CN108913922A - The sublimate method of smelting of Ni-based directional solidification cylindrulite, single crystal super alloy master alloy - Google Patents
The sublimate method of smelting of Ni-based directional solidification cylindrulite, single crystal super alloy master alloy Download PDFInfo
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Abstract
The invention belongs to high temperature alloy preparation technical fields, and in particular to the sublimate method of smelting of a kind of Ni-based directional solidification cylindrulite, single crystal super alloy master alloy.Present invention comprehensively control in terms of raw material, crucible material, control of sublimate fusion process etc. three, fusion process reduces alloy refining temperature, realizing in turn reduces element loss and slows down crucible reaction, it can be achieved that alloying component more precise control and reduction impurity content.After the alloying phase simultaneously, deoxidization desulfuration agent is added, a step to the greatest extent reduces the impurity elements such as O, S in alloy.The present invention can be achieved O, N, S impurity element overall control in Ni-based directional solidification cylindrulite, single crystal super alloy master alloy within 5ppm, the trace impurities overall control such as As, Bi, Pb, Sn, Sb simultaneously greatly improves the degree of purity of Ni-based directional solidification cylindrulite, single crystal super alloy within 5ppm.
Description
Technical field
The invention belongs to high temperature alloy preparation technical fields, and in particular to a kind of Ni-based directional solidification cylindrulite, monocrystalline high temperature
The sublimate method of smelting of alloy master alloy.
Background technique
With the continuous development of aero-engine and gas turbine industry, the usage amount of high temperature alloy is more and more, it is desirable that
Intake air temperature before turbine is continuously improved, to increase thrust, improve efficiency, reduce oil consumption, this is just to high temperature alloy and its technique
More stringent requirements are proposed.Directional solidification cylindrulite, single crystal super alloy are compared to common equiax crystal high temperature alloy, solely because of itself
Special chemical component and structural property, there is it substantially using temperature, service life, structure stability, comprehensive mechanical property
Degree improves.Alloying level is very high in design for directional solidification cylindrulite, single crystal super alloy, such as W, Mo, Ta, Hf, Re compare greatly
The additional proportion of weight refractory metal elements is continuously improved, this allows for being difficult to control pernicious gas and impurity in its fusion process
The use that the field trash that the content of element, these pernicious gases and impurity element are formed can seriously increase rejection rate, reduce material
Service life.
How to improve Ni-based directional solidification cylindrulite, single crystal super alloy degree of purity, further play the application of the material
Potentiality have become an important topic for study.The big portion of patent in terms of published high temperature alloy sublimate smelting technology
It point is all made of 1600 DEG C or more of high temperature refinery, as used 1614 DEG C~1624 DEG C in Publication No. CN106319255A patent
Superhigh temperature refining, Publication No. CN1360071A patent high temperature refining temperature be 1650 DEG C, Publication No. CN1552928A
Patent high temperature refining temperature is 1600 DEG C~1650 DEG C, and high temperature refinery is to deoxidation, denitrogenation and the volatile impurity of other low melting points
The removal of element has certain effect, but there is also following disadvantages for high temperature refinery:(1) aggravate crucible reaction:At a higher temperature
Aluminium alloy reacts more violent with inner surface of crucible refractory material, and MgO, Al are contained in common crucible2O3、SiO2、ZrO、Fe2O3Deng
Compound, aggravation above-mentioned material and [C] in aluminium alloy react under high temperature high vacuum condition, cause crucible material to aluminium alloy
Pollution;The erosion degree of crucible material is higher simultaneously, reduces the service life of crucible.(2) under high temperature high vacuum condition, Cr,
The higher alloying element volatilization of the saturated vapour pressures such as Al is more serious, in turn results in a large amount of losses of such alloying element.
It is also reported in published patent molten using the crucible materials such as calcium oxide, yttrium oxide progress high temperature alloy sublimate
Refining, as crucible material is calcium oxide, crucible in Publication No. CN103498063A patent in Publication No. CN1360071A patent
Material is yttrium oxide.Although the crucible of these materials can take off O, de- S to a certain extent, because of it there are higher cost, be not easy
The problems such as preservation and be difficult to realize industrialization promotion.
Therefore, more effectively control Ni-based directional solidification cylindrulite, single crystal super alloy degree of purity need to also from raw material degree of purity,
Crucible material, fusion process control etc. comprehensively consider.
Summary of the invention
It is an object of the invention to be directed to Ni-based directional solidification cylindrulite, this kind of high value high temperature alloy of monocrystalline to O, N, S etc.
Pernicious gas and impurity element are more sensitive, provide a kind of Ni-based directional solidification cylindrulite, single crystal super alloy master alloy it is pure
Change method of smelting.This method is controlled from raw material degree of purity, crucible material, the control of sublimate fusion process etc., can
Realize by Ni-based orientation, in single crystal super alloy O, N, S impurity element overall control within 5ppm, while As, Bi, Pb, Sn,
The trace impurities controllable amount systems such as Sb greatly improve Ni-based orientation, single crystal super alloy degree of purity within 5ppm.
To realize the above-mentioned technical purpose, the following technical solution is employed by the present invention:
The sublimate method of smelting of Ni-based directional solidification cylindrulite, single crystal super alloy master alloy selects degree of purity higher
Raw material;The high purity aluminium oxide or magnesia crucible of better heat stability, 92% or more purity are selected simultaneously;According to the following steps into
Row:
(1) it charges:Loading sequence from the bottom to top, is followed successively by crucible:Whole Co, Ni total amounts 20~30%, account for alloy
C, whole Cr, whole Mo, whole W, whole Ta, whole Re and the residue Ni of weight ratio 0.01%~0.03%;In feed compartment
It is packed into the raw materials such as residue C, Al, Ti, whole Hf, NiB, Zr;Deoxidization desulfuration is added by feed compartment again after feeding in the alloying phase
Agent;
The loading sequence is not limited to a certain trade mark alloy, as that, without above-mentioned a certain or certain elements, can add in alloy
The raw materials process is removed when material;
(2) melting stage:Carry out melting using vaccum sensitive stove send power to be warming up to paragraph by paragraph as vacuum degree≤1.33Pa
Furnace charge is melting down, melting down subsequent temperature of continuing rising;
(3) refining period:When temperature reaches 140 DEG C~180 DEG C of aluminium alloy liquidus temperature or more, start to refine, when refining
Between depending on vacuum induction heat size, 250Kg vacuum drying oven refining time be 10min~40min;
(4) the alloying phase:After refining period, cooling freezing processing to the temperature that has a power failure reaches aluminium alloy liquidus temperature or more
At 20 DEG C~60 DEG C, it is melting down that raw materials, the high-power stirring such as residue C, Al, Ti, whole Hf, NiB, Zr are added by feed compartment;To temperature
When degree reaches 100 DEG C~140 DEG C of aluminium alloy liquidus temperature or more, start to refine;Refining time depending on vacuum induction heat size,
250Kg vacuum drying oven refining time is 10min~20min;
(5) the deoxidization desulfuration phase:After the alloying phase, have a power failure cooling freezing processing, during which applying argon gas 5kPa~30kPa;
When temperature reaches 20 DEG C~60 DEG C of aluminium alloy liquidus temperature or more, deoxidization desulfuration agent is added by feed compartment, high-power stirring is molten
Clearly;When temperature reaches 60 DEG C~100 DEG C of aluminium alloy liquidus temperature or more, start to refine;Refining time regards vacuum induction heat size
Depending on amount, 250Kg vacuum drying oven refining time is 5min~15min;
(6) casting cycle:After deoxidization desulfuration, have a power failure cooling, while being evacuated to≤1.33Pa, high-power stirring, when
When temperature reaches 100 DEG C~120 DEG C of aluminium alloy liquidus temperature or more, it is poured.
Wherein, the higher raw material of degree of purity are respectively:The nickel of Ni9999, the crome metal of GHCr-1, GHCr-2, Co9998
Metallic cobalt, the metal tantalum of GDT-1, GDT-2, GDT-3, the hafnium sponge of HHf-01, the rhenium metal of Re-04, Al99.99 and higher
The remelting of trade mark refined aluminium ingot, 0AGrade titanium sponge.
In step (5), deoxidization desulfuration agent is Y and nickel calcium alloy, the additional amount of Y be weight alloy ratio 0.02%~
0.1%, the additional amount of nickel calcium alloy is the 0.5%~1.0% of weight alloy ratio, and calcium content is 5%~30% in nickel calcium alloy.
Due to the adoption of the above technical scheme, compared with prior art, the present invention has at least following beneficial effect:
(1) present invention selects the high purity aluminium oxide or magnesia crucible of better heat stability, 92% or more purity, can reduce
Bring the impurity in aluminium alloy into because of crucible reaction.
(2) impurity in high temperature alloy largely derives from production raw material, and the present invention is directed to Ni-based directional solidification column
Brilliant, single crystal super alloy master alloy, proposition are selected high-purity raw material, are controlled from source impurity element, can be effective
The Ni-based orientation of reduction, the impurity content in single crystal super alloy master alloy, improve alloy degree of purity.
(3) sublimate smelting technology of the present invention reduces the refining temperature of alloy, thereby reduces alloy in fusion process
Liquid is reacted with crucible refractory material, secondary pollution caused by further decreasing because of crucible reaction;Meanwhile reducing saturated vapor
Loss of the higher alloying element in fusion process is pressed, element recovery rate is improved.
(4) sublimate smelting technology of the present invention proposes a kind of novel deoxidization desulfuration agent and deoxidization desulfuration technique, can have
Effect reduces the impurity contents such as O, S in alloy.
(5) Ni-based directional solidification cylindrulite, the single crystal super alloy master alloy of sublimate smelting technology production of the present invention are harmful
Gas and impurity content are extremely low, can improve by a relatively large margin Ni-based directional solidification cylindrulite, single crystal super alloy blade yield rate and
Service life.Can be achieved by O, N, S impurity element overall control in Ni-based directional solidification cylindrulite, single crystal super alloy 5ppm with
It is interior, while the trace impurities controllable amount system such as As, Bi, Pb, Sn, Sb is within 5ppm.
(6) sublimate smelting technology process of the present invention is simple, easily operated, it can be achieved that industrialized production and popularization.
Specific embodiment
Below with reference to embodiment, the present invention is further explained.In the following detailed description, it is only retouched by way of explanation
Certain exemplary embodiments of the invention are stated.Undoubtedly, those skilled in the art will recognize, without departing from
In the case where the spirit and scope of the present invention, the described embodiments may be modified in various different ways.Therefore,
Description is regarded as illustrative in nature, and is not intended to limit the scope of the claims.
It is pure that embodiment 1,2 selects 250Kg vacuum induction furnace apparatus to carry out Ni-based directional solidification cylindrulite, single crystal super alloy
Purify melting.
Embodiment 1:
The Ni-based directional solidification cylindrulite high temperature alloy of DZ125 is produced using sublimate smelting technology of the present invention, through looking into《Middle Air China
Empty Materials Handbook》The aluminium alloy liquidus temperature is 1377 DEG C.The alloy composition (mass fraction) is:0.09%C, 8.9%
Cr, 10%Co, 7%W, 2%Mo, 5.1%Al, 0.95%Ti, 3.8%Ta, 1.5%Hf, 0.015%B, 0.04%Zr, surplus
For Ni.
The present embodiment specific implementation step is as follows:
1, the selection of high-purity raw material:The nickel of Ni9999, the crome metal of GHCr-1, GHCr-2, the metallic cobalt of Co9998,
The metal tantalum of GDT-1, GDT-2, GDT-3, the hafnium sponge of HHf-01, the remelting refined aluminium ingot of Al99.99 and the higher trade mark, 0A grades
Titanium sponge, C, W, Mo, Zr etc. choose HB/Z131 and provide that the higher ranked trade mark, B are chosen among the self-produced high purity nickel boron of company
Alloy;
2, crucible is selected:Selecting purity is 95% high-purity magnesium oxide crucible;
3, method of smelting:
(1) it charges:Loading sequence from the bottom to top, is followed successively by crucible:Whole Co, Ni total amounts 20~30%, account for alloy
C, whole Cr, whole Mo, whole W, whole Ta and the residue Ni of weight ratio 0.01~0.03%;It is packed into feed compartment remaining
C, deoxidization desulfuration agent is added by feed compartment again after the charging of alloying phase in the raw materials such as Al, Ti, whole Hf, NiB, Zr;
(2) melting stage:As vacuum degree≤1.33Pa, power is sent to be warming up to furnace charge paragraph by paragraph melting down, it is melting down high-power subsequent
Temperature of continuing rising;
(3) refining period:When temperature reaches 1517 DEG C~1557 DEG C, start to refine, refining time is 10min~40min;
(4) the alloying phase:After refining period, when cooling freezing processing to the temperature that has a power failure reaches 1397 DEG C~1437 DEG C,
It is melting down that raw materials, the high-power stirring such as residue C, Al, Ti, whole Hf, NiB, Zr are added by feed compartment;To temperature reach 1477 DEG C~
At 1517 DEG C, start to refine, refining time is 10min~20min;
(5) the deoxidization desulfuration phase:After the alloying phase, have a power failure cooling freezing processing, during which applying argon gas 5kPa~30kPa;
When temperature reaches 1397 DEG C~1437 DEG C, deoxidization desulfuration agent is added by feed compartment, high-power stirring is melting down;Reach to temperature
At 1437 DEG C~1477 DEG C, start to refine, refining time is 5min~15min;
(6) casting cycle:After deoxidization desulfuration, have a power failure cooling, while being evacuated to≤1.33Pa, high-power stirring, when
When temperature reaches 1477 DEG C~1497 DEG C of aluminium alloy liquidus temperature or more, it is poured.
Using Ni-based directional solidification cylindrulite high temperature alloy master alloy O, N, S content pole the DZ125 of above-mentioned process melting
It is low, while the trace impurities controllable amount system such as As, Bi, Pb, Sn, Sb is within 5ppm.Specifically as shown in table 1, table 2.
1 O, N, S content (ppm) of table
Element | O | N | S | It amounts to |
Content | 1 | 2 | 1.5 | 4.5 |
2 As, Bi, Pb, Sn, Sb content (ppm) of table
Element | As | Bi | Pb | Sn | Sb | It amounts to |
Content | 1.6 | 0.05 | 0.3 | 2.1 | 0.15 | 4 |
Embodiment 2:
Certain trade mark second generation nickel-base high-temperature single crystal alloy, the aluminium alloy phase line are produced using sublimate smelting technology of the present invention
Temperature is 1385 DEG C.The alloy composition (mass fraction) is:0.06%C, 7.0%Cr, 8.0%Co, 5.0%W, 2.0%
Mo, 6.2%Al, 7.0%Ta, 3.0%Re, 0.20%Hf, 0.004%B, surplus Ni.
The present embodiment specific implementation step is as follows:
1, the selection of high-purity raw material:The nickel of Ni9999, the crome metal of GHCr-1, GHCr-2, the metallic cobalt of Co9998,
The metal tantalum of GDT-1, GDT-2, GDT-3, the hafnium sponge of HHf-01, Re-04 rhenium metal, the remelting of Al99.99 and the higher trade mark
With refined aluminium ingot, C, W, Mo etc. choose HB/Z131 and provide that the higher ranked trade mark, B are chosen among the self-produced high purity nickel boron of company
Alloy.
2, crucible is selected:Selecting purity is 96% high purity aluminium oxide crucible.
3, method of smelting:
(1) it charges:Loading sequence from the bottom to top, is followed successively by crucible:Whole Co, Ni total amounts 20~30%, account for orientation,
The C of monocrystal nickel-base high-temperature alloy weight ratio 0.01%~0.03%, whole Cr, whole Mo, whole W, whole Ta, whole Re and surplus
Remaining Ni;It is packed into the raw materials such as residue C, Al, whole Hf, NiB in feed compartment, is added again by feed compartment after the charging of alloying phase
Deoxidization desulfuration agent;
(2) melting stage:As vacuum degree≤1.33Pa, power is sent to be warming up to furnace charge paragraph by paragraph melting down, it is melting down high-power subsequent
Temperature of continuing rising;
(3) refining period:When temperature reaches 1525 DEG C~1565 DEG C, start to refine, refining time is 10min~40min;
(4) the alloying phase:After refining period, when cooling freezing processing to the temperature that has a power failure reaches 1405 DEG C~1445 DEG C,
It is melting down that raw materials, the high-power stirring such as residue C, Al, whole Hf, NiB are added by feed compartment;Reach 1485 DEG C~1525 DEG C to temperature
When, start to refine, refining time is 10min~20min;
(5) the deoxidization desulfuration phase:After the alloying phase, have a power failure cooling freezing processing, during which applying argon gas 5kPa~30kPa;
When temperature reaches 1405 DEG C~1445 DEG C, deoxidization desulfuration agent is added by feed compartment, high-power stirring is melting down;Reach to temperature
At 1445 DEG C~1485 DEG C, start to refine, refining time is 5min~15min;
(6) casting cycle:After deoxidization desulfuration, have a power failure cooling, while being evacuated to≤1.33Pa, high-power stirring, when
When temperature reaches 1485 DEG C~1505 DEG C of aluminium alloy liquidus temperature or more, it is poured.
It is extremely low using certain trade mark the second generation single crystal superalloy master alloy O, N, S content of above-mentioned process melting, together
When the trace impurities controllable amount system such as As, Bi, Pb, Sn, Sb within 5ppm.Specifically as shown in table 3, table 4.
3 O, N, S content (ppm) of table
Element | O | N | S | It amounts to |
Content | 1 | 1 | 0.5 | 2.5 |
4 As, Bi, Pb, Sn, Sb content (ppm) of table
Element | As | Bi | Pb | Sn | Sb | It amounts to |
Content | 1.4 | 0.05 | 0.1 | 1.6 | 0.1 | 3.25 |
The foregoing is merely the schematical specific embodiment of the present invention, the range being not intended to limit the invention.It is any
Those skilled in the art, made equivalent changes and modifications under the premise of not departing from design and the principle of the present invention,
It should belong to the scope of protection of the invention.
Claims (4)
1. the sublimate method of smelting of Ni-based directional solidification cylindrulite, single crystal super alloy master alloy, it is characterised in that:It selects pure
It spends higher raw material while selecting high purity aluminium oxide or magnesia crucible;It carries out according to the following steps:
(1) it charges:Loading sequence from the bottom to top, is followed successively by crucible:Whole Co, Ni total amounts 20~30%, account for weight alloy
C, whole Cr, whole Mo, whole W, whole Ta, whole Re and residue Ni than 0.01%~0.03%;It is packed into feed compartment
The raw materials such as remaining C, Al, Ti, whole Hf, NiB, Zr;Deoxidization desulfuration agent is added by feed compartment again after feeding in the alloying phase;
(2) melting stage:Carry out melting using vaccum sensitive stove send power to be warming up to furnace charge paragraph by paragraph as vacuum degree≤1.33Pa
It is melting down, melting down subsequent temperature of continuing rising;
(3) refining period:When temperature reaches 140 DEG C~180 DEG C of aluminium alloy liquidus temperature or more, start to refine;
(4) the alloying phase:After refining period, cooling freezing processing to the temperature that has a power failure reaches 20 DEG C of aluminium alloy liquidus temperature or more
At~60 DEG C, it is melting down that raw materials, the high-power stirring such as residue C, Al, Ti, whole Hf, NiB, Zr are added by feed compartment;It is reached to temperature
More than to aluminium alloy liquidus temperature at 100 DEG C~140 DEG C, start to refine;
(5) the deoxidization desulfuration phase:After the alloying phase, have a power failure cooling freezing processing, during which applying argon gas 5kPa~30kPa;Work as temperature
When degree reaches 20 DEG C~60 DEG C of aluminium alloy liquidus temperature or more, deoxidization desulfuration agent is added by feed compartment, high-power stirring is melting down;To
When temperature reaches 60 DEG C~100 DEG C of aluminium alloy liquidus temperature or more, start to refine;
(6) casting cycle:After deoxidization desulfuration, have a power failure cooling, while being evacuated to≤1.33Pa, and temperature is worked as in high-power stirring
When reaching 100 DEG C~120 DEG C of aluminium alloy liquidus temperature or more, it is poured.
2. the sublimate method of smelting of Ni-based directional solidification cylindrulite as described in claim 1, single crystal super alloy master alloy,
It is characterized in that, the higher raw material of degree of purity are respectively:The nickel of Ni9999, the crome metal of GHCr-1, GHCr-2, the gold of Co9998
Belong to cobalt, the metal tantalum of GDT-1, GDT-2, GDT-3, the hafnium sponge of HHf-01, the rhenium metal of Re-04, Al99.99 and the higher trade mark
Remelting refined aluminium ingot, 0AGrade titanium sponge.
3. the sublimate method of smelting of Ni-based directional solidification cylindrulite as described in claim 1, single crystal super alloy master alloy,
It is characterized in that:Crucible is the aluminium oxide or magnesia crucible of 92% or more purity.
4. the sublimate method of smelting of Ni-based directional solidification cylindrulite as described in claim 1, single crystal super alloy master alloy,
It is characterized in that:In step (5), deoxidization desulfuration agent is Y and nickel calcium alloy, the additional amount of Y be weight alloy ratio 0.02%~
0.1%, the additional amount of nickel calcium alloy is the 0.5%~1.0% of weight alloy ratio, and calcium content is 5%~30% in nickel calcium alloy.
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CN117363960A (en) * | 2023-12-08 | 2024-01-09 | 成都先进金属材料产业技术研究院股份有限公司 | Low-carbon aluminum-free high-niobium-iron-based superalloy and preparation method thereof |
CN117363960B (en) * | 2023-12-08 | 2024-03-08 | 成都先进金属材料产业技术研究院股份有限公司 | Low-carbon aluminum-free high-niobium-iron-based superalloy and preparation method thereof |
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CN117660810B (en) * | 2024-01-31 | 2024-04-16 | 四川航大新材料有限公司 | High-purity high-temperature master alloy for variable-cycle gas engine turbine blade and preparation method and application thereof |
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