CN103240412A - Method for preparing powder super-alloy by near net shape - Google Patents
Method for preparing powder super-alloy by near net shape Download PDFInfo
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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 the powder injection forming technical field, provide a kind of nearly end form to prepare the method for powder superalloy especially.
Background technology
The powder superalloy has good high-temperature intensity 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 height of powder superalloy, conventional cast product often exist serious component segregation and tissue odds to spare, and its performance can not be brought into play fully.Compare with cast superalloy, the powder superalloy has advantages such as structural constituent is even, no gross segregation, and 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 " technology, when making complex-shaped parts (particularly small-sized complex parts), need more machining processes toward contact, utilization rate of raw materials is low, and, the superalloy machinability is poor, part manufacturing cost is very high, and this has limited the extensive use of powder superalloy.Powder injection forming has in prepared in batches and has special advantages aspect the small-sized parts of 3 D complex shape, the high temperature parts such as high pressure blade, cellular turbine seal, locking nut and adjusting rod that for example hot-end component (as charging turbine, adjusting vane etc.) in the locomotive engine turbocharger, and the size in the aero-engine is less.Yet up to this point, injection moulding powder metallurgy superalloy product does not obtain industrial applications widely yet, and its reason mainly contains two: the one, and product sintering densification difficulty, required sintering temperature is higher, and sintering warpage is often bigger, and the finished product rate is low; The 2nd, powder injection forming often needs the attritive powder (particle mean size ~ 10 μ m) of selecting for use granularity less, and the productive rate that existing alloy powder production technology is produced attritive powder is low, the source of the fine superalloy powder of manufacturing cost height, particularly high-quality (low oxygen content, few nonmetal inclusion) is extremely limited.The present invention carries out alloying from reducing the angle of material powder cost by adding fine intermediate alloy powder, and adopts the 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.Mixed-powder with intermediate alloy powder and fine pure metal powder (as carbonyl nickel powder, carbonyl iron dust, reduction tungsten powder, reduction molybdenum powder etc.) is raw material, improve the driving gesture of atomic migration in the sintering process by the chemical composition gradient that increases between the long-pending and distortion of lattice of specific surface area, raising powder, reduce sintering temperature, sintering process can be carried out under the condition that does not have liquid phase or have only a small amount of liquid phase to occur.This method helps to solve product sintering warpage problem, can also significantly reduce material powder cost and process energy consumption.
The present invention at first adopts vacuum melting and air-flow crushing technology to prepare high cleanliness intermediate alloy powder; in having the high energy ball mill of protective atmosphere, mix in fine grain metal dust (carbonyl nickel powder, carbonyl iron dust, super-fine cobalt powder, reduction tungsten powder, reduction molybdenum powder etc.) and the intermediate alloy powder then, obtain distributed components, have suitable apparent density and flowability and have the mixed-powder that distorts than macrolattice.Then, mixed-powder and the premixed of paraffinic base binding agent is even, and mixed-powder obtains the uniform feeding of rheological property through after mixing, and feeding is shaped at 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, carry out solid solution and Ageing Treatment at last, obtain complicated shape superalloy part, preparation technology as shown in Figure 1, concrete processing step has:
1, material powder preparation: according to kind and the content design intermediate alloy of alloying element in the target superalloy, the content of matrix element in the 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 the target superalloy.Intermediate alloy carries out melting in vacuum induction melting furnace, obtain the intermediate alloy ingot casting.Then, the intermediate alloy ladle barrow is whittled into chip, and chip is broken into fine grained at high speed disintegrator.Further by the air-flow dispersion and fining, gas pressure is 3 ~ 8MPa to fine grained, and the 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 high-energy ball milling with the intermediate alloy powder, obtain mixed-powder;
The iron-base superalloy that described target superalloy is various standard brands (for example K213, GH2036, GH2038 or GH2132 etc.), nickel base superalloy (for example 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: be that the condition of 30-50 commentaries on classics/min under mixing 60-120min make rheological property uniform feeding in 135-150 ℃, rotating speed less than the mixed-powder of 20 μ m and paraffinic base binding agent with particle diameter in duplicate rows star mixing roll, wherein the powder useful load is 60-64vol%;
The content of each constituent element is in the described paraffinic base binding agent: 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 are that 135-150 ℃, injection pressure are 70-110MPa, obtain the complicated shape base substrate;
3, degreasing: adopt solvent degreasing and two step of hot degreasing degreasing process, solution-off 6-12h in trichloro-ethylene earlier; In high-purity argon gas atmosphere, carry out hot degreasing and presintering then.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, at 650-750 ℃ of presintering 1-1.5h, obtains degreasing blank at last;
4, sintering: degreasing blank carries 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;
5, cladless HIP: sintered blank is carried out cladless HIP in 1150-1200 ℃ temperature range, and pressure is 100-200MPa, and 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 ℃, and water-cooled behind the insulation 1-2h is carried out Ageing Treatment at 650-700 ℃ then, finally obtains the complicated shape superalloy.
The present invention makes intermediate alloy in advance to 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 the material, be not subjected to the restriction of conditions such as the easy oxidation of alloying element, can effectively avoid the oxidation of active element, be conducive to reduce oxygen content, enlarged the approach of alloying.Intermediate alloy is broken easily, is convenient to obtain the fine alloy powder.The cost of material powder is lower, can reduce sintering temperature, sintering process can be carried out under the condition that does not have liquid phase or have only a small amount of liquid phase to occur, help 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.
Description of drawings
Fig. 1 is process chart of the present invention.
The specific embodiment
Embodiment 1: nearly end form prepares iron-base superalloy K213
Composition (35wt.%Ni, 15wt.%Cr, 1.8wt.%Al, 3.5wt.%Ti, 5wt.%W, 0.08wt.%B, 0.08wt.%C and surplus Fe) design intermediate alloy according to iron-base superalloy K213, the content of matrix element Fe is 25wt.% in the intermediate alloy, 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, obtain the intermediate alloy ingot casting.Then, the intermediate alloy ladle barrow is whittled into chip, and this chip is broken into fine grained at high speed disintegrator.Further by the air-flow dispersion and fining, gas pressure is 8MPa to fine grained, and the 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 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.Be that the condition of 30 commentaries on classics/mins under mixing 120min make rheological property uniform feeding in 135 ℃, rotating speed with mixed-powder and paraffinic base binding agent in duplicate rows star mixing roll at first, the powder useful load is 60vol.%.Feeding is injection moulding on CJ80-E type injection machine, and injection temperature is 140 ℃, and injection pressure is 100MPa, obtains the complicated shape base substrate.The complicated shape base substrate in trichloro-ethylene in 40 ℃ of solution-off 10h, hot degreasing in high-purity argon gas atmosphere then, 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, at 650 ℃ of presintering 1.5h, obtain degreasing blank at last.Degreasing base sintering in vacuum atmosphere, vacuum are 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 behind 1150 ℃ of solution treatment 2h then at 650 ℃ of Ageing Treatment 2h, obtains complicated shape superalloy part.
Embodiment 2: nearly end form prepares nickel base superalloy K418
Composition (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 according to nickel base superalloy K418, the content of matrix element Ni is 30wt.% in the intermediate alloy, 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, obtain the intermediate alloy ingot casting.Intermediate alloy carries out melting in vacuum induction melting furnace, obtain the intermediate alloy ingot casting.Then, the intermediate alloy ladle barrow is whittled into chip, and this chip is broken into fine grained at high speed disintegrator.Further by the air-flow dispersion and fining, gas pressure is 6MPa to fine grained, and the 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 high-energy ball milling with the 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.Be that the condition of 35 commentaries on classics/mins under mixing 90min make rheological property uniform feeding in 140 ℃, rotating speed with mixed-powder and paraffinic base binding agent in duplicate rows star mixing roll at first, the powder useful load is 62vol.%.Feeding is injection moulding on CJ80-E type injection machine, and injection temperature is 135 ℃, and injection pressure is 110MPa, obtains the complicated shape base substrate.The complicated shape base substrate in trichloro-ethylene in 40 ℃ of solution-off 10h, hot degreasing in high-purity argon gas atmosphere then, 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, at 700 ℃ of presintering 1.5h, obtain degreasing blank at last.Degreasing base sintering in vacuum atmosphere, vacuum are 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 behind 1180 ℃ of solution treatment 2h then at 680 ℃ of Ageing Treatment 2h, obtains complicated shape superalloy part.
Embodiment 3: nearly end form prepares nickel base superalloy Ren é 104
Composition (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 according to nickel base superalloy Ren é 104, the content of matrix element Ni is 35wt.% in the intermediate alloy, 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, obtain the intermediate alloy ingot casting.Intermediate alloy carries out melting in vacuum induction melting furnace, obtain the intermediate alloy ingot casting.Then, the intermediate alloy ladle barrow is whittled into chip, and this chip is broken into fine grained at high speed disintegrator.Further by the air-flow dispersion and fining, gas pressure is 5MPa to fine grained, and the 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 high-energy ball milling with the 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.Be that the condition of 40 commentaries on classics/mins under mixing 90min make rheological property uniform feeding in 145 ℃, rotating speed with mixed-powder and paraffinic base binding agent in duplicate rows star mixing roll at first, the powder useful load is 64vol.%.Feeding is injection moulding on CJ80-E type injection machine, and injection temperature is 145 ℃, and injection pressure is 80MPa, obtains the complicated shape base substrate.The complicated shape base substrate in trichloro-ethylene in 40 ℃ of solution-off 10h, hot degreasing in high-purity argon gas atmosphere then, 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, at 750 ℃ of presintering 1h, obtain degreasing blank at last.Degreasing base sintering in vacuum atmosphere, vacuum are 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 behind 1200 ℃ of solution treatment 2h then at 680 ℃ of Ageing Treatment 2h, obtains complicated shape superalloy part.
Embodiment 4: nearly end form prepares cobalt base superalloy Mar-M509
Composition (10%Ni, 24%Cr, 7%W, 3.5%Ta, 0.2%Ti, 0.5%Zr, 0.6%C and surplus cobalt) design intermediate alloy according to cobalt base superalloy Mar-M509, the content of matrix element Co is 40wt.% in the intermediate alloy, 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, obtain the intermediate alloy ingot casting.Intermediate alloy carries out melting in vacuum induction melting furnace, obtain the intermediate alloy ingot casting.Then, the intermediate alloy ladle barrow is whittled into chip, and this chip is broken into fine grained at high speed disintegrator.Further by the air-flow dispersion and fining, gas pressure is 3MPa to fine grained, and the 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 high-energy ball milling with the 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.Be that the condition of 50 commentaries on classics/mins under mixing 60min make rheological property uniform feeding in 150 ℃, rotating speed with mixed-powder and paraffinic base binding agent in duplicate rows star mixing roll at first, the powder useful load is 63vol.%.Feeding is injection moulding on CJ80-E type injection machine, and injection temperature is 150 ℃, and injection pressure is 70MPa, obtains the complicated shape base substrate.The complicated shape base substrate in trichloro-ethylene in 40 ℃ of solution-off 10h, hot degreasing in high-purity argon gas atmosphere then, 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, at 700 ℃ of presintering 1.5h, obtain degreasing blank at last.Degreasing base sintering in vacuum atmosphere, vacuum are 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 behind 1180 ℃ of solution treatment 2h then at 700 ℃ of Ageing Treatment 2h, obtains complicated shape superalloy part.
Claims (2)
1. a nearly end form prepares the method for powder superalloy, it is characterized in that:
Step 1, according to the kind of alloying element in the target superalloy and content design intermediate alloy, the content of matrix element is 25-40wt.% in the intermediate alloy, all the other are active elements, and the mass ratio of various active elements is consistent with the mass ratio of each element in the target superalloy;
Intermediate alloy carries out melting in vacuum induction melting furnace, obtain the intermediate alloy ingot casting;
Then, the intermediate alloy ladle barrow is whittled into chip, and chip is broken into fine grained at high speed disintegrator;
Fine grained further obtains the intermediate alloy powder by the air-flow dispersion and fining, and gas pressure is 3 ~ 8MPa, and the separation wheel frequency is 40 ~ 60Hz;
On high energy ball mill, in 99.999% high-purity Ar atmosphere, the 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, be that the condition of 30-50 commentaries on classics/min under mixing 60-120min make rheological property uniform feeding in 135-150 ℃, rotating speed less than the mixed-powder of 20 μ m and paraffinic base binding agent with particle diameter in duplicate rows star mixing roll, wherein the powder useful load is 60-64vol%;
Step 3, on injection machine direct injection moulding, injection temperature is that 135-150 ℃, injection pressure are 70-110MPa, obtains the complicated shape base substrate;
Step 4, employing solvent degreasing and two step of hot degreasing degreasing process, solution-off 6-12h in trichloro-ethylene earlier; In high-purity argon gas atmosphere, carry out hot degreasing and presintering then; 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, at 650-750 ℃ of presintering 1-1.5h, obtains degreasing blank at last;
Step 5, degreasing blank carry out sintering in vacuum atmosphere, 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 1150-1200 ℃ temperature range, pressure is 100-200MPa, and temperature retention time is 60-120min, obtain density greater than 99% full dense green;
Step 7, full dense green are carried out solution treatment at 1150-1200 ℃, and water-cooled behind the insulation 1-2h is carried out Ageing Treatment at 650-700 ℃ then, finally obtains the complicated shape superalloy.
2. the method for preparing the powder superalloy according to the described nearly end form of 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 K213, GH2036, GH2038 or GH2132, nickel base superalloy for being Mar-M509, FSX-414, Mar-M302 or Haynes25 as K418, Ren é 104, GH4049 or GH4169, cobalt base superalloy;
Prepare the method for powder superalloy according to the described nearly end form of claim 1, it is characterized in that: the average grain diameter of intermediate alloy powder≤10 μ m;
Prepare the method for powder superalloy according to the described nearly end form of claim 1, it is characterized in that: the content of each constituent element is in the described paraffinic base binding agent: 15-30wt.% low density polyethylene (LDPE), 10-15wt.% polypropylene, 5-7wt.% stearic acid and surplus paraffin.
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