CN108546834A - A kind of nickel base superalloy master alloy sublimate method of smelting - Google Patents
A kind of nickel base superalloy master alloy sublimate method of smelting Download PDFInfo
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- C22C1/00—Making non-ferrous alloys
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Abstract
A kind of sublimate method of smelting of nickel base superalloy master alloy, steps are as follows：(1) hydrochloric acid and supersound process are carried out to raw material metal；Prepare CaO CaF2Pre-melted slag；Pre-melted slag is uniformly mixed to simultaneously briquetting with pure nickel powder；(2) raw material and briquetting are put into togerther in crucible, are vacuumized；C, Nb, Ti, Al are added after fusing；B and Zr is added in applying argon gas, until aluminium alloy is poured into after melting again in punching block, obtains high temperature alloy ingot casting；Oxide skin, the riser for removing ingot casting, obtain high temperature alloy fine fodder；(3) fine fodder is put into copper crucible；It vacuumizes, is melted, quickly solidify, obtain high temperature alloy master alloy.Slag refining is carried out when vacuum induction melting of the present invention, sulphur, phosphorus content are low；Copper crucible can avoid pollution of the crucible to alloy melt；Magnetic suspension can promote non-metallic inclusion to float；Oxygen, nitrogen content are low, to reduce the quantity of the non-metallic inclusion formed in aluminium alloy cooling, process of setting；It is easy to operate using the smelting equipment of existing maturation.
Description
Technical field
The invention belongs to the sublimate melting fields of high temperature alloy, are related to the melting of nickel base superalloy.
Background technology
Nickel base superalloy is the preferred material of aero-engine hot-end component (blade and the turbine disk), master alloy it is pure
Degree is the key factor for influencing its service life.The degree of purity of master alloy includes the harmful elements such as oxygen, nitrogen, sulphur, phosphorus and nonmetallic
Field trash.Currently, the sublimate melting technique of high temperature alloy master alloy is mainly vacuum induction melting (Vacuum Induction
Melting,VIM).The advantages of process for vacuum induction smelting is technology maturation, simple and easy to do, is answered extensively in the industrial production
With.But the high temperature alloy for requiring degree of purity very high, there are still following deficiencies for VIM technologies：The pollution problem of ceramic crucible；
It cannot remove the harmful elements such as sulphur removal, phosphorus；It cannot be removed effectively non-metallic inclusion.
Vacuum magnetic suspension melting technique (Vacuum Magnetic Levitation Melting, VMLM) uses copper crucible
As reactor, molten steel is in suspended state in fusion process, avoids pollution of the sidewall of crucible to molten steel；It incudes the huge of generation
Lorentz force being capable of removal of inclusions well；Have the characteristics that rapidly and efficiently.
The present invention is directed to vacuum induction melting (VIM) above shortcomings, proposes a kind of nickel base superalloy master alloy
Sublimate melting technique, i.e. the double melting technique of vacuum induction melting+vacuum magnetic suspension melting (VIM+VMLM).
Invention content
Present invention aims at provide a kind of sublimate melting technique of nickel base superalloy master alloy, it is intended to improve Ni-based
The degree of purity of high temperature alloy master alloy.Nickel base superalloy of the present invention, chemical composition ranges include《GB/T
The classification of 14992-2005 high temperature alloys and intermetallic compound high-temperature material and the trade mark》Nickel is the high temperature of essential element in standard
Alloy.
A kind of nickel base superalloy master alloy sublimate method of smelting, it is characterised in that the high temperature alloy includes《GB/T
The classification of 14992-2005 high temperature alloys and intermetallic compound high-temperature material and the trade mark》Nickel is the high temperature of essential element in standard
Alloy；Specific process step is：
(1) pretreatment of raw material and briquetting：With blocky pure nickel, pure chromium, pure cobalt, pure tungsten, pure molybdenum, pure niobium, fine aluminium, pure titanium, pure
Iron, high purity graphite and boron, zirconium are pre-processed as raw material, and the purity of various raw material is all higher than 99.9%；It prepares
CaF2Percentage composition is the CaO-CaF of 5~20wt.%2Slag is melted, keep the temperature 10~30min postcoolings, and Mechanical Crushing at
The pre-melted slag of 0.1~5mm of granularity；Pre-melted slag and pure nickel powder are pressed 1:1~1:5 (mass ratioes) are uniformly mixed, and are pressed into
It is blocky；Briquetting is toasted using preceding in heat-treatment furnace, and temperature is 200~300 DEG C, and the time is 6~10 hours, removes it
In moisture；
(2) various raw material in step (1) are weighed in proportion, first will with the lower element Ni, Cr of O, N affinity, Co, W,
Mo, Fe metal derby and CaO-CaF2Fritting slag briquetting is put into togerther in the crucible of vacuum induction melting, is carried out vacuum melting and is obtained
The ratio that high temperature alloy ingot casting, wherein briquetting account for alloy raw material is 3~9wt.%；Crucible material is magnesia；
(3) by after the high temperature alloy ingot casting scale removal of step (2) preparation, riser, high temperature alloy fine fodder is obtained；
(4) high temperature alloy fine fodder prepared by step (3) melting in the copper crucible of vacuum magnetic suspension smelting furnace is put into obtain
High temperature alloy master alloy.
Further, described pre-process of step (1) is：Raw material metal is located in advance in 5vol.% aqueous hydrochloric acid solutions
Reason, removes oxide on surface, and pretreatment time is 20~40min；Various raw material metals after HCl treatment are placed on anhydrous
It is ultrasonically treated in ethyl alcohol, processing time is 10~20min.
Further, step (2) the vacuum melting step is：It is evacuated to 5 × 10-1Pa~5 × 10-3Pa is melted
Refining；C is added after melt is melting down, refines 15~30min；Strong nitride and oxide forming elements Nb, Ti, Al is added, heats
It is completely melt to added material；To 1.0~2.0kPa easy scaling loss and volatile micro- B and Zr is added, simultaneously in applying argon gas
It is stirred, until aluminium alloy is poured into after being completely melt again in punching block.
Further, step (4) described melting step is：It is evacuated to 5 × 10-3Pa is then charged with high-purity argon gas extremely
0.01Pa, the step is in triplicate with clean vacuum chambers；It is melted, fusion temperature is 1350~1450 DEG C, and soaking time is
10~20min；It is quickly solidified by the way of water flowing cooling.
The present invention uses vacuum induction melting+vacuum magnetic suspension melting double melting technique (VIM+VMLM), relative to existing
There is technology, has the following advantages that：
(1) CaO-CaF is added when vacuum induction melting2Pre-melted slag, has carried out slag refining, and sulphur, phosphorus content are low；
(2) pollution that copper crucible can be to avoid crucible material under high temperature to alloy melt when vacuum magnetic suspension melting；
(3) the sufficiently large Lorentz force that magnetic suspension generates can promote non-metallic inclusion to float, to effectively remove
Non-metallic inclusion；
(4) oxygen, nitrogen content are low, to reduce the non-gold such as the oxide, the nitride that are formed in aluminium alloy cooling, process of setting
Belong to the quantity of field trash；
(5) this method utilizes the smelting equipment of existing maturation, easy to operate.
Specific implementation mode
Embodiment 1：FGH96 high temperature alloy master alloy sublimate meltings
Using blocky pure nickel, pure chromium, pure cobalt, pure tungsten, pure molybdenum, pure niobium, fine aluminium, pure titanium, high purity graphite and boron, zirconium etc. as
The purity of raw material, various raw materials is all higher than 99.9%；Raw material metal is pre-processed in 5vol.% aqueous hydrochloric acid solutions,
Remove oxide on surface, pretreatment time 30min；Then various raw material metals are placed in absolute ethyl alcohol and are carried out at ultrasound
Reason, processing time 15min.Prepare CaF2Percentage composition is the CaO-CaF of 10wt.%2Slag carries out fritting processing, is completely melt
After keep 25min, then cool down, and Mechanical Crushing is at the pre-melted slag of granularity 1mm.Then pre-melted slag and pure nickel powder are pressed 1:1 into
Row uniformly mixing, and briquetting.Briquetting is carrying out 220 DEG C of bakings using preceding, and the time is 7 hours, removes moisture therein.First true
It is put into the crucible of empty induction melting furnace and is accounted for O, N affinity lower element Ni, Cr, Co, W, Mo, Fe and briquetting, briquetting
The ratio of alloy raw material is wt.3%；It is evacuated to 5 × 10-2Pa carries out melting；C is added after melt is melting down, refines
25min；Strong nitride and oxide forming elements Nb, Ti, Al is added, is heated to added material and is completely melt；Applying argon gas arrives
1.5kPa is eventually adding easy scaling loss and volatile micro- B and Zr, is carried out at the same time stirring, until aluminium alloy is complete again
It is poured into punching block after fusing, obtains high temperature alloy ingot casting；After high temperature alloy ingot casting scale removal, riser, high temperature is obtained
Alloy fine fodder；High temperature alloy fine fodder is put into the copper crucible of vacuum magnetic suspension smelting furnace, is evacuated to 5 × 10-3Then Pa fills
Enter high-purity argon gas to 0.01Pa, the step is in triplicate with clean vacuum chambers；Remelting is carried out, fusion temperature is 1350~1450
DEG C, soaking time is 10~20min；It is quickly solidified by the way of water flowing cooling, obtains high temperature alloy master alloy.
Embodiment 2：FGH96 high temperature alloy master alloy sublimate meltings
Using blocky pure nickel, pure chromium, pure cobalt, pure tungsten, pure molybdenum, pure niobium, fine aluminium, pure titanium, high purity graphite and boron, zirconium etc. as
The purity of raw material, various raw materials is all higher than 99.9%；Raw material metal is pre-processed in 5vol.% aqueous hydrochloric acid solutions,
Remove oxide on surface, pretreatment time 30min；Then various raw material metals are placed in absolute ethyl alcohol and are carried out at ultrasound
Reason, processing time 15min.Prepare CaF2Percentage composition is the CaO-CaF of 15wt.%2Slag carries out fritting processing, is completely melt
After keep 25min, then cool down, and Mechanical Crushing is at the pre-melted slag of granularity 1mm.Then pre-melted slag and pure nickel powder are pressed 1:2 into
Row uniformly mixing, and briquetting.Briquetting is carrying out 230 DEG C of bakings using preceding, and the time is 8 hours, removes moisture therein.First true
It is put into the crucible of empty induction melting furnace and is accounted for O, N affinity lower element Ni, Cr, Co, W, Mo, Fe and briquetting, briquetting
The ratio of alloy raw material is 5wt.%；It is evacuated to 5 × 10-2Pa carries out melting；C is added after melt is melting down, refines
25min；Strong nitride and oxide forming elements Nb, Ti, Al is added, is heated to added material and is completely melt；Applying argon gas arrives
1.5kPa is eventually adding easy scaling loss and volatile micro- B and Zr, is carried out at the same time stirring, until aluminium alloy is complete again
It is poured into punching block after fusing, obtains high temperature alloy ingot casting；After high temperature alloy ingot casting scale removal, riser, high temperature is obtained
Alloy fine fodder；High temperature alloy fine fodder is put into the copper crucible of vacuum magnetic suspension smelting furnace, is evacuated to 5 × 10-3Then Pa fills
Enter high-purity argon gas to 0.01Pa, the step is in triplicate with clean vacuum chambers；Remelting is carried out, fusion temperature is 1350~1450
DEG C, soaking time is 10~20min；It is quickly solidified by the way of water flowing cooling, obtains high temperature alloy master alloy.
Embodiment 3：GH4169 high temperature alloy master alloy sublimate meltings
Using blocky pure nickel, pure chromium, pure molybdenum, pure niobium, fine aluminium, pure titanium, pure iron, high purity graphite and boron, zirconium etc. as former material
Material, the purity of various raw materials are all higher than 99.9%；Raw material metal is pre-processed in 5vol.% aqueous hydrochloric acid solutions, removal
Oxide on surface, pretreatment time 25min；Then various raw material metals are placed in absolute ethyl alcohol and are ultrasonically treated,
Processing time is 15min.Prepare CaF2Percentage composition is the CaO-CaF of wt.10%2Slag carries out fritting processing, after being completely melt
25min is kept, is then cooled down, and Mechanical Crushing is at the pre-melted slag of granularity 1mm.Then pre-melted slag and pure nickel powder are pressed 1:1 carries out
Uniformly mixing, and briquetting.Briquetting is carrying out 220 DEG C of bakings using preceding, and the time is 7 hours, removes moisture therein.First in vacuum
It is put into the crucible of induction melting furnace and accounts for alloy original with O, N affinity lower element Ni, Cr, Mo, Fe and briquetting, briquetting
The ratio of material is 3wt.%；It is evacuated to 5 × 10-2Pa carries out melting；C is added after melt is melting down, refines 25min；It is added
Strong nitride and oxide forming elements Nb, Ti, Al are heated to added material and are completely melt；Applying argon gas finally adds to 1.5kPa
Enter easy scaling loss and volatile micro- B and Zr, be carried out at the same time stirring, until aluminium alloy is poured into steel after being completely melt again
In mould, high temperature alloy ingot casting is obtained；After high temperature alloy ingot casting scale removal, riser, high temperature alloy fine fodder is obtained；By high temperature
Alloy fine fodder is put into the copper crucible of vacuum magnetic suspension smelting furnace, is evacuated to 5 × 10-3Pa is then charged with high-purity argon gas extremely
0.01Pa, the step is in triplicate with clean vacuum chambers；Remelting is carried out, fusion temperature is 1350~1450 DEG C, and soaking time is
10~20min；It is quickly solidified by the way of water flowing cooling, obtains high temperature alloy master alloy.
Embodiment 4：GH4169 high temperature alloy master alloy sublimate meltings
With blocky pure nickel, pure chromium, pure cobalt, pure tungsten, pure molybdenum, pure niobium, fine aluminium, pure titanium, pure iron, high purity graphite and boron, zirconium
It is all higher than 99.9% Deng the purity as raw material, various raw materials；Raw material metal carries out in advance in 5vol.% aqueous hydrochloric acid solutions
Processing removes oxide on surface, pretreatment time 35min；Then various raw material metals are placed in absolute ethyl alcohol and are carried out
It is ultrasonically treated, processing time 15min.Prepare CaF2Percentage composition is the CaO-CaF of wt.15%2Slag carries out fritting processing, complete
25min is kept after running down, is then cooled down, and Mechanical Crushing is at the pre-melted slag of granularity 1mm.Then pre-melted slag and pure nickel powder are pressed
1:2 are uniformly mixed, and briquetting.Briquetting is carrying out 270 DEG C of bakings using preceding, and the time is 7 hours, removes moisture therein.
Elder generation is put into the crucible of vacuum induction melting furnace and O, N affinity lower element Ni, Cr, Co, W, Mo, Fe and briquetting,
The ratio that briquetting accounts for alloy raw material is 5wt.%；It is evacuated to 5 × 10-2Pa carries out melting；C is added after melt is melting down, essence
Refine 20min；Strong nitride and oxide forming elements Nb, Ti, Al is added, is heated to added material and is completely melt；Applying argon gas arrives
1.5kPa is eventually adding easy scaling loss and volatile micro- B and Zr, is carried out at the same time stirring, until aluminium alloy is complete again
It is poured into punching block after fusing, obtains high temperature alloy ingot casting；After high temperature alloy ingot casting scale removal, riser, high temperature is obtained
Alloy fine fodder；High temperature alloy fine fodder is put into the copper crucible of vacuum magnetic suspension smelting furnace, is evacuated to 5 × 10-3Then Pa fills
Enter high-purity argon gas to 0.01Pa, the step is in triplicate with clean vacuum chambers；Remelting is carried out, fusion temperature is 1350~1450
DEG C, soaking time is 10~20min；It is quickly solidified by the way of water flowing cooling, obtains high temperature alloy master alloy.
Several embodiments of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
Cannot the limitation to the scope of the claims of the present invention therefore be interpreted as.The present disclosure applies equally to other nickel base superalloy master alloys
Sublimate melting.It should be pointed out that for those of ordinary skill in the art, before not departing from present inventive concept
It puts, various modifications and improvements can be made, these are all within the scope of protection of the present invention.Therefore, the guarantor of patent of the present invention
Shield range should be determined by the appended claims.
Claims (4)
1. a kind of nickel base superalloy master alloy sublimate method of smelting, it is characterised in that the high temperature alloy includes《GB/T
The classification of 14992-2005 high temperature alloys and intermetallic compound high-temperature material and the trade mark》Nickel is the high temperature of essential element in standard
Alloy；Specific process step is：
(1) pretreatment of raw material and briquetting：With blocky pure nickel, pure chromium, pure cobalt, pure tungsten, pure molybdenum, pure niobium, fine aluminium, pure titanium, pure iron, height
Pure graphite and boron, zirconium are pre-processed as raw material, and the purity of various raw material is all higher than 99.9%；Prepare CaF2Percentage
Content is the CaO-CaF of 5~20wt.%2Slag is melted, and keeps the temperature 10~30min postcoolings, and Mechanical Crushing is at granularity 0.1
The pre-melted slag of~5mm；Pre-melted slag and pure nickel powder are pressed 1:1~1:5 (mass ratioes) are uniformly mixed, and are pressed into bulk；Pressure
Block is toasted using preceding in heat-treatment furnace, and temperature is 200~300 DEG C, and the time is 6~10 hours, removes water therein
Point；
(2) various raw material in step (1) are weighed in proportion, first will with the lower element Ni, Cr of O, N affinity, Co, W, Mo,
Fe metal derbies and CaO-CaF2Fritting slag briquetting is put into togerther in the crucible of vacuum induction melting, is carried out vacuum melting and is obtained high temperature
The ratio that alloy cast ingot, wherein briquetting account for alloy raw material is 3~9wt.%；Crucible material is magnesia；
(3) by after the high temperature alloy ingot casting scale removal of step (2) preparation, riser, high temperature alloy fine fodder is obtained；
(4) high temperature alloy fine fodder prepared by step (3) is put into melting in the copper crucible of vacuum magnetic suspension smelting furnace and obtains high temperature
Alloy master alloy.
2. a kind of nickel base superalloy master alloy sublimate method of smelting as described in claim 1, it is characterised in that step (1) institute
Stating pretreatment is：Raw material metal is pre-processed in 5vol.% aqueous hydrochloric acid solutions, oxide on surface is removed, when pretreatment
Between be 20~40min；Various raw material metals after HCl treatment are placed in absolute ethyl alcohol and are ultrasonically treated, processing time
For 10~20min.
3. a kind of nickel base superalloy master alloy sublimate method of smelting as described in claim 1, it is characterised in that step (2) institute
Stating vacuum melting step is：It is evacuated to 5 × 10-1Pa~5 × 10-3Pa carries out melting；C is added after melt is melting down, refines
15~30min；Strong nitride and oxide forming elements Nb, Ti, Al is added, is heated to added material and is completely melt；Applying argon gas
To 1.0~2.0kPa, easy scaling loss and volatile micro- B and Zr is added, is carried out at the same time stirring, until aluminium alloy is complete again
It is poured into punching block after running down.
4. a kind of nickel base superalloy master alloy sublimate method of smelting as described in claim 1, it is characterised in that step (4) institute
Stating melting step is：It is evacuated to 5 × 10-3Pa is then charged with high-purity argon gas to 0.01Pa, and the step is true to clean in triplicate
Empty room；It is melted, fusion temperature is 1350~1450 DEG C, and soaking time is 10~20min；Using water flowing cooling by the way of into
Row quickly solidification.
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