CN102268563B - Casting high temperature alloy refiner and high temperature alloy casting method using the same - Google Patents
Casting high temperature alloy refiner and high temperature alloy casting method using the same Download PDFInfo
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- CN102268563B CN102268563B CN 201010189406 CN201010189406A CN102268563B CN 102268563 B CN102268563 B CN 102268563B CN 201010189406 CN201010189406 CN 201010189406 CN 201010189406 A CN201010189406 A CN 201010189406A CN 102268563 B CN102268563 B CN 102268563B
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- 239000000956 alloy Substances 0.000 title claims abstract description 57
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000005266 casting Methods 0.000 title claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 71
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 55
- 238000005245 sintering Methods 0.000 claims abstract description 54
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 44
- 238000000465 moulding Methods 0.000 claims abstract description 36
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 35
- 230000006698 induction Effects 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 238000002360 preparation method Methods 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 238000002844 melting Methods 0.000 claims abstract description 16
- 238000005516 engineering process Methods 0.000 claims abstract description 15
- 230000008018 melting Effects 0.000 claims abstract description 15
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 10
- 239000010937 tungsten Substances 0.000 claims abstract description 10
- 230000002829 reductive effect Effects 0.000 claims abstract description 9
- 239000006025 fining agent Substances 0.000 claims description 73
- 229910000601 superalloy Inorganic materials 0.000 claims description 68
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 33
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 32
- 239000001257 hydrogen Substances 0.000 claims description 28
- 229910052739 hydrogen Inorganic materials 0.000 claims description 28
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 24
- 238000000498 ball milling Methods 0.000 claims description 24
- 239000003870 refractory metal Substances 0.000 claims description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 12
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 11
- 229910000838 Al alloy Inorganic materials 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 229910000851 Alloy steel Inorganic materials 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 8
- 230000001681 protective effect Effects 0.000 claims description 8
- ZCUFMDLYAMJYST-UHFFFAOYSA-N thorium dioxide Chemical compound O=[Th]=O ZCUFMDLYAMJYST-UHFFFAOYSA-N 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 5
- 238000000462 isostatic pressing Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 7
- 238000000748 compression moulding Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 235000015895 biscuits Nutrition 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- 229910052727 yttrium Inorganic materials 0.000 description 4
- 230000003068 static effect Effects 0.000 description 3
- 230000009931 harmful effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000007663 fining method Methods 0.000 description 1
- 238000009415 formwork Methods 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- MOWMLACGTDMJRV-UHFFFAOYSA-N nickel tungsten Chemical compound [Ni].[W] MOWMLACGTDMJRV-UHFFFAOYSA-N 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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Abstract
A preparation technology of a casting high temperature alloy refiner comprises steps of: mixing micronsized nickel powder, tungsten powder and high-melting metal oxide powder; then moulding by isothermal sintering under a reductive atmosphere; and insulating to obtain a tungsten nickel-metal oxide intermediate alloy refiner. A high temperature alloy casting method using the casting high temperature alloy refiner is also required to be protected in the invention. The method comprises steps of: first, preparing the casting high temperature alloy refiner; then melting the refiner and a mother alloy of the high temperature alloy together in an induction furnace; after complete fusing of the alloy, carrying out an electromagnetic stirring with an increased power; after well mixing, reducing the power for cooling; and casting until a alloy liquid temperature reducing to a casting temperature. The invention can satisfy demand of refinement of high temperature alloy containing tungsten and endow better integral performance on the high temperature alloy.
Description
Technical field:
The present invention relates to superalloy casting technology field science, a kind of cast superalloy fining agent is provided especially and has used its superalloy castmethod.
Background technology:
In prior art, superalloy has been widely used in the fields such as Aeronautics and Astronautics, and different purposes and applied environment are not identical to the requirement of the composition of superalloy, tissue, performance yet.Some parts of aircraft engine are as relatively low in the use temperature of the structural parts such as low-pressure turbine blade and starter motor blisk.
As a rule, even tiny equiax crystal can improve the over-all properties of material.Some new castmethods can be produced very thin crystal grain in recent years, at the industrial three kinds of crystal fining methods that have commonly used, be in thermal control method, mechanical vibration method and chemical method, adopt the thermal control method, namely can obtain thinner crystal grain by the preheating temperature of controlling casting pouring temperature and formwork, but have a large amount of microporosities in foundry goods; Vibratory drilling method is by introducing mechanical vibration, makes the dendrite fragmentation that solidifies in aluminium alloy and forms more nucleus, and then make crystal grain obtain refinement, but need transformation or drop into a large amount of fund reforming equipments, and price comparison is expensive; Simple to operate, good in refining effect that chemical method has, for example: use CoO+Al
2O
3Be coated on the precise casting mould shell internal surface, make the refinement of cast(ing) surface layer tissue.The B that adds trace also has certain thinning effect, and adding in addition intermetallic compound such as Co-Nb-Ni etc. also has certain effect; But concerning superalloy, these elements can only change in very little scope, otherwise it is unstable that tissue can become, mutually harmful or low melting point phase appear, the thinning effect that a small amount of fining agent does not have, and too much fining agent also may fall low-alloyed performance, in addition, because the fusing point of superalloy is very high, fining agent at high temperature easily lost efficacy, and caused thinning effect and not obvious.Good fining agent should have high fusing point; With melt, similar crystalline structure is arranged; With melt, close density is arranged; Good dispersiveness is arranged, and the alloy performance is without harmful effect.Therefore, be necessary to adopt new fining agent to satisfy the particular requirement of superalloy industry and make foundry goods have higher performance.
Therefore, people expect the superalloy castmethod that obtains the better cast superalloy fining agent of a kind of technique effect and use it.
Summary of the invention:
The superalloy castmethod that the purpose of this invention is to provide the better cast superalloy fining agent of a kind of technique effect and use it.
The invention provides a kind of cast superalloy fining agent, it is characterized in that: the preparation technology of described cast superalloy fining agent is as follows; At first micron-sized nickel powder, tungsten powder and refractory metal oxide powder are mixed, then carry out moulding, carry out isothermal sintering under reducing atmosphere, then insulation, make tungsten nickel-metal oxide master alloy fining agent.
Cast superalloy fining agent of the present invention, also claimed following preferred content:
The preparation technology of described cast superalloy fining agent satisfies following requirement one or a combination set of:
1) described metal oxide powder is the yttrium oxide powder, a kind of in aluminium sesquioxide powder or Thorotrast powder, and its granularity is the 0.1-1 micron; The granularity of described tungsten powder and nickel powder is the 0.5-5 micron;
2) micron level tungsten powder, nickel powder and oxidate powder are carried out mixed uniformly method and specifically adopt the mechanical ball milling mode, blending agent adopts acetone or hexane, and Ball-milling Time is 1-60 hour;
3) carry out after nickel powder, tungsten powder and the refractory metal oxide powder of micron level being carried out evenly mix moulding specifically adopt mold pressing or etc. the molding modes such as static pressure;
Satisfy following requirement when 4) carrying out sintering after moulding under reducing atmosphere: adopt continous way atmosphere protection tube furnace or intermittent type atmosphere protection tube furnace to carry out sintering;
5) the sintering and reducing protective atmosphere adopts the mixed gas of high-purity hydrogen or high-purity hydrogen and high-purity nitrogen, and wherein the ratio of hydrogen and nitrogen is between (1: 1)～(1: 5); Flow can be controlled in 5～50ml/min.cm
2
6) described sintering temperature requirement is 1200 ℃-1600 ℃;
7) soaking time after described sintering is 1-3 hour.
In the preparation process of described cast superalloy fining agent, the nickel powder that uses, tungsten powder and refractory metal oxide powder proportion relation each other are: (70～90): (10～5): (5～20).
The present invention is the superalloy castmethod of claimed use cast superalloy fining agent as above also, it is characterized in that: described superalloy castmethod satisfies following requirement:
At first prepare the cast superalloy fining agent; Then with fining agent melting in induction furnace together with the superalloy mother alloy, all after fusing, add the high-power induction stirring of carrying out until alloy, the rear reduction power and lowering the temperature of stirring is poured into a mould when the aluminium alloy temperature is reduced to teeming temperature;
The preparation technology of described cast superalloy fining agent satisfies following requirement: at first nickel powder, tungsten powder and the refractory metal oxide powder with certain proportioning mixes, then carry out moulding, carry out isothermal sintering under reducing atmosphere, insulation makes tungsten nickel-metal oxide master alloy fining agent; Wherein:
1) in the preparation process of described cast superalloy fining agent, the nickel powder that uses, tungsten powder and refractory metal oxide powder proportion relation each other are: (70～90): (10～5): (5～20);
2) described metal oxide powder is the yttrium oxide powder, aluminium sesquioxide powder or Thorotrast powder, and its granularity is the 0.1-1 micron; The granularity of described tungsten powder and nickel powder is the 0.5-5 micron;
3) micron level tungsten powder, nickel powder and oxidate powder are carried out mixed uniformly method and specifically adopt the mechanical ball milling mode, blending agent adopts acetone or hexane, and Ball-milling Time is 1-60 hour;
4) carry out after nickel powder, tungsten powder and the refractory metal oxide powder of micron level being carried out evenly mix moulding specifically adopt mold pressing or etc. the molding modes such as static pressure;
Satisfy following requirement when 5) carrying out sintering after moulding under reducing atmosphere: adopt continous way atmosphere protection tube furnace or intermittent type atmosphere protection tube furnace to carry out sintering;
6) the sintering and reducing protective atmosphere adopts the mixed gas of high-purity hydrogen or high-purity hydrogen and high-purity nitrogen, and wherein the ratio of hydrogen and nitrogen is between (1: 1)～(1: 5); Flow can be controlled in 5～50ml/min.cm
2
7) described sintering temperature requirement is 1200 ℃-1600 ℃;
8) soaking time after described sintering is 1-3 hour.
In addition, when fining agent melting in vacuum induction furnace together with the mother alloy material, and thoroughization of furnace charge clear after, improve power and carry out stir process, churning time 2～10 minutes is poured into a mould after temperature drops to the normal teeming temperature of alloy, obtains at last the alloy-steel casting of refinement.
The ultimate principle that the present invention is correlated with:
The present invention adopts powder metallurgy process, according to certain proportioning, utilize tungsten nickel dystectic metal oxide particle to be bondd by high temperature sintering as binding agent, make the master alloy of required different densities, then with the melting together with the mother alloy material of a certain amount of master alloy, adopt normal casting process parameters to pour into a mould, utilize high-melting-point, tiny metal oxide particle to form great number of grains as the nucleating center, obtain at last compact grained superalloy tissue.
Innovative point of the present invention relates to a kind of new fining agent, and the demand that it can satisfy tungstenic type high temp alloy refinement makes superalloy have better over-all properties.
Description of drawings:
Fig. 1 is W-Ni-5%Y
2O
3The fining agent microstructure;
Fig. 2 is W-Ni-10%Y
2O
3The fining agent microstructure;
Fig. 3 is that alloy macrostructure (from left to right, is respectively and does not add fining agent, add 0.1%-W-Ni-5%Y
2O
3Fining agent adds 0.1%-W-Ni-10%Y
2O
3Fining agent).
Embodiment:
Embodiment 1: a kind of cast superalloy fining agent and use its superalloy castmethod
At first tungsten powder, nickel powder (0.5-3 micron) are prepared burden by a certain percentage with yttrium oxide powder (0.1-1 micron), its mass ratio is 85: 10: 5, adopt the mechanical ball milling mode evenly to mix, blending agent adopts acetone or hexane, and Ball-milling Time is 20 hours; After evenly mixing, adopt the compression molding mode that the powder mix that mixes is carried out moulding. forming pressure is 150MPa; The biscuit of moulding is put into continous way atmosphere protection tube furnace, and restitutive protection's property atmosphere adopts high-purity hydrogen, and flow control is at 20ml/min.cm
2The isothermal sintering temperature is 1500 ℃, and soaking time is 1 hour; Then the alloy furnace cooling to room temperature, makes fining agent at last, and alloy structure is seen Fig. 1; With fining agent (accounting for mass ratio 0.1%) melting in induction furnace together with superalloy K441 mother alloy (accounting for mass ratio 99.9%), after alloy all melts, add the high-power induction stirring of carrying out, churning time 2 minutes, rear reduction power and lowering the temperature stirs, pour into a mould when the aluminium alloy temperature is reduced to 1420 ℃, obtain at last the alloy-steel casting of refinement, Fig. 3 sees in foundry goods macrostructure.
Embodiment 2: a kind of cast superalloy fining agent and use its superalloy castmethod
At first tungsten powder, nickel powder (0.5-3 micron) are prepared burden by a certain percentage with yttrium oxide powder (0.1-1 micron), its mass ratio is 80: 10: 10, adopt the mechanical ball milling mode evenly to mix, blending agent adopts acetone or hexane, and Ball-milling Time is 20 hours; After evenly mixing, adopt the compression molding mode that the powder mix that mixes is carried out moulding, forming pressure is 150MPa; The biscuit of moulding is put into continous way atmosphere protection tube furnace, and restitutive protection's property atmosphere adopts high-purity hydrogen, and flow control is at 20ml/min.cm
2The isothermal sintering temperature is 1550 ℃, and soaking time is 1 hour; Then the alloy furnace cooling to room temperature, makes fining agent at last, and alloy structure is seen Fig. 2; With fining agent (accounting for mass ratio 0.1%) melting in induction furnace together with superalloy K441 mother alloy (accounting for mass ratio 99.9%), after alloy all melts, add the high-power induction stirring of carrying out, churning time 2 minutes, rear reduction power and lowering the temperature stirs, pour into a mould when the aluminium alloy temperature is reduced to 1420 ℃, obtain at last the alloy-steel casting of refinement, Fig. 3 sees in foundry goods macrostructure.
Embodiment 3: a kind of cast superalloy fining agent and use its superalloy castmethod
At first tungsten powder, nickel powder (0.5-3 micron) are prepared burden by a certain percentage with yttrium oxide powder (0.1-1 micron), its mass ratio is 70: 10: 20, adopt the mechanical ball milling mode evenly to mix, blending agent adopts acetone or hexane, and Ball-milling Time is 15 hours; After evenly mixing, adopt the compression molding mode that the powder mix that mixes is carried out moulding, forming pressure is 150MPa; The biscuit of moulding is put into continous way atmosphere protection tube furnace, and restitutive protection's property atmosphere adopts high-purity hydrogen, and flow control is at 20ml/min.cm
2The isothermal sintering temperature is 1550 ℃, and soaking time is 0.5 hour; Then the alloy furnace cooling to room temperature, makes fining agent at last; With fining agent (accounting for mass ratio 0.2%) melting in induction furnace together with superalloy K417 mother alloy (accounting for mass ratio 99.8%), after alloy all melts, add the high-power induction stirring of carrying out, churning time 3 minutes, rear reduction power and lowering the temperature stirs, pour into a mould when the aluminium alloy temperature is reduced to 1430 ℃, obtain at last the alloy-steel casting of refinement.
Embodiment 4: a kind of cast superalloy fining agent and use its superalloy castmethod
At first tungsten powder, nickel powder (0.5-3 micron) are prepared burden by a certain percentage with aluminium sesquioxide powder (0.1-1 micron), its mass ratio is 80: 10: 10, adopt the mechanical ball milling mode evenly to mix, blending agent adopts acetone or hexane, and Ball-milling Time is 30 hours; After evenly mixing, adopt the compression molding mode that the powder mix that mixes is carried out moulding, forming pressure is 150MPa; The biscuit of moulding is put into continous way atmosphere protection tube furnace, and restitutive protection's property atmosphere adopts high-purity hydrogen, and flow control is at 20ml/min.cm
2The isothermal sintering temperature is 1550 ℃, and soaking time is 2 hours; Then the alloy furnace cooling to room temperature, makes fining agent at last; With fining agent (accounting for mass ratio 0.1%) melting in induction furnace together with superalloy K418 mother alloy (accounting for mass ratio 99.9%), after alloy all melts, add the high-power induction stirring of carrying out, churning time 3 minutes, rear reduction power and lowering the temperature stirs, pour into a mould when the aluminium alloy temperature is reduced to 1430 ℃, obtain at last the alloy-steel casting of refinement.
Embodiment 5
A kind of cast superalloy fining agent, its preparation technology is as follows: at first micron-sized nickel powder, tungsten powder and refractory metal oxide powder are mixed, then carry out moulding, carry out isothermal sintering under reducing atmosphere, then insulation, make tungsten nickel-metal oxide master alloy fining agent.
The preparation technology of described cast superalloy fining agent satisfies following requirement:
1) described metal oxide powder is the yttrium oxide powder, a kind of in aluminium sesquioxide powder or Thorotrast powder, and its granularity is 1 micron; The granularity of described tungsten powder and nickel powder is 5 microns;
2) micron level tungsten powder, nickel powder and oxidate powder are carried out mixed uniformly method and specifically adopt the mechanical ball milling mode, blending agent adopts acetone or hexane, and Ball-milling Time is 60 hours;
3) carry out after nickel powder, tungsten powder and the refractory metal oxide powder of micron level being carried out evenly mix moulding specifically adopt mold pressing or etc. the molding modes such as static pressure;
Satisfy following requirement when 4) carrying out sintering after moulding under reducing atmosphere: adopt continous way atmosphere protection tube furnace or intermittent type atmosphere protection tube furnace to carry out sintering;
5) the sintering and reducing protective atmosphere adopts the mixed gas of high-purity hydrogen or high-purity hydrogen and high-purity nitrogen, and wherein the ratio of hydrogen and nitrogen is 1: 5; Flow can be controlled in 50ml/min.cm
2
6) described sintering temperature requirement is 1600 ℃;
7) soaking time after described sintering is 3 hours.
In the preparation process of described cast superalloy fining agent, the nickel powder that uses, tungsten powder and refractory metal oxide powder proportion relation each other are: 90: 5: 5.
The superalloy castmethod of cast superalloy fining agent as above, satisfy following requirement:
At first prepare the cast superalloy fining agent; Then with fining agent melting in induction furnace together with the superalloy mother alloy, all after fusing, add the high-power induction stirring of carrying out until alloy, the rear reduction power and lowering the temperature of stirring is poured into a mould when the aluminium alloy temperature is reduced to teeming temperature;
The preparation technology of described cast superalloy fining agent satisfies following requirement: at first nickel powder, tungsten powder and the refractory metal oxide powder with certain proportioning mixes, then carry out moulding, carry out isothermal sintering under reducing atmosphere, insulation makes tungsten nickel-metal oxide master alloy fining agent; Wherein:
1) in the preparation process of described cast superalloy fining agent, the nickel powder that uses, tungsten powder and refractory metal oxide powder proportion relation each other are: 90: 5: 5;
2) described metal oxide powder is yttrium oxide powder or aluminium sesquioxide powder or Thorotrast powder, and its granularity is 1 micron; The granularity of described tungsten powder and nickel powder is 5 microns;
3) micron level tungsten powder, nickel powder and oxidate powder are carried out mixed uniformly method and specifically adopt the mechanical ball milling mode, blending agent adopts acetone or hexane, and Ball-milling Time is 60 hours;
4) carry out moulding after nickel powder, tungsten powder and the refractory metal oxide powder of micron level being carried out evenly mix and specifically adopt the isostatic pressing mode;
Satisfy following requirement when 5) carrying out sintering after moulding under reducing atmosphere: adopt intermittent type atmosphere protection tube furnace to carry out sintering;
6) the sintering and reducing protective atmosphere adopts the mixed gas of high-purity hydrogen or high-purity hydrogen and high-purity nitrogen, and wherein the ratio of hydrogen and nitrogen is 1: 5; Flow can be controlled in 50ml/min.cm
2
7) described sintering temperature requirement is 1600 ℃;
8) soaking time after described sintering is 3 hours.
In addition, when fining agent melting in vacuum induction furnace together with the mother alloy material, and thoroughization of furnace charge clear after, improve power and carry out stir process, churning time 10 minutes is poured into a mould after temperature drops to the normal teeming temperature of alloy, obtains at last the alloy-steel casting of refinement.
Embodiment 6
A kind of cast superalloy fining agent, its preparation technology is as follows: at first micron-sized nickel powder, tungsten powder and refractory metal oxide powder are mixed, then carry out moulding, carry out isothermal sintering under reducing atmosphere, then insulation, make tungsten nickel-metal oxide master alloy fining agent.
The preparation technology of described cast superalloy fining agent satisfies following requirement:
1) described metal oxide powder is the yttrium oxide powder, a kind of in aluminium sesquioxide powder or Thorotrast powder, and its granularity is 0.1 micron; The granularity of described tungsten powder and nickel powder is 0.5 micron;
2) micron level tungsten powder, nickel powder and oxidate powder are carried out mixed uniformly method and specifically adopt the mechanical ball milling mode, blending agent adopts acetone or hexane, and Ball-milling Time is 1 hour;
3) carry out moulding after nickel powder, tungsten powder and the refractory metal oxide powder of micron level being carried out evenly mix and specifically adopt the compression molding mode;
Satisfy following requirement when 4) carrying out sintering after moulding under reducing atmosphere: adopt continous way atmosphere protection tube furnace to carry out sintering;
5) the sintering and reducing protective atmosphere adopts the mixed gas of high-purity hydrogen or high-purity hydrogen and high-purity nitrogen, and wherein the ratio of hydrogen and nitrogen is 1: 1; Flow can be controlled in 5ml/min.cm
2
6) described sintering temperature requirement is 1200 ℃;
7) soaking time after described sintering is 1 hour.
In the preparation process of described cast superalloy fining agent, the nickel powder that uses, tungsten powder and refractory metal oxide powder proportion relation each other are: 70: 10: 20.
The present embodiment also comprises the superalloy castmethod of using cast superalloy fining agent as above, satisfies following requirement:
At first prepare the cast superalloy fining agent; Then with fining agent melting in induction furnace together with the superalloy mother alloy, all after fusing, add the high-power induction stirring of carrying out until alloy, the rear reduction power and lowering the temperature of stirring is poured into a mould when the aluminium alloy temperature is reduced to teeming temperature;
The preparation technology of described cast superalloy fining agent satisfies following requirement: at first nickel powder, tungsten powder and the refractory metal oxide powder with certain proportioning mixes, then carry out moulding, carry out isothermal sintering under reducing atmosphere, insulation makes tungsten nickel-metal oxide master alloy fining agent; Wherein:
1) in the preparation process of described cast superalloy fining agent, the nickel powder that uses, tungsten powder and refractory metal oxide powder proportion relation each other are: 70: 10: 20;
2) described metal oxide powder is the yttrium oxide powder, aluminium sesquioxide powder or Thorotrast powder, and its granularity is 0.1 micron; The granularity of described tungsten powder and nickel powder is 0.5 micron;
3) micron level tungsten powder, nickel powder and oxidate powder are carried out mixed uniformly method and specifically adopt the mechanical ball milling mode, blending agent adopts acetone, and Ball-milling Time is 1 hour;
4) carry out moulding after nickel powder, tungsten powder and the refractory metal oxide powder of micron level being carried out evenly mix and specifically adopt the compression molding mode;
Satisfy following requirement when 5) carrying out sintering after moulding under reducing atmosphere: adopt continous way atmosphere protection tube furnace to carry out sintering;
6) the sintering and reducing protective atmosphere adopts the mixed gas of high-purity hydrogen or high-purity hydrogen and high-purity nitrogen, and wherein the ratio of hydrogen and nitrogen is 1: 1; Flow can be controlled in 5ml/min.cm
2
7) described sintering temperature requirement is 1200 ℃;
8) soaking time after described sintering is 1 hour.
In addition, when fining agent melting in vacuum induction furnace together with the mother alloy material, and thoroughization of furnace charge clear after, improve power and carry out stir process, churning time 2 minutes is poured into a mould after temperature drops to the normal teeming temperature of alloy, obtains at last the alloy-steel casting of refinement.
Claims (2)
1. cast superalloy fining agent, the preparation technology of described cast superalloy fining agent is as follows: at first micron-sized nickel powder, tungsten powder and refractory metal oxide powder are mixed, then carry out moulding, carry out isothermal sintering under reducing atmosphere, then insulation, make tungsten nickel-metal oxide master alloy fining agent;
It is characterized in that: the preparation technology of described cast superalloy fining agent satisfies following requirement:
1) nickel powder that uses, tungsten powder and refractory metal oxide powder proportion relation each other are: (70～90): (10～5): (5～20);
2) described metal oxide powder yttrium oxide specifically, aluminium sesquioxide or Thorotrast powder are wherein a kind of, and its granularity is the 0.1-1 micron; The granularity of described tungsten powder and nickel powder is the 0.5-5 micron;
3) micron level tungsten powder, nickel powder and oxidate powder are carried out mixed uniformly method and specifically adopt the mechanical ball milling mode, blending agent adopts acetone or hexane, and Ball-milling Time is 1-60 hour;
4) carry out moulding after nickel powder, tungsten powder and the refractory metal oxide powder of micron level being carried out evenly mix and specifically adopt mold pressing or isostatic pressing mode;
Satisfy following requirement when 5) carrying out sintering after moulding under reducing atmosphere: adopt continous way atmosphere protection tube furnace or intermittent type atmosphere protection tube furnace to carry out sintering;
6) the sintering and reducing protective atmosphere adopts the mixed gas of high-purity hydrogen or high-purity hydrogen and high-purity nitrogen, and wherein the ratio of hydrogen and nitrogen is between (1:1)～(1:5); Flow control is at 5～50ml/min.cm
2
7) described sintering temperature requirement is 1200 ℃-1600 ℃;
8) soaking time after described sintering is 1-3 hour.
2. a right to use requires the superalloy castmethod of 1 described cast superalloy fining agent, and it is characterized in that: described superalloy castmethod satisfies following requirement:
At first prepare the cast superalloy fining agent; Then with fining agent melting in induction furnace together with the superalloy mother alloy, all after fusing, add the high-power induction stirring of carrying out until alloy, the rear reduction power and lowering the temperature of stirring is poured into a mould when the aluminium alloy temperature is reduced to teeming temperature;
When fining agent melting in vacuum induction furnace together with the mother alloy material, and thoroughization of furnace charge clear after, improve power and carry out stir process, churning time 2～10 minutes is poured into a mould after temperature drops to the normal teeming temperature of alloy, obtains at last the alloy-steel casting of refinement;
The preparation technology of described cast superalloy fining agent satisfies following requirement: at first nickel powder, tungsten powder and the refractory metal oxide powder with certain proportioning mixes, then carry out moulding, carry out isothermal sintering under reducing atmosphere, insulation makes tungsten nickel-metal oxide master alloy fining agent; Wherein:
1) in the preparation process of described cast superalloy fining agent, the nickel powder that uses, tungsten powder and refractory metal oxide powder proportion relation each other are: (70～90): (10～5): (5～20);
2) described metal oxide powder is the yttrium oxide powder, a kind of in aluminium sesquioxide powder or Thorotrast powder, and its granularity is the 0.1-1 micron; The granularity of described tungsten powder and nickel powder is the 0.5-5 micron;
3) micron level tungsten powder, nickel powder and oxidate powder are carried out mixed uniformly method and specifically adopt the mechanical ball milling mode, blending agent adopts acetone or hexane, and Ball-milling Time is 1-60 hour;
4) carry out moulding after nickel powder, tungsten powder and the refractory metal oxide powder of micron level being carried out evenly mix and specifically adopt mold pressing or isostatic pressing mode;
Satisfy following requirement when 5) carrying out sintering after moulding under reducing atmosphere: adopt continous way atmosphere protection tube furnace or intermittent type atmosphere protection tube furnace to carry out sintering;
6) the sintering and reducing protective atmosphere adopts the mixed gas of high-purity hydrogen or high-purity hydrogen and high-purity nitrogen, and wherein the ratio of hydrogen and nitrogen is between (1:1)～(1:5); Flow control is at 5～50ml/min.cm
2
7) described sintering temperature requirement is 1200 ℃-1600 ℃;
8) soaking time after described sintering is 1-3 hour.
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| CN108330306B (en) * | 2017-10-31 | 2019-10-22 | 中国科学院金属研究所 | For in the case of the higher degree of superheat high temperature alloy fining agent and its preparation and application |
| CN110193592B (en) * | 2019-06-24 | 2021-08-31 | 阜阳佳派生产力促进中心有限公司 | Method for improving corrosion resistance of differential case |
| CN114453567B (en) * | 2022-01-27 | 2024-06-11 | 江苏大学 | High-temperature alloy solidification structure refiner and preparation method and application thereof |
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| CN101724761A (en) * | 2008-10-22 | 2010-06-09 | 沈阳工业大学 | Method for preparing nickel-tungsten-yttrium (III) oxide master alloy for casting |
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