CN109402428A - A kind of preparation method of high cleanliness powder metallurgy high-temperature alloy master alloy - Google Patents
A kind of preparation method of high cleanliness powder metallurgy high-temperature alloy master alloy Download PDFInfo
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Abstract
A kind of preparation method of high cleanliness powder metallurgy high-temperature alloy master alloy, belongs to the preparation field of high temperature alloy.Include the following steps: the purification of (1) raw material；(2) raw material surface preparation；(3) vacuum induction melting；(4) vacuum electroslag remelting；(5) vacuum consumable remelting.Using trace impurity content in the powder metallurgy high-temperature alloy master alloy of this method preparation are as follows: As < 0.00005%, Sn < 0.00007%, Pb < 0.00005%, Sb < 0.00003%, Bi < 0.00005%, K < 0.00001%, Ca < 0.00001%, S < 0.0003%, P < 0.0005%, N < 0.0008%, O < 0.0006%, the content of non-metallic inclusion are < 0.32mg/kg.Invention removes trace impurity As, Sn, Pb, Sb, Bi, K, Ca, S, P, very low oxygen, nitrogen content are obtained, reduces the quantity of oxide, nitride.
Description
Technical field
The invention belongs to the preparation fields of high temperature alloy, are related to the preparation of powder metallurgy high-temperature alloy master alloy.
Background technique
Powder metallurgy high-temperature alloy is the essential material of the critical components such as modern high performance aero-engine turbine disk, special
Point be no gross segregation, even tissue, crystal grain it is tiny, with excellent mechanical property and thermal process performance, be effectively guaranteed
The reliability and durability of engine, and can be with near-net-shape, the manufacturing cycle is short.The use of the powder turbine disk is advanced aviation
The important symbol of engine.The turbine disk prepared using domestic superalloy powder, the indexs such as service life, reliability and beauty
There are a biggish gap in the countries such as state, Russia, trace impurity and non-metallic inclusion controlled level it is lower be that it is main former
One of because.At present in China's raw material, the content of several impurity elements such as As, Sn, Pb, Sb, Bi, K, Ca is higher, other impurity
The content of element is lower.The performances such as impurity element, creep lasting to high temperature alloy can produce serious influence, it is necessary to they
Content is controlled to alap level.Powder metallurgy high-temperature alloy firstly the need of in vacuum induction melting furnace be added nickel, chromium,
A variety of alloying element raw materials such as cobalt, tungsten, molybdenum, niobium, aluminium, titanium carry out fusion smelting and are cast into the satisfactory female conjunction of chemical component
Then golden stick carries out remelting again, improve the degree of purity of master alloy.Therefore, powder metallurgy high-temperature alloy not only contains above-mentioned alloy
Element, at the same it is also miscellaneous containing detrimental traces such as oxygen, nitrogen, sulphur, phosphorus, arsenic, tin, potassium, the calcium brought by above-mentioned alloying element raw material
Prime element.Oxygen therein, nitrogen are easy to form oxide and nitride in fusion process.Due to powder metallurgy high-temperature alloy
Turbine disk use condition is harsh, so having strict requirements to master alloy, especially has to the control of trace impurity stringent
It is required that.
Raw material preparation is the first procedure in the production of powder metallurgy high-temperature alloy master alloy, is the most key process
One of.The trace impurity of powder metallurgy high-temperature alloy master alloy is mainly derived from raw material, and many impurity elements exist
It is difficult to be removed during subsequent technique.It therefore, is impurity content in control high temperature alloy using the raw material of sublimate
Maximally efficient method.Moreover, master alloy preparation is the most key process when preparing superalloy powder using atomization
One of.The low powder metallurgy high-temperature alloy master alloy of trace impurity is prepared, the parts such as the turbine disk can be significantly improved
Tissue and performance.
Advantage is significant in terms of impurity element in accurately control alloying component, removal alloy for process for vacuum induction smelting.But
Be master alloy can be generated in process of setting shrinkage cavity, it is loose, segregation the defects of.Further, since the use of ceramic crucible, master alloy
In inevitably introduce ceramics and inclusion defect.Drawbacks described above can produce bigger effect the preparation of superalloy powder.
Field trash in master alloy not can be removed in pulverizing process, shrinkage cavity, it is loose the defects of also will cause hollow powder and powder surface
Oxidation.
Vacuum electroslag remelting technology advantage in terms of removal element sulphur, P elements, foreign impurity and large-sized inclusions
Significantly, and make endogenous inclusion Dispersed precipitate.Meanwhile electroslag remelting has the characteristics that consecutive solidification, dense structure is conducive to tie up
Hold the technology stability of superalloy powder preparation process.
Vacuum consumable Technology For Remelting removal alloy in impurity element, control dense structure's degree and inhibit segregation, go unless
Metallic inclusion etc. advantage is significant.The pollution of aluminium alloy is avoided using water cooled copper mould.Moreover, vacuum consumable reflow process
In there is no clinker participation, therefore ingot casting surface is bright and clean, blocks without slag crust thermally conductive, and cooling velocity is bigger, dense structure Du Genggao,
It is very suitable for preparing the powder metallurgy high-temperature alloy master alloy of high-compactness.
Therefore, the present invention proposes a kind of preparation method of high cleanliness powder metallurgy high-temperature alloy master alloy.Basic ideas
To carry out sublimate processing to raw material first, it is therefore an objective to reduce the content of trace impurity；Sublimate melting is carried out again,
Including vacuum induction melting, vacuum electroslag remelting and vacuum consumable remelting, it is therefore an objective to prepare the master alloy of high cleanliness.
Summary of the invention
It is an object of that present invention to provide a kind of preparation methods of high cleanliness powder metallurgy high-temperature alloy master alloy, it is intended to mention
The degree of purity of high powder metallurgy high-temperature alloy master alloy reduces the content of trace impurity and non-metallic inclusion.
Powder metallurgy high-temperature alloy of the present invention, chemical composition ranges include that " GB/T 14992-2005 high temperature closes
The classification of gold and intermetallic compound high-temperature material and the trade mark " powder metallurgy high-temperature alloy and other non-standard boards in standard
Number powder metallurgy high-temperature alloy.Specific process step are as follows:
(1) purification of raw material: to several basic raw materials of powder metallurgy high-temperature alloy (Ni, Cr, Co, W, Mo, Nb,
Al, Ti) it is purified, using extraction, ion exchange, diaphragm electrodeposition, high-purity hydrogen reduction, zone refining technology, electron-beam smelting
Etc. technologies several trace impurities such as As, Sn, Pb, Sb, Bi, K, Ca very harmful in raw material are carried out it is targeted
Removal, the raw material purified；
(2) pickling, removal oxide on surface etc. raw material surface preparation: are carried out to the raw material after purification.Metal is former
Material is pre-processed in 5vol.% aqueous hydrochloric acid solution, removes oxide on surface, pretreatment time 30min；It then will be each
Kind raw material metal, which is placed in dehydrated alcohol, to be ultrasonically treated, and the processing time is 15min；
(3) vacuum induction melting: weighing various raw material in step (2) in proportion, is added according to certain charging sequence
Raw material are evacuated to 5 × 10-1Pa~5 × 10-3Pa carries out melting；It is poured into punching block after being completely melt, obtains vacuum electric
Slag remelting consutrode；Using high purity alumina crucible；
(4) vacuum electroslag remelting: solid-state start is used；Slag charge proportion is 10~30wt.%CaO, 10~30wt.%
Al2O3, 1~3wt.%TiO2, 5~10wt.%MgF2, 1~6wt.%CeO2, surplus CaF2.Slag charge carries out fritting processing, and machine
Tool crushes, and is then layered on crystalliser feet；It is put into the consutrode of step (3) preparation；After being evacuated to 1000~2000Pa, change
The slag starting the arc.Striking electric current is 800~1500A, and normal electric current of smelting is 2000~3000A, 35~45V of voltage.To resmelting ingot into
The polishing of row surface, scale removal, slag crust etc., and mouth of a river end and riser end are cut away, obtain vacuum electroslag remelting ingot；
(5) vacuum consumable remelting: using the vacuum electroslag remelting ingot that step (4) obtains as consutrode, using low-voltage,
High current technique carries out remelting, and melting voltage is 20~30V, and melting electric current is 4000~5000A.Molten drop rate be 6~8 drop/
S, and using water cooling with the type of cooling filling helium gas cooling and combining, wherein helium pressure is 300~500Pa.It obtains high-purity
Cleanliness powder metallurgy high-temperature alloy master alloy.
Further, step (3) vacuum induction melting, it is characterised in that: first will be with the lower element of O, N affinity
Ni, Cr, Co, W, Mo etc. add after C, Nb, Ti, Al, B, Zr wait melt melting down and C are added, refine 15~30min, the degree of superheat
It is 150~200 DEG C；Strong nitride and oxide forming elements Nb, Ti, Al is added, is heated to added material and is completely melt；It fills again
Argon gas is added easy scaling loss and volatile microelement B and Zr, is stirred simultaneously to 0.01~0.06MPa, until aluminium alloy
It is poured into punching block after being completely melt again.
Further, step (3) vacuum induction melting, it is characterised in that: use high purity alumina crucible, MgO
Content is less than 0.0010wt.%.
Further, step (4) solid-state start, it is characterised in that: the CaF for being 0.9:1~1.1:1 with mass ratio2
With TiO2Prepare striking agent；Contain MgF in slag system2And CeO2；Slag system raw material is matched and is uniformly mixed, then 1300
Melted between~1700 DEG C, 10~30min of time, it is ensured that liquid slag charge it is uniform；It pours into metal die and is cooled down；
It is sieved after mechanical crushing, obtains the pre-melted slag that granularity is 1~15mm；Pre-melted slag is using preceding in 600~800 DEG C of baking at least 8h.
Further, step (4) the striking agent and pre-melted slag, it is characterised in that: content of MgO is less than 0.0010wt.%.
Further, in the raw material of the purification trace impurity content are as follows: As < 0.0002%, Sn <
0.0001%, Pb < 0.0001%, Sb < 0.0001%, Bi < 0.0001%, K < 0.0005%, Ca < 0.0005%.
Further, As < 0.00005%, Sn < 0.00007%, Pb in the powder metallurgy high-temperature alloy master alloy <
0.00005%, Sb < 0.00003%, Bi < 0.00005%, K < 0.00001%, Ca < 0.00001%, S < 0.0003%, P <
0.0005%, the content of N < 0.0008%, O < 0.0006%, non-metallic inclusion is
<0.32mg/kg。
The present invention has the advantages that (1) uses extraction, ion exchange, diaphragm electrodeposition, high-purity hydrogen reduction, zone refining etc.
Technology can remove trace impurity K and Ca in six kinds of main raw material(s)s (Ni, Cr, Co, W, Mo, Nb)；(2) vacuum induction
Melting can accurately control alloying component, remove impurity element aspect in alloy, very low oxygen, nitrogen content be obtained, to reduce
The quantity of oxide, nitride；(3) relative to the electroslag remelting carried out under ordinary atmosphere, vacuum electroslag remelting can be tight
Lattice control oxygen content, nitrogen content；Using containing MgF2And CeO2Slag charge, wherein MgF2The fusing point that slag system can be reduced, facilitates
Slugging when solid-state start；CeO2With deoxidation；It can remove due to raw material and fire-clay crucible melting bring simultaneously
A non-metallic inclusion based on oxide；(4) vacuum consumable remelting can further remove impurity element O and N, reduce
The quantity of Reoxides field trash；And it further removes since raw material and fire-clay crucible melting bring are based on oxide
A non-metallic inclusion；Dense structure simultaneously.
Detailed description of the invention
Fig. 1 is process flow chart.
Specific embodiment
The preparation of embodiment 1:FGH4096 powder metallurgy high-temperature alloy master alloy
(1) raw material purification process: to several basic raw materials of powder metallurgy high-temperature alloy (Ni, Cr, Co, W, Mo,
Nb, Al, Ti) it is purified, it is molten using extraction, ion exchange, diaphragm electrodeposition, high-purity hydrogen reduction, zone refining technology, electron beam
The technologies such as refining carry out several trace impurities such as As, Sn, Pb, Sb, Bi, K, Ca very harmful in raw material targeted
Removal, the raw material purified；
(2) pickling, removal oxide on surface etc. raw material surface pretreatment process: are carried out to the raw material after purification；Gold
Belong to raw material to be pre-processed in 5vol.% aqueous hydrochloric acid solution, removes oxide on surface, pretreatment time 30min；Then
Various raw material metals are placed in dehydrated alcohol and are ultrasonically treated, the processing time is 15min.
(3) it vacuum induction melting process: is first put into the crucible of vacuum induction melting furnace and the lower member of O, N affinity
Plain Ni, Cr, Co, W, Mo, Fe；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 is to 0.02MPa, finally
Easy scaling loss and volatile microelement B and Zr is added, is stirred simultaneously, until aluminium alloy is poured into after being completely melt again
In punching block, high temperature alloy consutrode is obtained；Consutrode is machined, surface scale, riser are removed, completes electricity
The preparation of pole；
(4) vacuum electroslag remelting: solid-state start is used；Slag charge proportion is 20wt.%CaO, 20wt.%Al2O3, 3wt.%
TiO2, 6wt.%MgF2, 4wt.%CeO2, surplus CaF2.Slag charge carries out fritting processing, and being mechanically pulverized into granularity is 1~15mm
Particle, be then layered on crystalliser feet；It is put into the consutrode of step (3) preparation；After being evacuated to 1000Pa, slugging is risen
Arc.Striking electric current is 1000A, and normal electric current of smelting is 2000~3000A, 35~45V of voltage.Surface is carried out to resmelting ingot to beat
Mill, scale removal, slag crust etc., and mouth of a river end and riser end are cut away, obtain vacuum electroslag remelting ingot；
(5) vacuum consumable remelting process: using the vacuum electroslag remelting ingot of step (4) preparation as electrode, using low-voltage,
High current technique carry out remelting, melting voltage be 20~30V, melting electric current be 4000~5000A, molten drop rate be 6~8 drop/
S, and using water cooling with the type of cooling filling helium gas cooling and combining, wherein helium pressure is 300~500Pa.
As < 0.00005%, Sn in FGH4096 powder metallurgy high-temperature alloy master alloy by above-mentioned operation step <
0.00007%, Pb < 0.00005%, Sb < 0.00003%, Bi < 0.00005%, K < 0.00001%, Ca < 0.00001%, S <
0.0003%, P < 0.0005%, N < 0.0008%, O < 0.0006%, the content of non-metallic inclusion are less than 0.32mg/kg.
Embodiment 2:FGH4096 high temperature alloy master alloy sublimate melting
(1) raw material purification process: to several basic raw materials of powder metallurgy high-temperature alloy (Ni, Cr, Co, W, Mo,
Nb, Al, Ti) it is purified, it is molten using extraction, ion exchange, diaphragm electrodeposition, high-purity hydrogen reduction, zone refining technology, electron beam
The technologies such as refining carry out several trace impurities such as As, Sn, Pb, Sb, Bi, K, Ca very harmful in raw material targeted
Removal, the raw material purified；
(2) pickling, removal oxide on surface etc. raw material surface pretreatment process: are carried out to the raw material after purification；Gold
Belong to raw material to be pre-processed in 5vol.% aqueous hydrochloric acid solution, removes oxide on surface, pretreatment time 30min；Then
Various raw material metals are placed in dehydrated alcohol and are ultrasonically treated, the processing time is 15min.
(3) it vacuum induction melting process: is first put into the crucible of vacuum induction melting furnace and the lower member of O, N affinity
Plain Ni, Cr, Co, W, Mo, Fe；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 is to 0.05MPa, finally
Easy scaling loss and volatile microelement B and Zr is added, is stirred simultaneously, until aluminium alloy is poured into after being completely melt again
In punching block, high temperature alloy consutrode is obtained；Consutrode is machined, surface scale, riser are removed, completes electricity
The preparation of pole；
(4) vacuum electroslag remelting: solid-state start is used；Slag charge proportion is 20wt.%CaO, 20wt.%Al2O3, 2wt.%
TiO2, 6wt.%MgF2, 3wt.%CeO2, surplus CaF2.Slag charge carries out fritting processing, and being mechanically pulverized into granularity is 1~15mm
Particle, be then layered on crystalliser feet；It is put into the consutrode of step (3) preparation；After being evacuated to 1200Pa, slugging is risen
Arc.Striking electric current is 1000A, and normal electric current of smelting is 2000~3000A, 35~45V of voltage.Surface is carried out to resmelting ingot to beat
Mill, scale removal, slag crust etc., and mouth of a river end and riser end are cut away, obtain vacuum electroslag remelting ingot；
(5) vacuum consumable remelting process: using the vacuum electroslag remelting ingot of step (4) preparation as electrode, using low-voltage,
High current technique carry out remelting, melting voltage be 20~30V, melting electric current be 4000~5000A, molten drop rate be 6~8 drop/
S, and using water cooling with the type of cooling filling helium gas cooling and combining, wherein helium pressure is 300~500Pa.
As < 0.00005%, Sn in FGH4096 powder metallurgy high-temperature alloy master alloy by above-mentioned operation step <
0.00007%, Pb < 0.00005%, Sb < 0.00003%, Bi < 0.00005%, K < 0.00001%, Ca < 0.00001%, S <
0.0003%, P < 0.0005%, N < 0.0008%, O < 0.0006%, the content of non-metallic inclusion are 0.31mg/kg.
Embodiment 3:FGH4097 high temperature alloy master alloy sublimate melting
(1) raw material purification process: to several basic raw materials of powder metallurgy high-temperature alloy (Ni, Cr, Co, W, Mo,
Nb, Al, Ti) it is purified, it is molten using extraction, ion exchange, diaphragm electrodeposition, high-purity hydrogen reduction, zone refining technology, electron beam
The technologies such as refining carry out several trace impurities such as As, Sn, Pb, Sb, Bi, K, Ca very harmful in raw material targeted
Removal, the raw material purified；
(2) pickling, removal oxide on surface etc. raw material surface pretreatment process: are carried out to the raw material after purification；Gold
Belong to raw material to be pre-processed in 5vol.% aqueous hydrochloric acid solution, removes oxide on surface, pretreatment time 30min；Then
Various raw material metals are placed in dehydrated alcohol and are ultrasonically treated, the processing time is 15min.
(3) it vacuum induction melting process: is first put into the crucible of vacuum induction melting furnace and the lower member of O, N affinity
Plain Ni, Cr, Co, W, Mo, Fe；It is evacuated to 5 × 10-3Pa 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 is to 0.04MPa, finally
Easy scaling loss and volatile microelement B and Zr is added, is stirred simultaneously, until aluminium alloy is poured into after being completely melt again
In punching block, high temperature alloy consutrode is obtained；Consutrode is machined, surface scale, riser are removed, completes electricity
The preparation of pole；
(4) vacuum electroslag remelting: solid-state start is used；Slag charge proportion is 18wt.%CaO, 18wt.%Al2O3, 2wt.%
TiO2, 6wt.%MgF2, 3wt.%CeO2, surplus CaF2.Slag charge carries out fritting processing, and being mechanically pulverized into granularity is 1~15mm
Particle, be then layered on crystalliser feet；It is put into the consutrode of step (3) preparation；After being evacuated to 1500Pa, slugging is risen
Arc.Striking electric current is 1200A, and normal electric current of smelting is 2000~3000A, 35~45V of voltage.Surface is carried out to resmelting ingot to beat
Mill, scale removal, slag crust etc., and mouth of a river end and riser end are cut away, obtain vacuum electroslag remelting ingot；
(5) vacuum consumable remelting process: using the vacuum electroslag remelting ingot of step (4) preparation as electrode, using low-voltage,
High current technique carry out remelting, melting voltage be 20~30V, melting electric current be 4000~5000A, molten drop rate be 6~8 drop/
S, and using water cooling with the type of cooling filling helium gas cooling and combining, wherein helium pressure is 300~500Pa.
As < 0.00005%, Sn in FGH4097 powder metallurgy high-temperature alloy master alloy by above-mentioned operation step <
0.00007%, Pb < 0.00005%, Sb < 0.00003%, Bi < 0.00005%, K < 0.00001%, Ca < 0.00001%, S <
0.0003%, P < 0.0005%, N < 0.0008%, O < 0.0006%, the content of non-metallic inclusion are 0.25mg/kg.
Embodiment 4:FGH4097 high temperature alloy master alloy sublimate melting
(1) raw material purification process: to several basic raw materials of powder metallurgy high-temperature alloy (Ni, Cr, Co, W, Mo,
Nb, Al, Ti) it is purified, it is molten using extraction, ion exchange, diaphragm electrodeposition, high-purity hydrogen reduction, zone refining technology, electron beam
The technologies such as refining carry out several trace impurities such as As, Sn, Pb, Sb, Bi, K, Ca very harmful in raw material targeted
Removal, the raw material purified；
(2) pickling, removal oxide on surface etc. raw material surface pretreatment process: are carried out to the raw material after purification；Gold
Belong to raw material to be pre-processed in 5vol.% aqueous hydrochloric acid solution, removes oxide on surface, pretreatment time 30min；Then
Various raw material metals are placed in dehydrated alcohol and are ultrasonically treated, the processing time is 15min.
(3) it vacuum induction melting process: is first put into the crucible of vacuum induction melting furnace and the lower member of O, N affinity
Plain Ni, Cr, Co, W, Mo, Fe；It is evacuated to 5 × 10-3Pa 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 is to 0.05MPa, finally
Easy scaling loss and volatile microelement B and Zr is added, is stirred simultaneously, until aluminium alloy is poured into after being completely melt again
In punching block, high temperature alloy consutrode is obtained；Consutrode is machined, surface scale, riser are removed, completes electricity
The preparation of pole；
(4) vacuum electroslag remelting: solid-state start is used；Slag charge proportion is 18wt.%CaO, 18wt.%Al2O3, 2wt.%
TiO2, 5wt.%MgF2, 4wt.%CeO2, surplus CaF2.Slag charge carries out fritting processing, and being mechanically pulverized into granularity is 1~15mm
Particle, be then layered on crystalliser feet；It is put into the consutrode of step (3) preparation；After being evacuated to 1200Pa, slugging is risen
Arc.Striking electric current is 1300A, and normal electric current of smelting is 2000~3000A, 35~45V of voltage.Surface is carried out to resmelting ingot to beat
Mill, scale removal, slag crust etc., and mouth of a river end and riser end are cut away, obtain vacuum electroslag remelting ingot；
(5) vacuum consumable remelting process: using the vacuum electroslag remelting ingot of step (4) preparation as electrode, using low-voltage,
High current technique carry out remelting, melting voltage be 20~30V, melting electric current be 4000~5000A, molten drop rate be 6~8 drop/
S, and using water cooling with the type of cooling filling helium gas cooling and combining, wherein helium pressure is 300~500Pa.
As < 0.00005%, Sn in FGH4097 powder metallurgy high-temperature alloy master alloy by above-mentioned operation step <
0.00007%, Pb < 0.00005%, Sb < 0.00003%, Bi < 0.00005%, K < 0.00001%, Ca < 0.00001%, S <
0.0003%, P < 0.0005%, N < 0.0008%, O < 0.0006%, the content of non-metallic inclusion are 0.30mg/kg.
Claims (7)
1. a kind of preparation method of high cleanliness powder metallurgy high-temperature alloy master alloy, it is characterised in that the high temperature alloy includes
Powder metallurgy in " classification of GB/T 14992-2005 high temperature alloy and intermetallic compound high-temperature material and the trade mark " standard is high
Temperature alloy and other non-standard trade mark powder metallurgy high-temperature alloys, specific process step are as follows:
(1) purification of raw material: to several basic raw materials of Ni, Cr, Co, W, Mo, Nb, Al, Ti of powder metallurgy high-temperature alloy
It is purified, using extraction, ion exchange, diaphragm electrodeposition, high-purity hydrogen reduction, zone refining technology, electron-beam smelting technology pair
Several trace impurities of very harmful As, Sn, Pb, Sb, Bi, K, Ca are targetedly removed in raw material, are obtained
The raw material of purification；
(2) raw material surface preparation: pickling is carried out to the raw material after purification, removes oxide on surface；Raw material metal exists
It is pre-processed in 5vol.% aqueous hydrochloric acid solution, removes oxide on surface, pretreatment time 30min；Then by various metals
Raw material are placed in dehydrated alcohol and are ultrasonically treated, and the processing time is 15min；
(3) vacuum induction melting: weighing various raw material in step (2) in proportion, and former material is added according to certain charging sequence
Material, is evacuated to 5 × 10-1Pa~5 × 10-3Pa carries out melting；It is poured into punching block after being completely melt, obtains vacuum electroslag weight
Molten consutrode；Using high purity alumina crucible；
(4) vacuum electroslag remelting: solid-state start is used；Slag charge proportion is 10~30wt.%CaO, 10~30wt.%Al2O3, 1~
3wt.%TiO2, 5~10wt.%MgF2, 1~6wt.%CeO2, surplus CaF2；Slag charge carry out fritting processing, and be mechanically pulverized at
Granularity is the particle of 1~15mm, is then layered on crystalliser feet；It is put into the consutrode of step (3) preparation；It is evacuated to 1000
After~2000Pa, the slugging starting the arc；Striking electric current is 800~1500A, and normal electric current of smelting is 2000~3000A, voltage 35~
45V；Surface polishing, scale removal, slag crust are carried out to resmelting ingot, and cut away mouth of a river end and riser end, obtains vacuum electroslag weight
Melted ingot；
(5) vacuum consumable remelting: using the vacuum electroslag remelting ingot that step (4) obtains as consutrode, using low-voltage, big electricity
It flows technique and carries out remelting, melting voltage is 20~30V, and melting electric current is 4000~5000A；Molten drop rate is 6~8 drops/s, and
And using water cooling with the type of cooling filling helium gas cooling and combining, wherein helium pressure is 300~500Pa, obtains high cleanliness
Powder metallurgy high-temperature alloy master alloy.
2. a kind of preparation method of high cleanliness powder metallurgy high-temperature alloy master alloy as described in claim 1, it is characterised in that
The charging sequence of step (3) described vacuum induction melting are as follows: it will first enter O, N affinity lower element Ni, Cr, Co, W, Mo, then
C, Nb, Ti, Al, B, Zr is added, C is added after melt is melting down, refines 15~30min, the degree of superheat is 150~200 DEG C；It is added strong
Nitride and oxide forming elements Nb, Ti, Al are heated to added material and are completely melt；Again applying argon gas to 0.01~
0.06MPa is added easy scaling loss and volatile microelement B and Zr, is stirred simultaneously.
3. a kind of preparation method of high cleanliness powder metallurgy high-temperature alloy master alloy as described in claim 1, it is characterised in that
Content of MgO is less than 0.0010wt.% in step (3) described high purity alumina crucible.
4. a kind of preparation method of high cleanliness powder metallurgy high-temperature alloy master alloy as described in claim 1, it is characterised in that
Step (4) described solid-state start is: the CaF for being 0.9:1~1.1:1 with mass ratio2With TiO2Prepare striking agent；Contain in slag system
MgF2And CeO2；Slag system raw material is matched and is uniformly mixed, is then melted between 1300~1700 DEG C, the time 10
~30min, it is ensured that liquid slag charge it is uniform；It pours into metal die and is cooled down；Screening, obtaining granularity is the pre- of 1~15mm
Slag；Pre-melted slag is using preceding in 600~800 DEG C of baking at least 8h.
5. a kind of preparation method of high cleanliness powder metallurgy high-temperature alloy master alloy as described in claim 1, it is characterised in that
Content of MgO is less than 0.0010wt.% in step (4) the striking agent and pre-melted slag.
6. a kind of preparation method of high cleanliness powder metallurgy high-temperature alloy master alloy as described in claim 1, which is characterized in that
The content of trace impurity in the raw material of the purification are as follows: As < 0.0002%, Sn < 0.0001%, Pb < 0.0001%,
Sb < 0.0001%, Bi < 0.0001%, K < 0.0005%, Ca < 0.0005%.
7. a kind of preparation method of high cleanliness powder metallurgy high-temperature alloy master alloy as described in claim 1, which is characterized in that
As < 0.00005%, Sn < 0.00007%, Pb < 0.00005%, Sb in prepared powder metallurgy high-temperature alloy master alloy <
0.00003%, Bi < 0.00005%, K < 0.00001%, Ca < 0.00001%, S < 0.0003%, P < 0.0005%, N <
0.0008%, O < 0.0006%, the content of non-metallic inclusion are < 0.32mg/kg.
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Application publication date: 20190301 |