CN114349491A - Composition for preparing silicon-based ceramic core, silicon-based ceramic core blade of aircraft engine and preparation method of silicon-based ceramic core blade - Google Patents
Composition for preparing silicon-based ceramic core, silicon-based ceramic core blade of aircraft engine and preparation method of silicon-based ceramic core blade Download PDFInfo
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Abstract
The invention belongs to the technical field of aviation materials, and particularly relates to a composition for preparing a silicon-based ceramic core, a silicon-based ceramic core blade of an aircraft engine and a preparation method of the silicon-based ceramic core blade. The composition for preparing the silicon-based ceramic core comprises the following components in parts by mass: 30-33 parts of 240-mesh quartz glass powder, 22-24 parts of 600-mesh quartz glass powder, 22-24 parts of 1000-mesh quartz glass powder, 16-20 parts of mineralizer, 0.5-1 part of yttrium oxide, 1-2 parts of mullite, 1-2 parts of cristobalite, 11-18 parts of paraffin, 1-2 parts of beeswax, 0.3-1 part of polyethylene and 0.5-1 part of oleic acid. The composition for preparing the silicon-based ceramic core provided by the invention is easy to depoling and high in high-temperature strength, and the prepared aeroengine silicon-based ceramic core blade is high in yield.
Description
Technical Field
The invention belongs to the technical field of aviation materials, and particularly relates to a composition for preparing a silicon-based ceramic core, a silicon-based ceramic core blade of an aircraft engine and a preparation method of the silicon-based ceramic core blade.
Background
Aircraft turbofan engines are currently the mainstream engines. The turbine front inlet temperature of the conventional 10-grade aero-turbine engine reaches 1800-2000K, and when the thrust-weight ratio of the aero-engine reaches 15-20 grade, the turbine front inlet temperature reaches 2100-2300K, which is far higher than the melting point of the conventional common high-temperature alloy. With the increase of the front inlet temperature of the turbine, in order to realize the long-term safe and reliable operation of the turbine blade of the aircraft engine in a high-temperature environment, an advanced cooling structure and a cooling mode are required to be adopted, so that the temperature of the blade is reduced to be lower than the working temperature which can be borne by materials. Therefore, in order to ensure safe and reliable operation of the turbine at the gas temperature of up to 2000K, advanced cooling technology must be adopted to reduce the wall temperature of the blade in addition to further improving the temperature bearing capacity of the metal material of the turbine.
With the continuous improvement of the performances of aero-engines and industrial gas turbines, turbine cooling technology comes, and more rigorous use requirements are put forward on ceramic cores used as pouring high-efficiency cooling single crystal blade adapters, such as requirements of better precision, higher high temperature resistance and thermal shock resistance.
The near-net-shape investment precision casting is an effective method for producing castings with high precision, low roughness and complex shapes, and is used as a main method for producing high-temperature alloy blades and complex structural parts of aero-engines. The inner cavity of investment casting is mostly formed together with the shape by coating, sand scattering and other methods. When the casting cavity is too narrow or complicated in shape, or the cavity cannot be dried and hardened, the casting cavity must be formed by means of a ceramic core prepared in advance. When the hollow blade is precisely cast, the dimensional accuracy and the qualification rate of the blade are determined to a great extent by the form and position accuracy and the high-temperature strength of the ceramic core. However, the problems of difficult depoling and low high-temperature strength generally exist in the conventional silicon-based ceramic core formula for the aero-engine blade, so that the yield of the aero-engine silicon-based ceramic core blade is low.
Disclosure of Invention
In view of the above, the invention aims to provide a composition for preparing a silicon-based ceramic core, the composition provided by the invention is easy to depoling and high in high-temperature strength, and the prepared aeroengine silicon-based ceramic core blade is high in yield.
In order to achieve the purpose of the invention, the invention provides the following technical scheme:
the invention provides a composition for preparing a silicon-based ceramic core, which comprises the following components in parts by mass:
30 to 33 parts of 240-mesh quartz glass powder,
22-24 parts of 600-mesh quartz glass powder,
22-24 parts of 1000-mesh quartz glass powder,
16-20 parts of a mineralizer,
0.5 to 1 part of yttrium oxide,
1-2 parts of mullite,
1-2 parts of cristobalite,
11-18 parts of paraffin wax,
1-2 parts of beeswax, and the preparation method comprises the following steps,
0.3 to 1 part of polyethylene,
0.5-1 part of oleic acid.
Preferably, the mineralising agent comprises zirconium silicate.
The invention also provides a preparation method of the silicon-based ceramic core blade of the aero-engine, which comprises the following steps:
mixing the components according to the composition of the silicon-based ceramic core to obtain core slurry; the composition of the silicon-based ceramic core is the composition of the silicon-based ceramic core in the technical scheme;
performing pressure injection molding on the mold core slurry under the condition of heat preservation, and removing the core to obtain a mold core;
placing the mold core in magnesia or alumina, and sintering to obtain a primary blade;
and strengthening the primary blade to obtain the silicon-based ceramic core blade of the aero-engine.
Preferably, the conditions of the injection molding include: the injection pressure is 40-50 bar, the pressure maintaining time is 20-25 s, the injection speed is 40-60 CC/s, the injection time is 15-25 s, and the mold temperature is 35-50 ℃; the temperature of heat preservation is 90-120 ℃.
Preferably, the sintering comprises: raising the temperature from room temperature to a first temperature at a first temperature raising rate for first heat preservation, wherein the first temperature is 160-180 ℃, and the first heat preservation time is 240-300 min;
raising the temperature from the first temperature to a second temperature at a second temperature raising rate for second heat preservation, wherein the second temperature is 400-500 ℃, and the second heat preservation time is 60-90 min;
raising the temperature from the second temperature to a third temperature at a third temperature raising rate, and carrying out third heat preservation, wherein the third temperature is 900-1000 ℃, and the third heat preservation time is 60-90 min;
heating from the third temperature to a fourth temperature at a fourth heating rate, and carrying out fourth heat preservation, wherein the fourth temperature is 1180-1230 ℃, and the fourth heat preservation time is 300-360 min;
and naturally cooling to room temperature from the fourth temperature.
Preferably, the first heating rate is 2.3-2.7 ℃/min, the second heating rate is 0.3-0.45 ℃/min, the third heating rate is 3-3.5 ℃/min, and the fourth heating rate is 3-3.5 ℃/min.
Preferably, the strengthening comprises sequentially performing high-temperature strengthening and room-temperature strengthening;
the high-temperature strengthening is as follows: placing the primary blades in an ethyl silicate aqueous solution, and sequentially airing and performing first drying after no air bubbles exist to obtain high-temperature reinforced blades;
the room temperature strengthening is as follows: and (3) soaking the high-temperature strengthened blades in epoxy resin hydrolysate, taking out, and then sequentially airing and drying for the second time.
Preferably, the composition of the ethyl silicate aqueous solution comprises: 85-90 vol.% of ethyl silicate, 3.5-8.5 vol.% of alcohol, 5 vol.% of distilled water and 1.5 vol.% of hydrochloric acid solution; the mass fraction of the hydrogen chloride in the hydrochloric acid solution is 36-38%.
Preferably, the epoxy resin hydrolysate comprises the following components: epoxy resins, polyamides and acetone; the mass ratio of the epoxy resin to the polyamide is (50-62.5): (37.5 to 50).
The invention also provides the aero-engine silicon-based ceramic core blade prepared by the preparation method in the technical scheme.
The invention provides a composition for preparing a silicon-based ceramic core, which comprises the following components in parts by mass: 30-33 parts of 240-mesh quartz glass powder, 22-24 parts of 600-mesh quartz glass powder, 22-24 parts of 1000-mesh quartz glass powder, 16-20 parts of mineralizer, 0.5-1 part of yttrium oxide, 1-2 parts of mullite, 1-2 parts of cristobalite, 11-18 parts of paraffin, 1-2 parts of beeswax, 0.3-1 part of polyethylene and 0.5-1 part of oleic acid.
According to the invention, 240-mesh quartz glass powder, 600-mesh quartz glass powder and 1000-mesh quartz glass powder are used as main materials of the silicon-based ceramic core for the blade of the aircraft engine, so that basic forming performance is provided, and meanwhile, a main body with a certain porosity is formed after sintering through different grain size compositions, so that the silicon-based ceramic core has good porosity and strength, and is convenient to cast and depoling; the mineralizer can reduce the sintering temperature and the mullite temperature in the core sintering process; the yttrium oxide is used as a stabilizer, has unique stress-induced phase change toughening property, can overcome the defect of high brittleness of ceramic, and improves the high-temperature strength by synergistically controlling the content and speed of cristobalite precipitated at high temperature by mullite and cristobalite, so that the content of the cristobalite at high temperature is controlled to be 15-20%, and the mold core has the maximum high-temperature strength; the paraffin, the beeswax, the polyethylene and the oleic acid are used as plasticizers to synergistically improve the molding performance, improve the net dimensional stability of the core in the injection molding process, provide the blank strength in the low-temperature sintering stage and play a role in supporting a main body material.
Experimental results show that the aero-engine silicon-based ceramic core blade obtained by adopting the formula of the aero-engine silicon-based ceramic core provided by the invention is easy to depore, high in high-temperature strength and high in yield.
Detailed Description
The invention provides a composition for preparing a silicon-based ceramic core, which comprises the following components in parts by mass:
30 to 33 parts of 240-mesh quartz glass powder,
22-24 parts of 600-mesh quartz glass powder,
22-24 parts of 1000-mesh quartz glass powder,
16-20 parts of a mineralizer,
0.5 to 1 part of yttrium oxide,
1-2 parts of mullite,
1-2 parts of cristobalite,
11-18 parts of paraffin wax,
1-2 parts of beeswax, and the preparation method comprises the following steps,
0.3 to 1 part of polyethylene,
0.5-1 part of oleic acid.
In the present invention, each component of the composition is a commercially available product well known to those skilled in the art unless otherwise specified.
The composition comprises 30-33 parts by mass of 240-mesh quartz glass powder, preferably 30.5-32.5 parts by mass, and more preferably 31-32 parts by mass.
The composition provided by the invention comprises 22-24 parts by mass of 600-mesh quartz glass powder, preferably 22.3-23.8 parts by mass, and more preferably 22.5-23.5 parts by mass based on 240-mesh quartz glass powder.
The composition provided by the invention comprises 22-24 parts by mass of 1000-mesh quartz glass powder, preferably 22.3-23.8 parts by mass, and more preferably 22.5-23.5 parts by mass based on 240-mesh quartz glass powder.
The composition provided by the invention comprises 16-20 parts of mineralizer, preferably 16.5-19.5 parts, and more preferably 17-19 parts by mass based on 240-mesh quartz glass powder. In the present invention, the mineralizer preferably comprises zirconium silicate.
The composition provided by the invention comprises 0.5-1 part of yttrium oxide, preferably 0.55-0.95 part, more preferably 0.6-0.9 part by mass based on 240-mesh quartz glass powder.
The composition provided by the invention comprises 1-2 parts of mullite, preferably 1-1.8 parts, and more preferably 1-1.5 parts by mass based on 240-mesh quartz glass powder.
The composition provided by the invention comprises 1-2 parts of cristobalite, preferably 1.2-1.8 parts, and more preferably 1.3-1.7 parts by mass based on 240-mesh quartz glass powder.
The composition provided by the invention comprises 11-18 parts of paraffin, preferably 11.5-17.5 parts of paraffin, and more preferably 12-17 parts of quartz glass powder of 240 meshes by mass.
The composition provided by the invention comprises 1-2 parts of beeswax by mass, preferably 1.1-1.9 parts of beeswax by mass, and more preferably 1.2-1.8 parts of beeswax by mass based on 240-mesh quartz glass powder.
The composition provided by the invention comprises 0.3-1 part of polyethylene, preferably 0.35-0.95 part, and more preferably 0.4-0.9 part by mass based on 240-mesh quartz glass powder.
The composition provided by the invention comprises 0.5-1 part of oleic acid, preferably 0.55-0.95 part, and more preferably 0.6-0.9 part by mass based on 240-mesh quartz glass powder.
The invention provides a preparation method of a silicon-based ceramic core blade of an aircraft engine, which comprises the following steps:
mixing the components according to the composition of the silicon-based ceramic core to obtain core slurry; the composition of the silicon-based ceramic core is the composition of the silicon-based ceramic core in the technical scheme;
performing pressure injection molding on the mold core slurry under the condition of heat preservation, and removing the core to obtain a mold core;
placing the mold core in magnesia or alumina, and sintering to obtain a primary blade;
and strengthening the primary blade to obtain the silicon-based ceramic core blade of the aero-engine.
The core slurry is obtained by mixing the ingredients of the composition for preparing the silicon-based ceramic core.
In the present invention, the composition for preparing the silicon-based ceramic core is the composition for preparing the silicon-based ceramic core according to the above technical scheme, and details are not repeated herein.
Before the ingredients are mixed, the invention preferably also comprises the steps of drying 240-mesh quartz glass powder, 600-mesh quartz glass powder, 1000-mesh quartz glass powder, mineralizer, yttrium oxide, mullite and cristobalite in the composition for preparing the silicon-based ceramic core; the drying temperature is preferably 70-90 ℃, and more preferably 75-85 ℃; the time is preferably 2 to 4 hours, and more preferably 2 to 3 hours.
In the present invention, the ingredient mix is preferably: melting and blending paraffin, beeswax and polyethylene, and mixing the obtained melting and blending system with oleic acid to obtain a plasticizing system;
the plasticizing system was mixed with the remaining formulation components.
In the invention, the plasticizing system and the rest of the formula components are preferably mixed by sequentially adding the rest of the formula components into the plasticizing system for three times, wherein the interval between each addition is 10-15 min, and finally stirring is carried out; the other formulation components are preferably added to the plasticizing system after being uniformly mixed.
In the present invention, the stirring preferably includes first stirring and second stirring. In the invention, the first stirring speed is preferably 700-900 rpm, and more preferably 750-850 rpm; the time is preferably 3 to 5 hours, and more preferably 3.5 to 4.5 hours. In the invention, the second stirring speed is preferably 500-700 rpm, more preferably 550-650 rpm; the time is preferably 2 to 3 hours, and more preferably 2 to 2.5 hours. In the present invention, the second stirring is preferably performed under vacuum. The invention achieves the effect of removing the defoamation by matching the second stirring with the vacuumizing.
After the core slurry is obtained, the core slurry is subjected to injection molding under the condition of heat preservation, and the core is removed to obtain the core.
In the present invention, the mold for injection molding is preferably preheated before injection molding. In the invention, the preheating temperature is preferably 35-50 ℃, and more preferably 40-45 ℃.
In the invention, the temperature of the heat preservation is preferably 90-120 ℃, more preferably 95-115 ℃, and further preferably 100-110 ℃. In the present invention, the conditions of the injection molding include: the injection pressure is preferably 40-50 bar, more preferably 42-48 bar, and still more preferably 43-47 bar; the pressure maintaining time is preferably 20-25 s, more preferably 21-24 s, and further preferably 22-23 s; the injection speed is preferably 40-60 CC/s, more preferably 42-58 CC/s, and still more preferably 45-55 CC/s; the injection time is preferably 15-25 s, more preferably 17-24 s, and further preferably 19-23 s; the mold temperature is preferably 35 to 50 ℃, and more preferably 40 to 45 ℃.
The present invention is not particularly limited to the core removal, and the core removal known to those skilled in the art may be employed.
After the core is obtained, the core is placed in magnesia or alumina and sintered to obtain the primary blade.
In the present invention, the core is preferably placed in magnesia: and pouring the magnesia filler into the sagger, inserting the mold core into the magnesia filler, and continuously adding the magnesia filler until the mold core is completely embedded into the magnesia filler and is tamped.
In the present invention, the insert is preferably placed in alumina: and pouring alumina filler into the sagger, inserting the core into the alumina filler, and continuously adding the alumina filler until the core is completely embedded into the alumina filler, and compacting.
In the present invention, the sintering includes: the temperature is increased from the room temperature to the first temperature at a first temperature increasing rate for first heat preservation, the temperature is increased from the first temperature to the second temperature at a second temperature increasing rate for second heat preservation, the temperature is increased from the second temperature to the third temperature at a third temperature increasing rate for third heat preservation, the temperature is increased from the third temperature to the fourth temperature at a fourth temperature increasing rate for fourth heat preservation, and the temperature is naturally reduced from the fourth temperature to the room temperature.
In the invention, the first temperature rise rate is preferably 2.3-2.7 ℃/min, and more preferably 2.4-2.6 ℃/min; the first temperature is preferably 160-180 ℃, and more preferably 165-175 ℃; the first heat preservation time is preferably 240-300 min, and more preferably 260-300 min. In the invention, the second heating rate is preferably 0.3-0.45 ℃/min, and more preferably 0.35-0.4 ℃/min; the second temperature is preferably 400-500 ℃, and more preferably 420-480 ℃; the second heat preservation time is preferably 60-90 min, and more preferably 60-80 min. In the invention, the third heating rate is preferably 3-3.5 ℃/min, and more preferably 3.05-3.4 ℃/min; the third temperature is preferably 900-1000 ℃, and more preferably 950-1000 ℃; the third heat preservation time is preferably 60-90 min, and more preferably 60-80 min. In the invention, the fourth heating rate is preferably 3-3.5 ℃/min, and more preferably 3.05-3.4 ℃/min; the fourth temperature is preferably 1180-1230 ℃, and more preferably 1190-1210 ℃; the fourth heat preservation time is preferably 300-360 min, and more preferably 320-360 min.
After the primary blade is obtained, the primary blade is strengthened to obtain the silicon-based ceramic core blade of the aero-engine.
In the present invention, the strengthening preferably includes sequentially performing high temperature strengthening and room temperature strengthening.
In the present invention, the high-temperature strengthening is preferably: and (3) placing the primary blades in an ethyl silicate aqueous solution, and airing and drying for the first time after no air bubbles exist to obtain the high-temperature strengthened blades.
In the present invention, the composition of the ethyl silicate aqueous solution preferably includes: 85-90 vol.% of ethyl silicate, 3.5-8.5 vol.% of alcohol, 5 vol.% of distilled water and 1.5 vol.% of hydrochloric acid solution. In the invention, the mass fraction of the hydrogen chloride in the hydrochloric acid solution is preferably 36-38%.
In the invention, the air drying time in the high-temperature strengthening is preferably 6-8 h, and more preferably 6-7 h.
In the invention, the temperature of the first drying is preferably 170-190 ℃, and more preferably 175-185 ℃; the time is preferably 1.5 to 2.5 hours, and more preferably 1.8 to 2.2 hours.
In the present invention, the room temperature strengthening is preferably: and (3) soaking the high-temperature strengthened blade in epoxy resin hydrolysate, taking out, and then sequentially airing and drying for the second time to obtain the silicon-based ceramic core blade of the aero-engine.
In the present invention, the composition of the epoxy resin hydrolysate preferably includes epoxy resin, polyamide and acetone. In the invention, the mass ratio of the epoxy resin to the polyamide is preferably (50-62.5): (37.5-50), more preferably (55-62.5): (37.5 to 45), most preferably 62.5: 37.5. in the present invention, the content of acetone in the epoxy resin hydrolysate is preferably 70 wt.%.
In the invention, the time for soaking the high-temperature reinforced blade in the epoxy resin hydrolysate is preferably 30-40 min, and more preferably 33-37 min.
In the invention, the airing time in room temperature reinforcement is preferably 6-8 h, and more preferably 6-7 h.
In the invention, the temperature of the second drying is preferably 100-120 ℃, and more preferably 105-115 ℃; the time is preferably 30 to 45min, and more preferably 35 to 40 min.
The invention also provides the aero-engine silicon-based ceramic core blade prepared by the preparation method in the technical scheme.
For further illustration of the present invention, the silicon-based ceramic core formulation for an aircraft engine blade, the aircraft engine silicon-based ceramic core blade and the method for manufacturing the same provided by the present invention will be described in detail with reference to the following examples, which should not be construed as limiting the scope of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The reagents used in the examples are all commercially available.
Example 1
The composition for preparing the silicon-based ceramic core comprises the following components in parts by mass:
30.4 parts of 240-mesh quartz glass powder, 22.8 parts of 600-mesh quartz glass powder, 22.8 parts of 1000-mesh quartz glass powder, 20 parts of mineralizer zirconium silicate, 1 part of yttrium oxide, 1 part of mullite, 2 parts of cristobalite, 11.9 parts of paraffin, 1.26 parts of beeswax, 0.84 part of polyethylene and 0.5 part of oleic acid.
Application example 1
Weighing the formula components according to the proportion of the embodiment 1, drying 240-mesh quartz glass powder, 600-mesh quartz glass powder, 1000-mesh quartz glass powder, a mineralizer, yttrium oxide, mullite and cristobalite at 80 ℃ for 2h, and uniformly mixing; melting and blending paraffin, beeswax and polyethylene, and mixing the obtained melting and blending system with oleic acid to obtain a plasticizing system; sequentially adding the components of the non-plasticizing system into the plasticizing system for three times at an interval of 10-15 min each time, stirring at 800rpm for 4h, and vacuumizing and stirring at 600rpm for 2h to obtain core slurry;
putting the core slurry into a charging barrel of a pressure injection machine for heating and melting, starting pressure injection molding when the core slurry can be injected out, preheating the temperature of a mold to 40 ℃, and then carrying out pressure injection molding on the core slurry, wherein the pressure injection molding conditions comprise: the injection pressure is 40bar, the dwell time is 20s, the injection speed is 50CC/s, the injection time is 20s, the heating melting temperature is 105 ℃, and silicone oil is used for demoulding in the injection molding process. Trimming the obtained mold core by using tools such as a brush and the like after the injection molding;
after the magnesia filler is poured into the sagger, inserting the obtained core into the magnesia filler, continuously adding the magnesia filler until the core is completely embedded into the magnesia filler, and then placing the sagger into a vibration experiment table for filler compaction; and (3) putting the sagger into a sintering furnace for sintering, wherein the sintering conditions comprise: heating from room temperature to 175 ℃ at the speed of 2.5 ℃/min, keeping the temperature for 300min, heating from 175 ℃ to 450 ℃ at the heating rate of 0.39 ℃/min, keeping the temperature for 60min, heating from 450 ℃ to 1000 ℃ at the heating rate of 3.06 ℃/min, keeping the temperature for 60min, heating from 1000 ℃ to 1200 ℃ at the heating rate of 2.98 ℃/min, keeping the temperature for 360min, naturally cooling to room temperature, closing a sintering furnace after sintering, cooling to below 80 ℃ along with the furnace, taking out a sagger, and obtaining a primary blade;
placing the primary leaves in ethyl silicate hydrolysate (ethyl silicate 90 vol.%, alcohol 3.5 vol.%, distilled water 5 vol.%, hydrochloric acid 1.5 vol.%), taking out and airing for 6h after bubbles overflow, and then placing in a drying oven to dry for 2h at 180 ℃ to obtain high-temperature strengthened leaves; and (2) placing the high-temperature strengthened blade into epoxy resin hydrolysate (the mass ratio of epoxy resin to polyamide is 62.5: 37.5, and the content of acetone in the epoxy resin hydrolysate is 70 wt.%) to be soaked for 35min, taking out and airing for 6h, and then placing the blade into a drying oven to be dried for 40min at 110 ℃ to obtain the silicon-based ceramic core blade of the aero-engine.
Example 2
The composition for preparing the silicon-based ceramic core comprises the following components in parts by mass:
32 parts of 240-mesh quartz glass powder, 24 parts of 600-mesh quartz glass powder, 24 parts of 1000-mesh quartz glass powder, 16 parts of mineralizer, 0.8 part of yttrium oxide, 1.6 parts of mullite, 1.6 parts of cristobalite, 17.8 parts of paraffin, 1 part of beeswax, 0.4 part of polyethylene and 0.5 part of oleic acid.
Application example 2
Weighing the formula components according to the proportion of the embodiment 2, drying 240-mesh quartz glass powder, 600-mesh quartz glass powder, 1000-mesh quartz glass powder, a mineralizer, yttrium oxide, mullite and cristobalite at 80 ℃ for 2h, and uniformly mixing; melting and blending paraffin, beeswax and polyethylene, and mixing the obtained melting and blending system with oleic acid to obtain a plasticizing system; sequentially adding the components of the non-plasticizing system into the plasticizing system for three times at an interval of 10-15 min each time, stirring at 800rpm for 4h, and vacuumizing and stirring at 600rpm for 2h to obtain core slurry;
putting the core slurry into a charging barrel of a pressure injection machine for heating and melting, starting pressure injection molding when the core slurry can be injected out, preheating the temperature of a mold to 40 ℃, and then carrying out pressure injection molding on the core slurry, wherein the pressure injection molding conditions comprise: the injection pressure is 45bar, the dwell time is 15s, the injection speed is 50CC/s, the injection time is 15s, the heating melting temperature is 105 ℃, and silicone oil is used for demoulding in the injection molding process. Trimming the obtained mold core by using tools such as a brush and the like after the injection molding;
after the magnesia filler is poured into the sagger, inserting the obtained core into the magnesia filler, continuously adding the magnesia filler until the core is completely embedded into the magnesia filler, and then placing the sagger into a vibration experiment table for filler compaction; and (3) putting the sagger into a sintering furnace for sintering, wherein the sintering conditions comprise: heating from room temperature to 175 ℃ at the speed of 2.5 ℃/min, keeping the temperature for 300min, heating from 175 ℃ to 450 ℃ at the heating rate of 0.39 ℃/min, keeping the temperature for 60min, heating from 450 ℃ to 1000 ℃ at the heating rate of 3.06 ℃/min, keeping the temperature for 60min, heating from 1000 ℃ to 1200 ℃ at the heating rate of 2.98 ℃/min, keeping the temperature for 360min, naturally cooling to room temperature, closing a sintering furnace after sintering, cooling to below 80 ℃ along with the furnace, taking out a sagger, and obtaining a primary blade;
placing the primary leaves in ethyl silicate hydrolysate (ethyl silicate 90 vol.%, alcohol 3.5 vol.%, distilled water 5 vol.%, hydrochloric acid 1.5 vol.%), taking out and airing for 6h after bubbles overflow, and then placing in a drying oven to dry for 2h at 180 ℃ to obtain high-temperature strengthened leaves; and (2) placing the high-temperature strengthened blade into epoxy resin hydrolysate (the mass ratio of epoxy resin to polyamide is 62.5: 37.5, and the content of acetone in the epoxy resin hydrolysate is 70 wt.%) to be soaked for 35min, taking out and airing for 6h, and then placing the blade into a drying oven to be dried for 40min at 110 ℃ to obtain the silicon-based ceramic core blade of the aero-engine.
Example 3
The composition for preparing the silicon-based ceramic core comprises the following components in parts by mass:
30 parts of 240-mesh quartz glass powder, 23 parts of 600-mesh quartz glass powder, 23 parts of 1000-mesh quartz glass powder, 20 parts of mineralizer, 1 part of yttrium oxide, 1 part of mullite, 2 parts of cristobalite, 11.9 parts of paraffin, 1.26 parts of beeswax, 0.84 part of polyethylene and 0.5 part of oleic acid.
Application example 3
Weighing the formula components according to the proportion of the embodiment 3, drying 240-mesh quartz glass powder, 600-mesh quartz glass powder, 1000-mesh quartz glass powder, a mineralizer, yttrium oxide, mullite and cristobalite at 80 ℃ for 2h, and uniformly mixing; melting and blending paraffin, beeswax and polyethylene, and mixing the obtained melting and blending system with oleic acid to obtain a plasticizing system; sequentially adding the components of the non-plasticizing system into the plasticizing system for three times at an interval of 10-15 min each time, stirring at 800rpm for 4h, and vacuumizing and stirring at 600rpm for 2h to obtain core slurry;
putting the core slurry into a charging barrel of a pressure injection machine for heating and melting, starting pressure injection molding when the core slurry can be injected out, preheating the temperature of a mold to 40 ℃, and then carrying out pressure injection molding on the core slurry, wherein the pressure injection molding conditions comprise: the injection pressure is 40bar, the pressure maintaining time is 15s, the injection speed is 50CC/s, the injection time is 15s, the heating melting temperature is 105 ℃, and silicone oil is used for demoulding in the injection molding process. Trimming the obtained mold core by using tools such as a brush and the like after the injection molding;
after the magnesia filler is poured into the sagger, inserting the obtained core into the magnesia filler, continuously adding the magnesia filler until the core is completely embedded into the magnesia filler, and then placing the sagger into a vibration experiment table for filler compaction; and (3) putting the sagger into a sintering furnace for sintering, wherein the sintering conditions comprise: heating from room temperature to 175 ℃ at the speed of 2.5 ℃/min, keeping the temperature for 300min, heating from 175 ℃ to 450 ℃ at the heating rate of 0.39 ℃/min, keeping the temperature for 60min, heating from 450 ℃ to 1000 ℃ at the heating rate of 3.06 ℃/min, keeping the temperature for 60min, heating from 1000 ℃ to 1200 ℃ at the heating rate of 2.98 ℃/min, keeping the temperature for 360min, naturally cooling to room temperature, closing a sintering furnace after sintering, cooling to below 80 ℃ along with the furnace, taking out a sagger, and obtaining a primary blade;
placing the primary leaves in ethyl silicate hydrolysate (ethyl silicate 90 vol.%, alcohol 3.5 vol.%, distilled water 5 vol.%, hydrochloric acid 1.5 vol.%), taking out and airing for 6h after bubbles overflow, and then placing in a drying oven to dry for 2h at 180 ℃ to obtain high-temperature strengthened leaves; and (2) placing the high-temperature strengthened blade into epoxy resin hydrolysate (the mass ratio of epoxy resin to polyamide is 62.5: 37.5, and the content of acetone in the epoxy resin hydrolysate is 70 wt.%) to be soaked for 35min, taking out and airing for 6h, and then placing the blade into a drying oven to be dried for 40min at 110 ℃ to obtain the silicon-based ceramic core blade of the aero-engine.
Comparative example 1
The composition comprises the following components in parts by mass:
38 parts of 240-mesh quartz glass powder, 28 parts of 600-mesh quartz glass powder, 28 parts of 1000-mesh quartz glass powder, 0 part of mineralizer zirconium silicate, 1 part of yttrium oxide, 0 part of mullite, 3 parts of cristobalite, 11.9 parts of paraffin, 1.26 parts of beeswax, 0.84 part of polyethylene and 0.5 part of oleic acid.
Comparative application example 1
The composition of comparative example 1 was used in place of the composition of example 1, and the remaining technical means were the same as those of application example 1, to obtain a silicon-based ceramic core blade for an aircraft engine.
Comparative example 2
The composition comprises the following components in parts by mass:
37 parts of 240-mesh quartz glass powder, 28.5 parts of 600-mesh quartz glass powder, 28.5 parts of 1000-mesh quartz glass powder, 0 part of mineralizer zirconium silicate, 2.1 parts of aluminum oxide, 1 part of yttrium oxide, 1 part of mullite, 2 parts of cristobalite, 11.9 parts of paraffin, 1.26 parts of beeswax, 0.84 part of polyethylene and 0.5 part of oleic acid.
Comparative application example 2
The composition of comparative example 2 was used in place of the composition of example 1, and the remaining technical means were the same as those of application example 1 to obtain a silicon-based ceramic core blade for an aircraft engine.
Preparing a plurality of batches in parallel for the corresponding application examples 1-3 and the comparative application examples 1-2, and respectively testing, wherein the test items and the corresponding test methods are respectively as follows: and (4) carrying out a three-point bending test by using a high-temperature bending machine, and testing the high-temperature strength under different temperature conditions.
The test results are shown in tables 1-5.
Table 1 strength test results (MPa) of application example 1
| Sample No. 1 | Sample No. 2 | Sample No. 3 | Sample No. 4 | Mean value of | Mean value after elimination of anomalies | |
| 1460℃ | 18.96 | 21.15 | 15.84 | / | 18.65 | 18.65 |
| 1480℃ | 19.92 | 17.6 | 21.79 | / | 19.77 | 19.77 |
| 1500℃ | 23.17 | 22.1 | 23.25 | / | 22.84 | 22.84 |
| 1520℃ | 22.31 | 24.86 | 22.7 | 22.91 | 23.2 | 23.20 |
| 1540℃ | 20.59 | 19.86 | 24.37 | / | 21.67 | 21.61 |
Table 2 strength test results (MPa) of application example 2
| Sample No. 1 | Sample No. 2 | Sample No. 3 | Sample No. 4 | Mean value of | Mean value after elimination of anomalies | |
| 1460℃ | 18.60 | 20.25 | 21.66 | 18.93 | 19.86 | 19.86 |
| 1480℃ | 23.22 | 21.82 | 24.72 | 17.02 | 21.70 | 21.70 |
| 1500℃ | 20.91 | 18.80 | 20.73 | 17.10 | 19.39 | 19.39 |
| 1520℃ | 16.66 | 17.99 | 19.54 | / | 18.05 | 18.05 |
| 1540℃ | 16.06 | 16.79 | 17.76 | / | 16.87 | 16.87 |
Table 3 strength test results (MPa) of application example 3
| Sample No. 1 | Sample No. 2 | Sample No. 3 | Sample No. 4 | Mean value of | Mean value after elimination of anomalies | |
| 1460℃ | 14.06 | 12.36 | 16.84 | / | 14.42 | 14.42 |
| 1480℃ | 19.28 | 21 | 19.48 | 22.27 | 20.51 | 20.51 |
| 1500℃ | 25.73 | 17.79 | 119.68 | / | 21.07 | 18.74 |
| 1520℃ | 18 | 12.67 | 14.58 | 17.87 | 15.78 | 15.78 |
| 1540℃ | 18.25 | 16.62 | 18.64 | / | 17.84 | 17.84 |
Table 4 strength test results (MPa) of comparative application example 1
| Sample No. 1 | Sample No. 2 | Sample No. 3 | Sample No. 4 | Mean value of | Mean value after elimination of anomalies | |
| 1460℃ | 9.17 | 9.33 | 6.04 | 4.29 | 7.21 | 7.21 |
| 1480℃ | 8.52 | 12.5 | 8.4 | 11.4 | 10.21 | 10.21 |
| 1500℃ | 10.11 | 12.67 | 8.28 | / | 10.35 | 10.35 |
| 1520℃ | 13.34 | 10.09 | 10.86 | 13.72 | 12 | 12 |
| 1540℃ | 11.09 | 12.29 | 9.67 | 12.15 | 11.3 | 11.3 |
TABLE 5 Strength test results (MPa) for comparative application example 2
| Sample No. 1 | Sample No. 2 | Sample No. 3 | Sample No. 4 | Mean value of | Mean value after elimination of anomalies | |
| 1460℃ | 23.80 | 27.02 | / | / | 25.41 | 25.41 |
| 1480℃ | 29.48 | 22.21 | 14.47 | / | 22.05 | 25.84 |
| 1500℃ | 28.67 | 24.38 | 26.20 | / | 26.42 | 26.42 |
| 1520℃ | 26.21 | 29.45 | 26.71 | / | 27.46 | 27.46 |
| 1540℃ | 26.84 | 21.63 | 25.64 | 28.02 | 25.53 | 25.53 |
As can be seen from tables 1-5, the silicon-based ceramic core prepared by the composition provided by the invention has excellent high-temperature strength. In addition, the composition provided in comparative application example 2, although the high temperature performance was still acceptable, had difficulty in decoring; when the composition provided by the invention is used for preparing the silicon-based ceramic core of the aero-engine, the core is easy to remove, the high-temperature strength of the blade can be ensured, and the yield is high.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The composition for preparing the silicon-based ceramic core comprises the following components in parts by mass:
2. the composition of claim 1, wherein the mineralizer comprises zirconium silicate.
3. A preparation method of a silicon-based ceramic core blade of an aircraft engine comprises the following steps:
mixing the components according to the composition of the silicon-based ceramic core to obtain core slurry; the silicon-based ceramic core composition is the silicon-based ceramic core composition as defined in any one of claims 1-2;
performing pressure injection molding on the mold core slurry under the condition of heat preservation, and removing the core to obtain a mold core;
placing the mold core in magnesia or alumina, and sintering to obtain a primary blade;
and strengthening the primary blade to obtain the silicon-based ceramic core blade of the aero-engine.
4. The production method according to claim 3, wherein the conditions of the injection molding include: the injection pressure is 40-50 bar, the pressure maintaining time is 20-25 s, the injection speed is 40-60 CC/s, the injection time is 15-25 s, and the mold temperature is 35-50 ℃; the temperature of heat preservation is 90-120 ℃.
5. The method of manufacturing according to claim 3, wherein the sintering includes:
raising the temperature from room temperature to a first temperature at a first temperature raising rate for first heat preservation, wherein the first temperature is 160-180 ℃, and the first heat preservation time is 240-300 min;
raising the temperature from the first temperature to a second temperature at a second temperature raising rate for second heat preservation, wherein the second temperature is 400-500 ℃, and the second heat preservation time is 60-90 min;
raising the temperature from the second temperature to a third temperature at a third temperature raising rate, and carrying out third heat preservation, wherein the third temperature is 900-1000 ℃, and the third heat preservation time is 60-90 min;
heating from the third temperature to a fourth temperature at a fourth heating rate, and carrying out fourth heat preservation, wherein the fourth temperature is 1180-1230 ℃, and the fourth heat preservation time is 300-360 min;
and naturally cooling to room temperature from the fourth temperature.
6. The method according to claim 5, wherein the first temperature rise rate is 2.3 to 2.7 ℃/min, the second temperature rise rate is 0.3 to 0.45 ℃/min, the third temperature rise rate is 3 to 3.5 ℃/min, and the fourth temperature rise rate is 3 to 3.5 ℃/min.
7. The production method according to claim 3, wherein the strengthening comprises sequentially performing high-temperature strengthening and room-temperature strengthening;
the high-temperature strengthening is as follows: placing the primary blades in an ethyl silicate aqueous solution, and sequentially airing and performing first drying after no air bubbles exist to obtain high-temperature reinforced blades;
the room temperature strengthening is as follows: and (3) soaking the high-temperature strengthened blades in epoxy resin hydrolysate, taking out, and then sequentially airing and drying for the second time.
8. The method according to claim 7, wherein the composition of the aqueous ethyl silicate solution comprises: 85-90 vol.% of ethyl silicate, 3.5-8.5 vol.% of alcohol, 5 vol.% of distilled water and 1.5 vol.% of hydrochloric acid solution; the mass fraction of the hydrogen chloride in the hydrochloric acid solution is 36-38%.
9. The method of claim 7, wherein the epoxy resin hydrolysate comprises epoxy resin, polyamide and acetone; the mass ratio of the epoxy resin to the polyamide is (50-62.5): (37.5 to 50).
10. An aeroengine silicon-based ceramic core blade obtained by the preparation method of any one of claims 3 to 9.
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