CN102079653A - Method for producing silicon-based ceramic core for aircraft engine blade - Google Patents
Method for producing silicon-based ceramic core for aircraft engine blade Download PDFInfo
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Abstract
The invention discloses a method for producing a silicon-based ceramic core for an aircraft engine blade. The method comprises the steps of: producing the complex ceramic core through hot injection molding by utilizing three high-purity silica powders with different particle sizes as raw materials, the high-purity silica powder in large particle size as a framework, the high-purity silica powder in small particle size as sintering additives, paraffin and beewax as plasticizers, and oleic acid as a surface active agent, carrying out low-temperature dewaxing and high-temperature roasting to the molded bisque ceramic core in a padding alumina to finally obtain the silicon-based ceramic core for the aircraft engine blade.
Description
Technical field
The present invention relates to a kind of ceramic core, more particularly say, be meant a kind of preparation method who is applicable to the high-purity silicon dioxide ceramic core that blade of aviation engine is used.
Background technology
As everyone knows, thrust-weight ratio is to weigh an important indicator of the performance of aircraft engine, and gas turbine is a heart of aero engine.Improve the thrust-weight ratio of aircraft engine, at first will improve the fuel gas temperature of turbine.Since the 1950's, the thrust-weight ratio of the aircraft engine that each advanced country produces improves 16% every year on average, and turbine inlet temperature then raises with the speed in 20 ℃～25 ℃ of every year.Improve turbine inlet temperature and mainly contain 2 kinds of approach: the cooling technology that holds warm ability and hollow blade that improves material.Temperature will reach 1757 ℃ before the advanced at present engine turbine, be subjected to the restriction of melting point metal, if on alloy material, want to improve the warm ability of holding of blade near the limit, therefore need the combination of 2 kinds of approach, adopt the blade-cooling system that becomes increasingly complex in design with in making, promptly produce the air cooling structure that the unusual complicated hollow blade of cavity shape constantly improves blade, improve cooling efficiency.The application of technique for cooling blades is that early stage solid vane is changed over hollow blade, makes cooling air reach the purpose of cooling blade by the complicated inner cavity of blade.In the manufacturing of efficient air cooling blade, because the cavity shape of efficient air cooling blade is very complicated, traditional methods such as forging and pressing, electro-chemical machining have seemed powerless, have only the melted module precise casting technology of employing could solve this difficult problem, but the common forming method (metal Tao Xin, solvable Tao Xin) with investment cast can't form complicated thin thin inner chamber, because refractory materials can not enter wherein during the module dip-coating, sand and drying can not realize.So, must adopt ceramic core, when fusible pattern injection, it is assemblied in the die mould, make the fusible pattern that has ceramic core.After the dewaxing, ceramic core is fixedly mounted in the shell, forms the inner chamber of blade when cast.Therefore, this key problem in technology just is the development of ceramic core.Though ceramic core is not the part of aircraft engine, turbine blade must could form required hollow shape by means of it.Therefore, it all has great effect to the quality of turbine blade and the performance of engine, and its performance and quality will directly influence the qualification rate and the cost of blade.
Ceramic core is to make the core mould according to part required hole or chamber, produces core, during the system wax-pattern core together is pressed in the wax-pattern, removes after the casting pouring moulding again.Ceramic core is used for forming the inner chamber of hollow blade, and the working order of core when casting of metals and blade solidify is very complicated.Core bears bending force under the effect of stress metal, shearing stress can occur at the tenon position that rigidly fixes simultaneously, and the working-surface of core can be subjected to the impact of metal liquid stream when cast.Especially under the directional freeze condition, ceramic core keeps the longer volume time in the molten metal more than 1500 ℃, and, therefore require core at high temperature to have enough strength stabilities owing to axially exist bigger thermograde to cause very big thermal stresses along ceramic core.Because the constructional feature of blade inner chamber can not be carried out machining, its surface smoothness depends on whose surfaces smooth finish fully, therefore requires ceramic core promptly must not have higher chemical stability with metal liquid generation chemical reaction.Ceramic core will bear high pressure, high speed wax liquid when pressing wax impact; To bear the boiling of hot water and steam during dewaxing; Long high temperature action during the shell roasting; Also to bear the mechanical shock and the thermal shocking of molten metal during cast.In addition, various physical abuses and thermal damage that ceramic core also will stand to bring in the manufacturing process flow also will remove from foundry goods by chemical method at last.
The performance of ceramic core depends on the performance of its body material to a great extent.For satisfying the ceramic core performance demands, its body material is selected higher refractory oxide of purity or compound usually for use, and needs to make ceramic core crystal formation that unlikely generation is bigger in heat-processed and variation through the high-temperature stable processing.What can be used as ceramic matrix material at present has silica glass, aluminum oxide, magnesium oxide, a zircon English etc., and wherein the most frequently used is silica glass.In addition, also need add zirconium English powder, mullite, spinel or rare earth oxide in the body material guarantees and improves the warm ability of holding of Tao Xin.
Except that body material, also need add the mineralizer of energy acceleration of sintering and the softening agent of promotion moulding etc. in the ceramic core.
(1) mineralizer requires should form sosoloid or eutectic with matrix, and not form the low melting glass phase in the core roasting process.Mineralizer commonly used both at home and abroad mainly contains zirconium white, magnesium oxide, mullite, commercial alumina and calcium oxide etc.
(2) softening agent is generally organic thermoplastic material, is melted in the filler in their roasting process afterwards, and vapors away.Therefore softening agent is not the moiety of ceramic core, just plays the moulding effect when pressure injection.
The add-on of softening agent (massfraction) is generally 10%～20% of powder.The softening agent add-on has a significant effect to the core performance, though the too much adding of softening agent makes moulding easy, the percent of firing shrinkage of core and void content is increased, and bending strength and volume density reduce, so add-on should strict control.
For the quartz glass substrate core and the alumina base core of widespread use, though wherein also there are some problems in each have their own scope of application.The quartz glass substrate core except the linear expansivity of silica glass is little, outside the good stability, also has an advantage to be easy to exactly fall with alkali liquid corrosion.In actual production, tend in silica-base material, add zirconium English powder, mullite, to improve its high-temperature behavior, comprise hot strength and high temperature creep, but so will reduce its corrosive nature greatly, be unfavorable for removing.Be exactly that silica glass has complicated polymorphic transition change in addition in heating or process of cooling.When silica glass is heated to 1200 ℃ of left and right sides, can change to crystalline state by non-crystalline state, cristobalite is separated out, and follows the appearance of volume effect and produce internal stress, produces tiny crack and cause strength degradation in core, and the performance of ceramic core is produced influence greatly.Therefore, content that must the controlling party quartz in sintering process is to guarantee the over-all properties of core.
Alumina ceramic core does not in use have crystal conversion, and Stability Analysis of Structures is high temperature resistant, and performance is good, raises with temperature, and corundum Tao Xin and corundum shell have the linear expansivity that is complementary again.But the gordian technique of aluminium base Tao Xin is the depoling problem.The depoling of aluminium base Tao Xin is difficulty very, and this also is the main reason that always hinders its widespread use for a long time.At present external depoling technology roughly has 2 kinds: as medium, principle is the first with the villiaumite compounds:
Al
2O
3+F
-——AlF
6 -3
This kind depoling method need be aided with high pressure water washing sometimes.Its two be with alkali lye as medium, with high pressure water washing, so, blade is immersed in for a long time certainly will be influential to its performance in the alkali lye.What have then reaches the purpose that removes core by the mode of developing compound Tao Xin.And still all be to be difficult to the problem that solves both at home and abroad for the depoling of the Tao Xin complex-shaped, that passage is tiny.Russia adopts the mode of High Temperature High Pressure to reach the depoling equipment of removing the aluminum oxide core, western countries are then by developing the mode of composite core, be that the core skin has solid intensive surface, and inside has cellular porous structure, thin and solid superficies can stand the surging force of molten metal, and in the molten metal process of cooling, cracking and make corrosive fluid to infiltrate, the porous internal structure can make corrosive fluid dissolve core quickly, thereby reaches the purpose that removes core.
Comprehensive the above as can be known, have good properties at high temperature and have good corrosion can the preparation research of ceramic core be necessary, so the high temperature use properties of the silicon-base ceramic core with good corrosive nature is mainly studied in this research.
Summary of the invention
Than aluminum oxide, the corrodibility of silicon-dioxide is good, but its high-temperature behavior relatively poor be the reason that restricts always and hinder its development and use.Silica-based ceramic core high-temperature behavior difference chief reason one is that raw material is impure, contains some low-melting metal oxides, produces liquid phase during high temperature, thereby reduces its high temperature use properties; Be exactly that the granular size proportioning is unreasonable in addition, be difficult to sintering.The present invention is based on above 2 points, a kind of preparation method of high-purity silicon dioxide ceramic core has been proposed, it is raw material that this method adopts the high-purity silicon dioxide powder of three kinds of different-grain diameters, is sintering aid with the macrobead for the skeleton small-particle, with paraffin and beeswax is softening agent, with oleic acid is tensio-active agent, prepare complicated ceramic core by hot die-casting molding, the biscuit ceramic core of moulding through low temperature dewaxing and high-temperature roasting, finally obtains the silicon-base ceramic core that is applicable to that blade of aviation engine is used in filling alumina then.Then its correlated performance is studied.
A kind of preparation method who is applicable to the silicon-base ceramic core that blade of aviation engine is used of the present invention, it includes following step:
The mixing of step 1, powder
With taking by weighing mass percent purity is the ball grinder that fine powder, middle powder and the meal of 99.99% silicon-dioxide put into tetrafluoroethylene, and dry grinding obtains powder mix after handling 30min～60min;
After then powder mix being put into oven temperature and be 80 ℃～100 ℃, time of drying 10min～30min, obtain the dry mixed powder;
Required fine powder 8～15g in the powder mix of consumption: 100g, the meal of middle powder 15～30g and surplus;
The median size of fine powder is 1～5 μ m;
The median size of middle powder is 10～25 μ m;
The median size of meal is 40～80 μ m;
Step 2, preparation slip
Putting softening agent into oil bath temperature is to dissolve in 70～90 ℃ the agitator, obtains first intermediate; Softening agent is paraffin and mellisic mixture, and paraffin is 9: 1 with the ratio of mellisic quality;
The dry mixed powder that then step 1 is made was added under whipped state in first intermediate for 5～10min/ time by the timed interval, obtained second intermediate;
Tensio-active agent is added in second intermediate under whipped state, obtains the 3rd intermediate;
The 3rd intermediate is carried out vacuumizing and exhausting bubble handle, the vacuum meter reading is 0.002～0.02MPa, vacuumize 10min～60min after, obtain distributed slurry;
The stirring velocity of agitator is 20～60r/min;
Required softening agent 10～12g in the dry mixed powder of consumption: 100g, tensio-active agent 1～2ml;
Step 3, compression moulding
The distributed slurry that step 2 obtains is passed through wax injector compression moulding, obtain the core base substrate; In order to guarantee formability, the wax slurry keeps 80～90 ℃ in wax injector, simultaneously mould also is preheating to 20～40 ℃ of temperature;
The wax injector pressure of exerting pressure is 0.4～0.6MPa, compression moulding time 30～60s;
Step 4, sintering
The core base substrate of step 3 compression moulding is placed saggar, and bury with silicon dioxide powder; The saggar that base substrate will be housed is then put into High Temperature Furnaces Heating Apparatus and is carried out low temperature dewaxing and high-temperature roasting processing, and the processing system is as follows:
Be warming up to 300 ℃ from 22 ℃, temperature rise rate is 0.5 ℃/min, and is incubated 40min～80min under 300 ℃ of environment;
Be warming up to 400 ℃ from 300 ℃ then, temperature rise rate is 1 ℃/min, and is incubated 40min～80min under 400 ℃ of environment;
Be warming up to 1000 ℃ from 400 ℃ then, temperature rise rate is 3 ℃/min, and is incubated 10min～30min under 1000 ℃ of environment;
Be warming up to 1250 ℃ from 1000 ℃ at last, temperature rise rate is 2 ℃/min, and is incubated 120～240min under 1250 ℃ of environment;
After cooling to 22 ℃～40 ℃ with the furnace, take out, make silicon-base ceramic core.
Preparation method's of the present invention advantage is:
1. this preparation method has realized under the situation of not adding any sintering aid and mineralizer, and has prepared ceramic core under relatively low sintering temperature.
2. the ceramic core that makes through method of the present invention has almost been realized near-net-shape, and sintering shrinks and is controlled at about 7 ‰, and this is for the ceramic core of present those complex-shaped thin-walleds, and is particularly important.
3. the ceramic core porosity that makes through method of the present invention is about 25%, and room temperature strength is about 15MPa, and 1550 ℃ of hot strengths are about 20MPa, and the high temperature amounts of deflection of 1550 ℃ of insulation 30min are almost nil, satisfy at high temperature (〉=1550 ℃) and use down.
Description of drawings
Fig. 1 is secondary electron phase (SEI) figure of powder in the high-purity silicon dioxide.
Fig. 2 is the XRD figure of the silicon-base ceramic core that makes of the embodiment of the invention 1.
Fig. 3 is the SEM figure of the silicon-base ceramic core that makes of the embodiment of the invention 1.
Embodiment
The present invention is a kind of preparation method who is applicable to the silicon-base ceramic core that blade of aviation engine is used, and it includes following step:
The mixing of step 1, powder
To take by weighing high-purity (mass percent purity is 99.99%) fine powder of silicon-dioxide, middle powder and meal and put into the ball grinder of tetrafluoroethylene, dry grinding obtains powder mix after handling 30min～60min;
After then powder mix being put into oven temperature and be 80 ℃～100 ℃, time of drying 10min～30min, obtain the dry mixed powder;
Required fine powder 8～15g in the powder mix of consumption: 100g, the meal of middle powder 15～30g and surplus;
The median size of fine powder is 1～5 μ m;
The median size of middle powder is 10～25 μ m;
The median size of meal is 40～80 μ m;
In the present invention, the powder mix behind the ball milling being carried out long-time drying, is in order to guarantee that it has good flowability in system wax slurry process.
Step 2, preparation slip
Putting softening agent into oil bath temperature is to dissolve in 70～90 ℃ the agitator, obtains first intermediate; Softening agent is paraffin and mellisic mixture, and paraffin is 9: 1 with the ratio of mellisic quality;
The dry mixed powder that then step 1 is made was added under whipped state in first intermediate for 5～10min/ time by the timed interval, obtained second intermediate;
Tensio-active agent is added in second intermediate under whipped state, obtains the 3rd intermediate;
The 3rd intermediate is carried out vacuumizing and exhausting bubble handle, the vacuum meter reading is 0.002～0.02MPa, vacuumize 10min～60min after, obtain distributed slurry;
The stirring velocity of agitator is 20～60r/min;
Required softening agent 10～12g in the dry mixed powder of consumption: 100g, tensio-active agent 1～2ml;
Tensio-active agent can be selected oleic acid, stearic acid for use;
In the present invention, the dry mixed powder that will have certain temperature mixes with softening agent, helps improving flowability, thereby reduces plasticizer dosage.The used plasticizer consumption of industrial general system Al-base ceramic core reaches about 15%.
Step 3, compression moulding
The distributed slurry that step 2 obtains is passed through wax injector compression moulding, obtain the core base substrate; In order to guarantee formability, the wax slurry keeps 80～90 ℃ in wax injector, simultaneously mould also is preheating to 20～40 ℃ of temperature;
The wax injector pressure of exerting pressure is 0.4～0.6MPa, compression moulding time 30～60s;
Step 4, sintering
The core base substrate of step 3 compression moulding is placed saggar, and bury with silicon dioxide powder; The saggar that base substrate will be housed is then put into High Temperature Furnaces Heating Apparatus and is carried out low temperature dewaxing and high-temperature roasting processing, and the processing system is as follows:
Be warming up to 300 ℃ from 22 ℃, temperature rise rate is 0.5 ℃/min, and is incubated 40min～80min under 300 ℃ of environment;
In the present invention, paraffin and beeswax fail to deviate from fully under 300 ℃ of environment, and sample presents black, and this is because of due to paraffin and the beeswax carbonization.
Be warming up to 400 ℃ from 300 ℃ then, temperature rise rate is 1 ℃/min, and is incubated 40min～80min under 400 ℃ of environment;
In the present invention, paraffin and beeswax almost take off to the greatest extent under 400 ℃ of environment, and sample presents the white of raw material (silicon-dioxide) self.
Be warming up to 1000 ℃ from 400 ℃ then, temperature rise rate is 3 ℃/min, and is incubated 10min～30min under 1000 ℃ of environment;
Be warming up to 1250 ℃ from 1000 ℃ at last, temperature rise rate is 2 ℃/min, and is incubated 120～240min under 1250 ℃ of environment;
In the present invention, under 1000 ℃, 1250 ℃ environment, carry out roasting, make sample generation sintering and phase transformation, thereby obtain use properties, as room temperature strength, hot strength, high temperature and creep resistance etc.
After cooling to 22 ℃～40 ℃ with the furnace, take out, make silicon-base ceramic core.
Embodiment 1
The mixing of step 1, powder
To take by weighing high-purity (mass percent purity is 99.99%) fine powder of silicon-dioxide, middle powder and meal and put into the ball grinder of tetrafluoroethylene, dry grinding obtains powder mix after handling 40min;
After then powder mix being put into oven temperature and be 80 ℃, time of drying 30min, obtain the dry mixed powder;
Required fine powder 12.5g in the powder mix of consumption: 100g, the meal of middle powder 25g and surplus;
The median size of fine powder is 2.7 μ m;
The median size of middle powder is 12.44 μ m;
The median size of meal is 43.09 μ m;
In the present invention, the pattern of high-purity (mass percent purity is 99.99%) silicon-dioxide powder mix as shown in Figure 1, among the figure particle be comparatively the rule globosity, help improving the flowability of this silicon-dioxide in softening agent.
Step 2, preparation slip
Putting softening agent into oil bath temperature is to dissolve in 80 ℃ the agitator, obtains first intermediate; Softening agent is paraffin and mellisic mixture, and paraffin is 9: 1 with the ratio of mellisic quality;
The dry mixed powder that then step 1 is made was added in first intermediate under whipped state for 10min/ time by the timed interval, obtained second intermediate;
Oleic acid (tensio-active agent) is added in second intermediate under whipped state, obtains the 3rd intermediate;
The 3rd intermediate is carried out vacuumizing and exhausting bubble handle, the vacuum meter reading is 0.01MPa, vacuumize 30min after, obtain distributed slurry;
The stirring velocity of agitator is 40r/min;
Required softening agent 11g in the dry mixed powder of consumption: 100g, tensio-active agent 1.5ml;
Step 3, compression moulding
The distributed slurry that step 2 obtains is passed through wax injector compression moulding, obtain the core base substrate; In order to guarantee formability, the wax slurry keeps 90 ℃ in wax injector, simultaneously mould also is preheating to 30 ℃ of temperature;
The wax injector pressure of exerting pressure is 0.5MPa, compression moulding time 30s;
Step 4, sintering
The core base substrate of step 3 compression moulding is placed saggar, and bury with silicon dioxide powder; The saggar that base substrate will be housed is then put into High Temperature Furnaces Heating Apparatus and is carried out low temperature dewaxing and high-temperature roasting processing, and the sintering temperature system is as follows:
Be warming up to 300 ℃ from 22 ℃, temperature rise rate is 0.5 ℃/min, and is incubated 60min under 300 ℃ of environment;
Be warming up to 400 ℃ from 300 ℃ then, temperature rise rate is 1 ℃/min, and is incubated 60min under 400 ℃ of environment;
Be warming up to 1000 ℃ from 400 ℃ then, temperature rise rate is 3 ℃/min, and is incubated 30min under 1000 ℃ of environment;
Be warming up to 1250 ℃ from 1000 ℃ at last, temperature rise rate is 2 ℃/min, and is incubated 240min under 1250 ℃ of environment;
After cooling to 30 ℃ with the furnace, take out, make silicon-base ceramic core.
Carry out thing phase XRD analysis with implementing 1 silicon-base ceramic core that makes, find that different-grain diameter raw material powder (silicon-dioxide) has been transformed into cristobalite phase (cristobalite) mutually fully by amorphous glass behind 1250 ℃ of sintering, as shown in Figure 2, among the figure, intensity represents intensity, and tangible phase transformation has taken place silicon dioxide powder before and after the sintering.
Observe the observation sample surface with scanning electronic microscope SEM, sintering has taken place between the particle as can be seen, and porous occurred, as shown in Figure 3.
Adopt the Archimedes method to carry out the apparent porosity measurement to implementing 1 silicon-base ceramic core that makes, surveying its ceramic core porosity is 23.2%; Adopt the room temperature strength of three-point bending method test sample, sample size is 3mm * 4mm * 36mm, and span is 30mm, and room temperature strength is 15MPa; Adopt the hot strength of three-point bending method (HB5353) test sample, sample size is 10mm * 4mm * 60mm, and span is 50mm, and recording 1550 ℃ of hot strengths is 21MPa; Adopt the single cantilever beam method to measure the high temperature deflection test, specimen size 10mm * 4mm * 60mm, an end are fixed in the fire-resistant bearing, and the other end horizontal boom, cantilever end length are 12mm.When measuring 1550 ℃ of amounts of deflection, sample is incubated 0.5 hour in stove, takes out then and measures the cantilever end sag, is 1550 ℃ of amounts of deflection.Measure the back and find that 1550 ℃ high temperature amount of deflection is almost nil, satisfies production application fully.
Embodiment 2
The mixing of step 1, powder
To take by weighing high-purity (mass percent purity is 99.99%) fine powder of silicon-dioxide, middle powder and meal and put into the ball grinder of tetrafluoroethylene, dry grinding obtains powder mix after handling 30min;
After then powder mix being put into oven temperature and be 90 ℃, time of drying 15min, obtain the dry mixed powder;
Required fine powder 10g in the powder mix of consumption: 100g, the meal of middle powder 20g and surplus;
The median size of fine powder is 4.5 μ m;
The median size of middle powder is 20.2 μ m;
The median size of meal is 59.8 μ m;
Step 2, preparation slip
Putting softening agent into oil bath temperature is to dissolve in 90 ℃ the agitator, obtains first intermediate; Softening agent is paraffin and mellisic mixture, and paraffin is 9: 1 with the ratio of mellisic quality;
The dry mixed powder that then step 1 is made was added in first intermediate under whipped state for 5min/ time by the timed interval, obtained second intermediate;
Stearic acid (tensio-active agent) is added in second intermediate under whipped state, obtains the 3rd intermediate;
The 3rd intermediate is carried out vacuumizing and exhausting bubble handle, the vacuum meter reading is 0.005MPa, vacuumize 20min after, obtain distributed slurry;
The stirring velocity of agitator is 60r/min;
Required softening agent 12g in the dry mixed powder of consumption: 100g, tensio-active agent 2ml;
Step 3, compression moulding
The distributed slurry that step 2 obtains is passed through wax injector compression moulding, obtain the core base substrate; In order to guarantee formability, the wax slurry keeps 80 ℃ in wax injector, simultaneously mould also is preheating to 20 ℃ of temperature;
The wax injector pressure of exerting pressure is 0.6MPa, compression moulding time 60s;
Step 4, sintering
The core base substrate of step 3 compression moulding is placed saggar, and bury with silicon dioxide powder; The saggar that base substrate will be housed is then put into High Temperature Furnaces Heating Apparatus and is carried out low temperature dewaxing and high-temperature roasting processing, and the sintering temperature system is as follows:
Be warming up to 300 ℃ from 22 ℃, temperature rise rate is 0.5 ℃/min, and is incubated 80min under 300 ℃ of environment;
Be warming up to 400 ℃ from 300 ℃ then, temperature rise rate is 1 ℃/min, and is incubated 80min under 400 ℃ of environment;
Be warming up to 1000 ℃ from 400 ℃ then, temperature rise rate is 3 ℃/min, and is incubated 20min under 1000 ℃ of environment;
Be warming up to 1250 ℃ from 1000 ℃ at last, temperature rise rate is 2 ℃/min, and is incubated 180min under 1250 ℃ of environment;
After cooling to 22 ℃ with the furnace, take out, make silicon-base ceramic core.
The ceramic core porosity is about 25%, and room temperature strength is 16MPa, and 1550 ℃ of hot strengths are 22MPa, and 1550 ℃ high temperature amount of deflection is almost nil, satisfies production application fully.
Embodiment 3
The mixing of step 1, powder
To take by weighing high-purity (mass percent purity is 99.99%) fine powder of silicon-dioxide, middle powder and meal and put into the ball grinder of tetrafluoroethylene, dry grinding obtains powder mix after handling 60min;
After then powder mix being put into oven temperature and be 100 ℃, time of drying 10min, obtain the dry mixed powder;
Required fine powder 8.3g in the powder mix of consumption: 100g, the meal of middle powder 16.6g and surplus;
The median size of fine powder is 1.7 μ m;
The median size of middle powder is 11.3 μ m;
The median size of meal is 42.5 μ m;
Step 2, preparation slip
Putting softening agent into oil bath temperature is to dissolve in 70 ℃ the agitator, obtains first intermediate; Softening agent is paraffin and mellisic mixture, and paraffin is 9: 1 with the ratio of mellisic quality;
The dry mixed powder that then step 1 is made was added in first intermediate under whipped state for 7min/ time by the timed interval, obtained second intermediate;
Oleic acid (tensio-active agent) is added in second intermediate under whipped state, obtains the 3rd intermediate;
The 3rd intermediate is carried out vacuumizing and exhausting bubble handle, the vacuum meter reading is 0.02MPa, vacuumize 50min after, obtain distributed slurry;
The stirring velocity of agitator is 20r/min;
Required softening agent 12g in the dry mixed powder of consumption: 100g, tensio-active agent 1ml;
Step 3, compression moulding
The distributed slurry that step 2 obtains is passed through wax injector compression moulding, obtain the core base substrate; In order to guarantee formability, the wax slurry keeps 85 ℃ in wax injector, simultaneously mould also is preheating to 40 ℃ of temperature;
The wax injector pressure of exerting pressure is 0.4MPa, compression moulding time 45s;
Step 4, sintering
The core base substrate of step 3 compression moulding is placed saggar, and bury with silicon dioxide powder; The saggar that base substrate will be housed is then put into High Temperature Furnaces Heating Apparatus and is carried out low temperature dewaxing and high-temperature roasting processing, and the sintering temperature system is as follows:
Be warming up to 300 ℃ from 22 ℃, temperature rise rate is 0.5 ℃/min, and is incubated 40min under 300 ℃ of environment;
Be warming up to 400 ℃ from 300 ℃ then, temperature rise rate is 1 ℃/min, and is incubated 40min under 400 ℃ of environment;
Be warming up to 1000 ℃ from 400 ℃ then, temperature rise rate is 3 ℃/min, and is incubated 20min under 1000 ℃ of environment;
Be warming up to 1250 ℃ from 1000 ℃ at last, temperature rise rate is 2 ℃/min, and is incubated 150min under 1250 ℃ of environment;
After cooling to 30 ℃ with the furnace, take out, make silicon-base ceramic core.
The ceramic core porosity is about 25%, and room temperature strength is 13MPa, and 1550 ℃ of hot strengths are 19MPa, and 1550 ℃ high temperature amount of deflection is almost nil, satisfies production application fully.
Claims (4)
1. a blade of aviation engine is characterized in that following step is arranged with the preparation method of silicon-base ceramic core:
The mixing of step 1, powder
With taking by weighing mass percent purity is the ball grinder that fine powder, middle powder and the meal of 99.99% silicon-dioxide put into tetrafluoroethylene, and dry grinding obtains powder mix after handling 30min～60min;
After then powder mix being put into oven temperature and be 80 ℃～100 ℃, time of drying 10min～30min, obtain the dry mixed powder;
Required fine powder 8～15g in the powder mix of consumption: 100g, the meal of middle powder 15～30g and surplus;
The median size of fine powder is 1～5 μ m;
The median size of middle powder is 10～25 μ m;
The median size of meal is 40～80 μ m;
Step 2, preparation slip
Putting softening agent into oil bath temperature is to dissolve in 70～90 ℃ the agitator, obtains first intermediate; Softening agent is paraffin and mellisic mixture, and paraffin is 9: 1 with the ratio of mellisic quality;
The dry mixed powder that then step 1 is made was added under whipped state in first intermediate for 5～10min/ time by the timed interval, obtained second intermediate;
Tensio-active agent is added in second intermediate under whipped state, obtains the 3rd intermediate;
The 3rd intermediate is carried out vacuumizing and exhausting bubble handle, the vacuum meter reading is 0.002～0.02MPa, vacuumize 10min～60min after, obtain distributed slurry;
The stirring velocity of agitator is 20～60r/min;
Required softening agent 10～12g in the dry mixed powder of consumption: 100g, tensio-active agent 1～2ml;
Step 3, compression moulding
The distributed slurry that step 2 obtains is passed through wax injector compression moulding, obtain the core base substrate; In order to guarantee formability, the wax slurry keeps 80～90 ℃ in wax injector, simultaneously mould also is preheating to 20～40 ℃ of temperature;
The wax injector pressure of exerting pressure is 0.4～0.6MPa, compression moulding time 30～60s;
Step 4, sintering
The core base substrate of step 3 compression moulding is placed saggar, and bury with silicon dioxide powder; The saggar that base substrate will be housed is then put into High Temperature Furnaces Heating Apparatus and is carried out low temperature dewaxing and high-temperature roasting processing, and the processing system is as follows:
Be warming up to 300 ℃ from 22 ℃, temperature rise rate is 0.5 ℃/min, and is incubated 40min～80min under 300 ℃ of environment;
Be warming up to 400 ℃ from 300 ℃ then, temperature rise rate is 1 ℃/min, and is incubated 40min～80min under 400 ℃ of environment;
Be warming up to 1000 ℃ from 400 ℃ then, temperature rise rate is 3 ℃/min, and is incubated 10min～30min under 1000 ℃ of environment;
Be warming up to 1250 ℃ from 1000 ℃ at last, temperature rise rate is 2 ℃/min, and is incubated 120～240min under 1250 ℃ of environment;
After cooling to 22 ℃～40 ℃ with the furnace, take out, make silicon-base ceramic core.
2. the blade of aviation engine according to claim 1 preparation method of silicon-base ceramic core, it is characterized in that: tensio-active agent is selected oleic acid or stearic acid for use.
3. the blade of aviation engine according to claim 1 preparation method of silicon-base ceramic core, it is characterized in that: the ceramic core that makes has been transformed into the cristobalite phase mutually fully by amorphous glass behind 1250 ℃ of sintering.
4. the blade of aviation engine according to claim 1 preparation method of silicon-base ceramic core, it is characterized in that: the ceramic core porosity that makes is 25%, room temperature strength is 13～16MPa, 1550 ℃ of hot strengths are 19～21MPa, the high temperature amount of deflection of 1550 ℃ of insulation 30min is almost nil, and the high temperature that satisfies 〉=1550 ℃ uses down.
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