the oxidation of active element, be conducive to reduce oxygen content, expanded the approach of alloying.Intermediate alloy is easily broken, is convenient to obtain fine alloy powder.The cost of material powder is lower, can reduce sintering temperature, sintering process can be carried out under the condition that there is no liquid phase or only have a small amount of liquid phase to occur, contribute to solve product sintering warpage problem, the dimensional accuracy of sample can be improved, material powder cost and process energy consumption can also be significantly reduced.The superalloy of preparing approaches full densification, institutional framework is even, comprehensive mechanical property is excellent.
Accompanying drawing explanation
Fig. 1 is process chart of the present invention.
The specific embodiment
embodiment 1: nearly end form is prepared iron-base superalloy K213
According to the composition of iron-base superalloy K213 (35wt.%Ni, 15wt.%Cr, 1.8wt.%Al, 3.5wt.%Ti, 5wt.%W, 0.08wt.%B, 0.08wt.%C and surplus Fe) design intermediate alloy, in intermediate alloy, the content of matrix element Fe is 25wt.%, all the other are active element, wherein W
cr: W
al: W
ti: W
b: W
c=15:1.8:3.5:0.08:0.08).Intermediate alloy carries out melting in vacuum induction melting furnace, obtains intermediate alloy ingot casting.Then, intermediate alloy ladle barrow is whittled into chip, and this chip is broken into fine grained on high speed disintegrator.Fine grained is further by air-flow crushing refinement, and gas pressure is 8MPa, and separation wheel frequency is 60Hz, and obtaining average grain diameter is the intermediate alloy powder of 6.6 μ m.In high-purity Ar atmosphere (99.999%), fine grain (2-10 μ m) metal dust (as carbonyl nickel powder, carbonyl iron dust, reduction tungsten powder) and intermediate alloy powder are carried out to high-energy ball milling, obtain mixed-powder.The composition of paraffinic base binding agent is: 15wt.% low density polyethylene (LDPE), 15wt.% polypropylene, 6wt.% stearic acid and surplus paraffin.First by mixed-powder and paraffinic base binding agent, in double-planet mixing roll, in 135 ℃, rotating speed, be that under the condition of 30 turn/min, mixing 120min makes the uniform feeding of rheological property, powder loading is 60vol.%.Feeding is injection moulding on CJ80-E type injection machine, and injection temperature is 140 ℃, and injection pressure is 100MPa, obtains complicated shape base substrate.Complicated shape base substrate in trichloro-ethylene in 40 ℃ of solution-off 10h, then hot degreasing in high-purity argon gas atmosphere, degreasing process is: the heating rate with 2 ℃/min is heated to 250 ℃ of insulation 2h, then the heating rate with 3 ℃/min is heated to 420 ℃ of insulation 1h, heating rate with 5 ℃/min is heated to 500 ℃ of insulation 0.5h again, finally, at 650 ℃ of presintering 1.5h, obtain degreasing blank.Degreasing base sintering in vacuum atmosphere, vacuum is 1 * 10
-4pa, sintering temperature is 1180 ℃, temperature retention time is 180min, obtains sintered blank.Sintered blank is carried out cladless HIP at 1100 ℃, and pressure is 200MPa, and temperature retention time is 120min, obtains full dense green.Full dense green water-cooled after 1150 ℃ of solution treatment 2h, then at 650 ℃ of Ageing Treatment 2h, obtains complicated shape superalloy part.
embodiment 2: nearly end form is prepared nickel base superalloy K418
According to the composition of nickel base superalloy K418 (13%Cr, 6.0%Al, 0.8%Ti, 4.2%Mo, 2.3%Nb, 0.04%B, 0.09%Zr, 0.08%C and surplus Ni) design intermediate alloy, in intermediate alloy, the content of matrix element Ni is 30wt.%, all the other are active element, and the mass ratio of each active element is: W
cr: W
al: W
ti: W
nb: W
b: W
zr: W
c=13:6:0.8:2.3:0.04:0.09:0.08).Intermediate alloy carries out melting in vacuum induction melting furnace, obtains intermediate alloy ingot casting.Intermediate alloy carries out melting in vacuum induction melting furnace, obtains intermediate alloy ingot casting.Then, intermediate alloy ladle barrow is whittled into chip, and this chip is broken into fine grained on high speed disintegrator.Fine grained is further by air-flow crushing refinement, and gas pressure is 6MPa, and separation wheel frequency is 50Hz, and obtaining average grain diameter is the intermediate alloy powder of 7.2 μ m.In high-purity Ar atmosphere (99.999%), fine grain (2-10 μ m) metal dust (as carbonyl nickel powder, reduction molybdenum powder) is carried out to high-energy ball milling with intermediate alloy powder, obtain mixed-powder; The composition of paraffinic base binding agent is: 20wt.% low density polyethylene (LDPE), 12wt.% polypropylene, 5wt.% stearic acid and surplus paraffin.First by mixed-powder and paraffinic base binding agent, in double-planet mixing roll, in 140 ℃, rotating speed, be that under the condition of 35 turn/min, mixing 90min makes the uniform feeding of rheological property, powder loading is 62vol.%.Feeding is injection moulding on CJ80-E type injection machine, and injection temperature is 135 ℃, and injection pressure is 110MPa, obtains complicated shape base substrate.Complicated shape base substrate in trichloro-ethylene in 40 ℃ of solution-off 10h, then hot degreasing in high-purity argon gas atmosphere, degreasing process is: the heating rate with 2 ℃/min is heated to 250 ℃ of insulation 2h, then the heating rate with 3 ℃/min is heated to 420 ℃ of insulation 1h, heating rate with 5 ℃/min is heated to 500 ℃ of insulation 0.5h again, finally, at 700 ℃ of presintering 1.5h, obtain degreasing blank.Degreasing base sintering in vacuum atmosphere, vacuum is 1 * 10
-4pa, sintering temperature is 1200 ℃, temperature retention time is 180min, obtains sintered blank.Sintered blank is carried out cladless HIP at 1100 ℃, and pressure is 200MPa, and temperature retention time is 120min, obtains full dense green.Full dense green water-cooled after 1180 ℃ of solution treatment 2h, then at 680 ℃ of Ageing Treatment 2h, obtains complicated shape superalloy part.
embodiment 3: nearly end form is prepared nickel base superalloy Ren é 104
According to the composition of nickel base superalloy Ren é 104 (20%Co, 13%Cr, 3.8%Mo, 3.4%Al, 3.7%Ti, 2.1%W, 0.9Nb, 0.05%C, 0.025%B, 0.05%Zr, 2.4%Ta and surplus Ni) design intermediate alloy, in intermediate alloy, the content of matrix element Ni is 35wt.%, all the other are active element, and the mass ratio of each active element is: W
cr: W
al: W
ti: W
nb: W
c: W
b: W
zr: W
ta=13:3.4:3.7:0.9:0.05:0.025:0.05:2.4).Intermediate alloy carries out melting in vacuum induction melting furnace, obtains intermediate alloy ingot casting.Intermediate alloy carries out melting in vacuum induction melting furnace, obtains intermediate alloy ingot casting.Then, intermediate alloy ladle barrow is whittled into chip, and this chip is broken into fine grained on high speed disintegrator.Fine grained is further by air-flow crushing refinement, and gas pressure is 5MPa, and separation wheel frequency is 40Hz, and obtaining average grain diameter is the intermediate alloy powder of 8.0 μ m.In high-purity Ar atmosphere (99.999%), fine grain (2-10 μ m) metal dust (as super-fine cobalt powder, carbonyl nickel powder, reduction tungsten powder, reduction molybdenum powder) is carried out to high-energy ball milling with intermediate alloy powder, obtain mixed-powder.The composition of paraffinic base binding agent is: 25wt.% low density polyethylene (LDPE), 10wt.% polypropylene, 7wt.% stearic acid and surplus paraffin.First by mixed-powder and paraffinic base binding agent, in double-planet mixing roll, in 145 ℃, rotating speed, be that under the condition of 40 turn/min, mixing 90min makes the uniform feeding of rheological property, powder loading is 64vol.%.Feeding is injection moulding on CJ80-E type injection machine, and injection temperature is 145 ℃, and injection pressure is 80MPa, obtains complicated shape base substrate.Complicated shape base substrate in trichloro-ethylene in 40 ℃ of solution-off 10h, then hot degreasing in high-purity argon gas atmosphere, degreasing process is: the heating rate with 2 ℃/min is heated to 250 ℃ of insulation 2h, then the heating rate with 3 ℃/min is heated to 420 insulation 1h, heating rate with 5 ℃/min is heated to 500 ℃ of insulation 0.5h again, finally, at 750 ℃ of presintering 1h, obtain degreasing blank.Degreasing base sintering in vacuum atmosphere, vacuum is 1 * 10
-4pa, sintering temperature is 1210 ℃, temperature retention time is 180min, obtains sintered blank.Sintered blank is carried out cladless HIP at 1100 ℃, and pressure is 200MPa, and temperature retention time is 120min, obtains full dense green.Full dense green water-cooled after 1200 ℃ of solution treatment 2h, then at 680 ℃ of Ageing Treatment 2h, obtains complicated shape superalloy part.
embodiment 4: nearly end form is prepared cobalt base superalloy Mar-M509
According to the composition of cobalt base superalloy Mar-M509 (10%Ni, 24%Cr, 7%W, 3.5%Ta, 0.2%Ti, 0.5%Zr, 0.6%C and surplus cobalt) design intermediate alloy, in intermediate alloy, the content of matrix element Co is 40wt.%, all the other are active element, and the mass ratio of each active element is: W
cr: W
ta: W
ti: W
zr: W
c=24:3.5:0.2:0.5:0.6).Intermediate alloy carries out melting in vacuum induction melting furnace, obtains intermediate alloy ingot casting.Intermediate alloy carries out melting in vacuum induction melting furnace, obtains intermediate alloy ingot casting.Then, intermediate alloy ladle barrow is whittled into chip, and this chip is broken into fine grained on high speed disintegrator.Fine grained is further by air-flow crushing refinement, and gas pressure is 3MPa, and separation wheel frequency is 40Hz, and obtaining average grain diameter is the intermediate alloy powder of 9.6 μ m.In high-purity Ar atmosphere (99.999%), fine grain (2-10 μ m) metal dust (as carbonyl nickel powder, reduction tungsten powder, super-fine cobalt powder) is carried out to high-energy ball milling with intermediate alloy powder, obtain mixed-powder; The composition of paraffinic base binding agent is: 30wt.% low density polyethylene (LDPE), 15 wt.% polypropylene, 5wt.% stearic acid and surplus paraffin.First by mixed-powder and paraffinic base binding agent, in double-planet mixing roll, in 150 ℃, rotating speed, be that under the condition of 50 turn/min, mixing 60min makes the uniform feeding of rheological property, powder loading is 63vol.%.Feeding is injection moulding on CJ80-E type injection machine, and injection temperature is 150 ℃, and injection pressure is 70MPa, obtains complicated shape base substrate.Complicated shape base substrate in trichloro-ethylene in 40 ℃ of solution-off 10h, then hot degreasing in high-purity argon gas atmosphere, degreasing process is: the heating rate with 2 ℃/min is heated to 250 ℃ of insulation 2h, then the heating rate with 3 ℃/min is heated to 420 ℃ of insulation 1h, heating rate with 5 ℃/min is heated to 500 ℃ of insulation 0.5h again, finally, at 700 ℃ of presintering 1.5h, obtain degreasing blank.Degreasing base sintering in vacuum atmosphere, vacuum is 1 * 10
-4pa, sintering temperature is 1240 ℃, temperature retention time is 180min, obtains sintered blank.Sintered blank is carried out cladless HIP at 1100 ℃, and pressure is 200MPa, and temperature retention time is 120min, obtains full dense green.Full dense green water-cooled after 1180 ℃ of solution treatment 2h, then at 700 ℃ of Ageing Treatment 2h, obtains complicated shape superalloy part.
Claims (2)
1. nearly end form is prepared a method for powder superalloy, it is characterized in that:
Step 1, according to the kind of alloying element in target superalloy and content design intermediate alloy, in intermediate alloy, the content of matrix element is 25-40wt.%, all the other are active elements, and the mass ratio of various active elements is consistent with the mass ratio of each element in target superalloy;
Intermediate alloy carries out melting in vacuum induction melting furnace, obtains intermediate alloy ingot casting;
Then, intermediate alloy ladle barrow is whittled into chip, and chip is broken into fine grained on high speed disintegrator;
Fine grained further obtains intermediate alloy powder by air-flow crushing refinement, and gas pressure is 3-8MPa, and separation wheel frequency is 40-60Hz;
On high energy ball mill, in 99.999% high-purity Ar atmosphere, intermediate alloy powder is mixed with 2-10 μ m fine grain metal dust, obtain mixed-powder; Matrix element is Fe, Ni or Co, and active element is Cr, Ti, Al, Ta, Nb, Zr, Hf, B, Re and C, and metal dust is carbonyl nickel powder, carbonyl iron dust, super-fine cobalt powder, reduction tungsten powder, reduction molybdenum powder;
Step 2, particle diameter is less than to the mixed-powder of 20 μ m and paraffinic base binding agent is that under the condition of turn/min of 30-50, mixed 60-120min makes the uniform feeding of rheological property in 135-150 ℃, rotating speed in double-planet mixing roll, and wherein powder loading is 60-64vol%;
Step 3, on injection machine direct injection moulding, injection temperature is that 135-150 ℃, injection pressure are 70-110MPa, obtains complicated shape base substrate;
Step 4, employing solvent degreasing and hot degreasing two step degreasing process, first solution-off 6-12h in trichloro-ethylene; Then in high-purity argon gas atmosphere, carry out hot degreasing and presintering; Degreasing process is: the heating rate with 2 ℃/min is heated to 250 ℃ of insulation 2h, then the heating rate with 3 ℃/min is heated to 420 ℃ of insulation 1h, heating rate with 5 ℃/min is heated to 500 ℃ of insulation 0.5h again, finally, at 650-750 ℃ of presintering 1-1.5h, obtains degreasing blank;
Step 5, degreasing blank carry out sintering in vacuum atmosphere, and vacuum is 1 * 10
-4pa, sintering temperature is 1180-1240 ℃, temperature retention time is 60-180min, obtains sintered blank;
Step 6, sintered blank are carried out cladless HIP in the temperature range of 1150-1200 ℃, and pressure is 100-200MPa, and temperature retention time is 60-120min, obtain the full dense green that density is greater than 99%;
Step 7, full dense green are carried out solution treatment at 1150-1200 ℃, and water-cooled after insulation 1-2h, then carries out Ageing Treatment at 650-700 ℃, finally obtains complicated shape superalloy.
2. nearly end form is prepared the method for powder superalloy according to claim 1, it is characterized in that: iron-base superalloy, nickel base superalloy, cobalt base superalloy that described target superalloy is various standard brands, or according to the non-standard alloy of actual condition design; Iron-base superalloy is that K213, GH2036, GH2038 or GH2132, nickel base superalloy are that K418, Ren é 104, GH4049 or GH4169, cobalt base superalloy are Mar-M509, FSX-414, Mar-M302 or Haynes25;
Average grain diameter≤10 μ the m of intermediate alloy powder;
In described paraffinic base binding agent, the content of each constituent element is: 15-30wt.% low density polyethylene (LDPE), 10-15wt.% polypropylene, 5-7wt.% stearic acid and surplus paraffin.
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