CN105364001B - Liquid metal cooling directional solidification blade surface detinning method - Google Patents

Liquid metal cooling directional solidification blade surface detinning method Download PDF

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CN105364001B
CN105364001B CN201510665070.3A CN201510665070A CN105364001B CN 105364001 B CN105364001 B CN 105364001B CN 201510665070 A CN201510665070 A CN 201510665070A CN 105364001 B CN105364001 B CN 105364001B
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blade
formwork
coating
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temperature
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CN105364001A (en
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毛萍莉
姜卫国
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Weihai KaiHong New Material Co.,Ltd.
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Shenyang University of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D29/00Removing castings from moulds, not restricted to casting processes covered by a single main group; Removing cores; Handling ingots
    • B22D29/001Removing cores
    • B22D29/002Removing cores by leaching, washing or dissolving
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22CFOUNDRY MOULDING
    • B22C9/00Moulds or cores; Moulding processes
    • B22C9/02Sand moulds or like moulds for shaped castings
    • B22C9/04Use of lost patterns
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D31/00Cutting-off surplus material, e.g. gates; Cleaning and working on castings
    • B22D31/002Cleaning, working on castings

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Molds, Cores, And Manufacturing Methods Thereof (AREA)

Abstract

Liquid metal cooling directional solidification blade surface detinning method, process route is as follows:(1), blade formwork is prepared using precision casting process, using LIQUID Sn cooling directional solidification technique prepare directional columnargrain or single crystal blade;(2), blade formwork is cleared up;(3), the blade after clear shell is put into high pressure depoling kettle, inject alkali lye, carry out removing tin under certain temperature and pressure;(4), to being neutralized and being cleaned using acid solution except the blade surface after tin, finally dry, obtain the blade of surface Wuxi.It is based on the tin that high temperature alloy does not generate the principle for the salt for being dissolvable in water water with alkaline reaction, tin and alkaline reaction and removes blade surface, reaches that blade surface goes the purpose of tin.

Description

Liquid metal cooling directional solidification blade surface detinning method
Technical field
The invention belongs to the preparation technology of technical field of high temperature alloy, more particularly to high temperature alloy directional solidification blade.
Background technology
At present, the Directional Solidification of Nickel-Based Superalloy technology of industrial comparative maturity application mainly uses high speed freezing method (High Rate Solidification, HRS) and liquid metal cool down (Liquid Metal Cooling, LMC) method. Traditional HRS methods improve thermograde by way of mobile shell mould, and thermograde is generally 20-40 DEG C/cm.Concrete mode For formwork is placed in water-cooled chassis, and hot-zone is isolated with radiation baffle, after crystal growth starts, shell mould is with default speed Degree is removed by radiation baffle from hot-zone.And the distinguishing feature of LMC technologies is, by the use of liquid metal as cooling medium, to pass through heat Conduction substitutes common heat radiation mode to accelerate to have solidified part(That is solid phase area)Heat transfer, make solidification processing temperature ladder Degree is significantly improved.Relative to HRS technologies, LMC technologies are by the use of liquid metal as cooling medium, and solidification processing temperature gradient is notable Improve, thermograde is generally 80-100 DEG C/cm, be so likely to be obtained the less single crystal organization of defect, improve the mechanics of alloy Performance and environmental performance.In addition, LMC advantage is also manifested by and expands the control of freezing rate and select scope, by the improvement of technique not The tissue and performance of alloy can be only controlled, and save setting time, simplify production process.The liquid of LMC techniques Cooling metal is typically chosen metal Sn, Sn cooling effect more preferably, can obtain higher thermograde.This kind of cooling medium exists Foreign countries are widely used in the industrial production of blade, but there is also problem for this kind of medium, that is, in blade process of setting, Due to there is certain slight void between the alloy after formwork and solidification, liquid metal tin is in static pressure and the work of capillary force Can be by penetrating into the space under, and then the surface of the part of blade solidification lower end can be bonded in.Usual this layer of tin is very thin And with blade surface adhesion-tight, remove it is extremely difficult.Therefore, how to remove directional solidification blade surface to glue tin is liquid metal Cooling directional freeze method prepares the problem of blade must be solved.
The content of the invention
Goal of the invention:The present invention provides a kind of liquid metal cooling directional solidification blade surface detinning method, the purpose is to Solve the problems of conventional, the surface quality of raising blade.
Technical scheme:
Liquid metal cooling directional solidification blade surface detinning method, it is characterised in that:Process route is as follows:(1), use Precision casting process prepares blade formwork, and directional columnargrain or single crystal blade are prepared using LIQUID Sn cooling directional solidification technique; (2), blade formwork is cleared up;(3), the blade after clear shell is put into high pressure depoling kettle, alkali lye is injected, in certain temperature Carried out with pressure except tin;(4), to being neutralized and being cleaned using acid solution except the blade surface after tin, finally dry, obtain The blade of surface Wuxi.
The preparation technology of blade formwork is as follows:Investment precoat is prepared using 320-400 mesh schmigel with silicon sol solution, Powder liquor ratio(Mass ratio)For 3-3.5:1, it is dried at ambient temperature after the first coating, drying time 4-8 hour;The Stucco after two coatings, stucco material is 60-80 mesh emergies, drying time 4-8 hour;Sanding material is after third layer coating 32-60 mesh emergies, drying time is 4-8 hours;Sanding material is 24-32 mesh emergies after 4th coating, when drying Between be 4-8 hours;Five-layer 7 is that sanding material is 16-24 mesh emergies after coating, and drying time is 4-8 hours, most Slurry seal layer uses investment precoat afterwards, and drying time is 2-8 hours;
Wax-pattern is removed using steaming process, vapor (steam) temperature is 150 DEG C -170 DEG C, and the time is 10-20 minutes;
Formwork is put into roaster after formwork dewaxing and is calcined, sintering temperature is 850-1200 DEG C, soaking time is 2-6 hours, it is furnace-cooled to room temperature and is cleaned;
Formwork is placed in orientation stove, upper area is preheating to 1450-1550 DEG C, and lower area is preheating to 1480-1550 DEG C, will close Gold melts in smelting furnace, starts crystal-pulling after being poured, and pulling rate is 3-12 mm/mins, and drawing finishes rear furnace cooling, Then take out clear shell.
Blade after clear shell is put into high pressure depoling kettle, removed using the NaOH or KOH aqueous solution, alkali concn is 25- 40%(Mass ratio), temperature is 120 DEG C -280 DEG C, and pressure is 0.3-1MPa, removes time 2-50 hour;Remaining alkali lye on blade Neutralized using aqueous hydrochloric acid solution, concentration of hydrochloric acid solution is 1-10%;Finally blade is cleaned using water, drying.
The material of directional solidification blade is orientation or monocrystal nickel-base high-temperature alloy.
Advantage and effect:The present invention provides a kind of liquid metal cooling directional solidification blade surface detinning method, specifically Chemical equation is as follows:Sn+2OH-+H2O=2H2↑+SnO3 2-.It is based on high temperature alloy not with alkaline reaction, tin and alkali lye The tin for reacting the principle for generating the salt for being dissolvable in water water and removing blade surface, reaches that blade surface goes the purpose of tin.
Embodiment:
The present invention will be further described below:
Embodiment 1
Blade formwork is prepared using precision casting process, investment precoat is matched somebody with somebody using schmigel (320 mesh) with silicon sol solution System, powder liquor ratio is 3.5:1, it is dried at ambient temperature after the first coating, 8 hours drying times;Second coating Stucco afterwards, stucco material is 80 mesh emergies, 8 hours drying times;Sanding material is 60 mesh emergies after third layer coating, is done The dry time is 8 hours;Sanding material is 32 mesh emergies after 4th coating, and drying time is 8 hours;Five-layer 7 It is 24 mesh emergies for sanding material after coating, drying time is 8 hours, last slurry seal layer uses investment precoat, drying time For 8 hours;Wax-pattern is removed using steaming process, vapor (steam) temperature is 170 DEG C, and the time is 20 minutes;Formwork is put into after formwork dewaxing It is calcined in roaster, sintering temperature is 1200 DEG C, and soaking time is 6 hours, is furnace-cooled to room temperature and is cleaned;By formwork It is placed in orientation stove, upper area is preheating to 1550 DEG C, and lower area is preheating to 1550 DEG C, and alloy is melted and poured into a mould in smelting furnace, Alloy is orientation or monocrystal nickel-base high-temperature alloy, starts directional solidification growth after being poured, and pulling rate is 12 mm/mins, is drawn System finishes rear furnace cooling, then takes out clear shell.Blade after clear shell is put into high pressure depoling kettle, using the KOH aqueous solution Removing, alkali concn is 40%(Mass ratio), temperature is 280 DEG C, and pressure is 1MPa, removes 5 hours time;Remaining alkali lye on blade Neutralized using aqueous hydrochloric acid solution, concentration of hydrochloric acid solution is 5%;Finally blade is cleaned using water, drying.Sampled section Detection, blade surface tin layers are removed completely.
Embodiment 2
Blade formwork is prepared using precision casting process, investment precoat is matched somebody with somebody using schmigel (320 mesh) with silicon sol solution System, powder liquor ratio is 3.5:1, it is dried at ambient temperature after the first coating, 4 hours drying times;Second coating Stucco afterwards, stucco material is 60 mesh emergies, 4 hours drying times;Sanding material is 60 mesh emergies after third layer coating, is done The dry time is 4 hours;Sanding material is 32 mesh emergies after 4th coating, and drying time is 4 hours;Five-layer 7 It is 24 mesh emergies for sanding material after coating, drying time is 4 hours, last slurry seal layer uses investment precoat, drying time For 2 hours;Wax-pattern is removed using steaming process, vapor (steam) temperature is 170 DEG C, and the time is 10 minutes;Formwork is put into after formwork dewaxing It is calcined in roaster, sintering temperature is 850 DEG C, and soaking time is 6 hours, is furnace-cooled to room temperature and is cleaned;By formwork It is placed in orientation stove, upper area is preheating to 1500 DEG C, and lower area is preheating to 1480 DEG C, and alloy is melted and poured into a mould in smelting furnace, Alloy is orientation or monocrystal nickel-base high-temperature alloy, starts directional solidification growth after being poured, and pulling rate is 3 mm/mins, is drawn Rear furnace cooling is finished, clear shell is then taken out.Blade after clear shell is put into high pressure depoling kettle, taken off using the KOH aqueous solution Remove, alkali concn is 25%(Mass ratio), temperature is 150 DEG C, and pressure is 0.3MPa, removes 40 hours time;Remaining alkali lye on blade Neutralized using aqueous hydrochloric acid solution, concentration of hydrochloric acid solution is 4%;Finally blade is cleaned using water, drying.Sampled section Detection, blade surface tin layers are removed completely.
Embodiment 3
Blade formwork is prepared using precision casting process, investment precoat is matched somebody with somebody using schmigel (320 mesh) with silicon sol solution System, powder liquor ratio is 3:1, it is dried at ambient temperature after the first coating, 8 hours drying times;After second coating Stucco, stucco material is 80 mesh emergies, 4 hours drying times;Sanding material is 60 mesh emergies after third layer coating, is dried Time is 4 hours;Sanding material is 24 mesh emergies after 4th coating, and drying time is 4 hours;Five-layer 7 is Sanding material is 16 mesh emergies after coating, and drying time is 4 hours, and last slurry seal layer uses investment precoat, and drying time is 6 hours;Wax-pattern is removed using steaming process, vapor (steam) temperature is 150 DEG C, and the time is 20 minutes;Formwork is put into roasting after formwork dewaxing Burn in stove and be calcined, sintering temperature is 980 DEG C, and soaking time is 4 hours, is furnace-cooled to room temperature and is cleaned;Formwork is put Put in orientation stove, upper area is preheating to 1550 DEG C, and lower area is preheating to 1480 DEG C, and alloy is melted and poured into a mould in smelting furnace, close Gold is orientation or monocrystal nickel-base high-temperature alloy, starts directional solidification growth after being poured, and pulling rate is 6 mm/mins, has been drawn Furnace cooling after finishing, then takes out clear shell.Blade after clear shell is put into high pressure depoling kettle, taken off using the NaOH aqueous solution Remove, alkali concn is 38%(Mass ratio), temperature is 190 DEG C, and pressure is 0.5MPa, removes 30 hours time;Remaining alkali lye on blade Neutralized using aqueous hydrochloric acid solution, concentration of hydrochloric acid solution is 1%;Finally blade is cleaned using water, drying.Sampled section Detection, blade surface tin layers are removed completely.
Embodiment 4
Blade formwork is prepared using precision casting process, investment precoat is matched somebody with somebody using schmigel (320 mesh) with silicon sol solution System, powder liquor ratio is 3.3:1, it is dried at ambient temperature after the first coating, 8 hours drying times;Second coating Stucco afterwards, stucco material is 80 mesh emergies, 4 hours drying times;Sanding material is 60 mesh emergies after third layer coating, is done The dry time is 4 hours;Sanding material is 24 mesh emergies after 4th coating, and drying time is 6 hours;Five-layer 7 It is 24 mesh emergies for sanding material after coating, drying time is 6 hours, last slurry seal layer uses investment precoat, drying time For 6 hours;Wax-pattern is removed using steaming process, vapor (steam) temperature is 160 DEG C, and the time is 15 minutes;Formwork is put into after formwork dewaxing It is calcined in roaster, sintering temperature is 1000 DEG C, and soaking time is 4 hours, is furnace-cooled to room temperature and is cleaned;By formwork It is placed in orientation stove, upper area is preheating to 1500 DEG C, and lower area is preheating to 1500 DEG C, and alloy is melted and poured into a mould in smelting furnace, Alloy is orientation or monocrystal nickel-base high-temperature alloy, starts directional solidification growth after being poured, and pulling rate is 9 mm/mins, is drawn Rear furnace cooling is finished, clear shell is then taken out.Blade after clear shell is put into high pressure depoling kettle, taken off using the NaOH aqueous solution Remove, alkali concn is 28%(Mass ratio), temperature is 200 DEG C, and pressure is 0.6MPa, removes 20 hours time;Remaining alkali lye on blade Neutralized using aqueous hydrochloric acid solution, concentration of hydrochloric acid solution is 3%;Finally blade is cleaned using water, drying.Sampled section Detection, blade surface tin layers are removed completely.
Embodiment 5:
Blade formwork is prepared using precision casting process, investment precoat is matched somebody with somebody using schmigel (350 mesh) with silicon sol solution System, powder liquor ratio is 3.3:1, it is dried at ambient temperature after the first coating, 6 hours drying times;Second coating Stucco afterwards, stucco material is 60 mesh emergies, 6 hours drying times;Sanding material is 60 mesh emergies after third layer coating, is done The dry time is 6 hours;Sanding material is 24 mesh emergies after 4th coating, and drying time is 6 hours;Five-layer 7 It is 24 mesh emergies for sanding material after coating, drying time is 6 hours, last slurry seal layer uses investment precoat, drying time For 6 hours;Wax-pattern is removed using steaming process, vapor (steam) temperature is 160 DEG C, and the time is 18 minutes;Formwork is put into after formwork dewaxing It is calcined in roaster, sintering temperature is 1000 DEG C, and soaking time is 2 hours, is furnace-cooled to room temperature and is cleaned;By formwork It is placed in orientation stove, upper area is preheating to 1450 DEG C, and lower area is preheating to 1510 DEG C, and alloy is melted and poured into a mould in smelting furnace, Alloy is orientation or monocrystal nickel-base high-temperature alloy, starts directional solidification growth after being poured, and pulling rate is 10 mm/mins, is drawn System finishes rear furnace cooling, then takes out clear shell.Blade after clear shell is put into high pressure depoling kettle, using the NaOH aqueous solution Removing, alkali concn is 26%(Mass ratio), temperature is 120 DEG C, and pressure is 0.6MPa, removes time 2 h;However, residual base on blade Liquid is neutralized using aqueous hydrochloric acid solution, and concentration of hydrochloric acid solution is 10%;Finally blade is cleaned using water, drying.It is sampled to cut open Detect that blade surface tin layers are removed completely in face.
Embodiment 6:
Blade formwork is prepared using precision casting process, investment precoat is matched somebody with somebody using schmigel (400 mesh) with silicon sol solution System, powder liquor ratio is 3.5:1, it is dried at ambient temperature after the first coating, 4 hours drying times;Second coating Stucco afterwards, stucco material is 80 mesh emergies, 4 hours drying times;Sanding material is 32 mesh emergies after third layer coating, is done The dry time is 4 hours;Sanding material is 24 mesh emergies after 4th coating, and drying time is 4 hours;Five-layer 7 It is 16 mesh emergies for sanding material after coating, drying time is 4 hours, last slurry seal layer uses investment precoat, drying time For 2 hours;Wax-pattern is removed using steaming process, vapor (steam) temperature is 170 DEG C, and the time is 10 minutes;Formwork is put into after formwork dewaxing It is calcined in roaster, sintering temperature is 850 DEG C, and soaking time is 2 hours, is furnace-cooled to room temperature and is cleaned;By formwork It is placed in orientation stove, upper area is preheating to 1500 DEG C, and lower area is preheating to 1480 DEG C, and alloy is melted and poured into a mould in smelting furnace, Alloy is orientation or monocrystal nickel-base high-temperature alloy, starts directional solidification growth after being poured, and pulling rate is 3 mm/mins, is drawn Rear furnace cooling is finished, clear shell is then taken out.Blade after clear shell is put into high pressure depoling kettle, taken off using the KOH aqueous solution Remove, alkali concn is 25%(Mass ratio), temperature is 150 DEG C, and pressure is 0.3MPa, removes 50 hours time;Remaining alkali lye on blade Neutralized using aqueous hydrochloric acid solution, concentration of hydrochloric acid solution is 4%;Finally blade is cleaned using water, drying.Sampled section Detection, blade surface tin layers are removed completely.

Claims (2)

1. liquid metal cooling directional solidification blade surface detinning method, it is characterised in that:Process route is as follows:(1), using essence Close casting technique prepares blade formwork, and directional columnargrain or single crystal blade are prepared using LIQUID Sn cooling directional solidification technique;(2)、 Blade formwork is cleared up;(3), the blade after clear shell is put into high pressure depoling kettle, alkali lye is injected, in certain temperature and pressure Carry out removing tin under power;(4), to being neutralized and being cleaned using acid solution except the blade surface after tin, finally dry, obtain surface The blade of Wuxi;
The preparation technology of blade formwork is as follows:Investment precoat is prepared using 320-400 mesh schmigel with silicon sol solution, powder liquid Mass ratio is 3-3.5:1, it is dried at ambient temperature after the first coating, drying time 4-8 hour;Second coating Stucco afterwards, stucco material is 60-80 mesh emergies, drying time 4-8 hour;Sanding material is that 32-60 mesh is firm after third layer coating Beautiful sand, drying time is 4-8 hours;Sanding material is 24-32 mesh emergies after 4th coating, and drying time is 4-8 hours; Five-layer 7 is that sanding material is 16-24 mesh emergies after coating, and drying time is 4-8 hour, and last slurry seal layer uses face Coating, drying time is 2-8 hours;
Wax-pattern is removed using steaming process, vapor (steam) temperature is 150 DEG C -170 DEG C, and the time is 10-20 minutes;
Formwork is put into roaster after formwork dewaxing and is calcined, sintering temperature is 850-1200 DEG C, soaking time is that 2-6 is small When, it is furnace-cooled to room temperature and is cleaned;
Formwork is placed in orientation stove, upper area is preheating to 1450-1550 DEG C, and lower area is preheating to 1480-1550 DEG C, and alloy is existed Melted in smelting furnace, start crystal-pulling after being poured, pulling rate is 3-12 mm/mins, and drawing finishes rear furnace cooling, then Take out clear shell;
Blade after clear shell is put into high pressure depoling kettle, removed using the NaOH or KOH aqueous solution, alkali concn mass ratio is 25-40%, temperature is 120 DEG C -280 DEG C, and pressure is 0.3-1MPa, removes time 2-50 hour;Remaining alkali lye uses salt on blade Aqueous acid is neutralized, and concentration of hydrochloric acid solution is 1-10%;Finally blade is cleaned using water, drying.
2. liquid metal cooling directional solidification blade surface detinning method according to claim 1, it is characterised in that:Orientation It is orientation or monocrystal nickel-base high-temperature alloy to solidify the material of blade.
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UA39902C2 (en) * 1994-08-08 2001-07-16 Сіменс Акцієнгезельшафт METHOD AND DEVICE FOR DIRECTED HARDENING OF MELT
US20030234092A1 (en) * 2002-06-20 2003-12-25 Brinegar John R. Directional solidification method and apparatus
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CN100543164C (en) * 2007-04-25 2009-09-23 中国科学院金属研究所 A kind of directional solidification heat corrosion resistant nickel base cast superalloy and preparation method thereof
CN102632223B (en) * 2012-04-28 2013-12-25 沈阳工业大学 Surface tin-adhesion-proof method for directionally freezing blade by liquid metal cooling
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CN104646633B (en) * 2013-11-20 2017-06-30 沈阳工业大学 The single crystal blade of local retractable labyrinth ceramic core preparation technology
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