CN109384460A - A kind of silica-graphene composite ceramic core and preparation method thereof - Google Patents
A kind of silica-graphene composite ceramic core and preparation method thereof Download PDFInfo
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Abstract
A kind of silica-graphene composite ceramic core and preparation method thereof, for solving the problems, such as that silicon-base ceramic core poor fluidity, difficult, the plain embryo intensity low and high temperature performance of molding are poor in the prior art.The present invention provides a kind of good fluidities, the ceramic core material that ratio of briquetting is high, element embryo intensity and elevated temperature strength are high, will introduce ceramic core material system with the grapheme material of excellent mechanical performance and hot property.Grapheme material improves the elevated temperature strength of the mobility of ceramic core slurry, ceramic core ratio of briquetting, plain embryo intensity and ceramic core.In addition, ceramic core compacting qualification rate of the invention, sintering qualification rate are higher, ceramic core strong shock resistance has excellent high temperature stability and elevated temperature strength.
Description
Technical field
The invention belongs to hot investment casting fields, and in particular to a kind of silica-graphene composite ceramic core and its preparation
Method.
Background technique
Aero-engine is the jewel on industrial crown, and hollow blade is since in temperature highest, stress is most complicated, environment
Worst position and the first key component of referred to as aero-engine.High-performance aeroengine hollow blade preparation need through
Tens procedures are crossed, ceramic core is the first procedure for preparing hollow blade, and effect is the inner cavity to form hollow blade, this
Process directly affects the wall thickness and inner cavity dimensional accuracy of blade, determines the qualification rate and casting cost of blade.Aviation of new generation
Aircraft development needs to use more big thrust loading, cooling performance more preferably aero-engine, thus to hollow blade inner structure, ruler
More stringent requirements are proposed for very little precision.There are following characteristics for aero-engine hollow blade of new generation: 1. blade inner-cavity structures
Increasingly complex, inner cavity different parts size span is big, and there are the designs of many superthin structures, and most thin part thickness is only 0.1mm.2.
The pouring condition of blade is more harsh, it usually needs 2h is acted under >=1550 DEG C of pouring temperature could complete to form.It is hollow
Blade inner-cavity structure complexity requires ceramic core material to need to have better processability and corrosion performance；Pouring condition is more
It is harsh to need ceramic core that there is higher elevated temperature strength.
Graphene is a kind of single layer sheet two-dimension nano materials being made of carbon atom.Since its unique bi-dimensional cellular is brilliant
Body structure and high bond strength, graphene are the highest of specific strength in the world, the most hard nano material being currently known, and are broken
Resistance to spalling is up to 130GPa.In addition, graphene has extraordinary heat-conductive characteristic, pure flawless single-layer graphene is led
Hot coefficient is up to 5300W/mK, is the highest carbon material of thermal coefficient so far, is higher than single-walled carbon nanotube (3500W/mK)
With multi-walled carbon nanotube (3000W/mK).
Summary of the invention
The purpose of the present invention will solve to aoxidize that silicon-base ceramic core molding is difficult, elevated temperature strength is low and is not easy to take off in the prior art
The problem of core.The present invention will introduce the high silicon ceramic mould easily reacted with alkali with the grapheme material of excellent mechanical and thermal property
Core architecture, has prepared that a kind of ratio of briquetting is high, elevated temperature strength is good and is easy to the ceramic core material of depoling.
A kind of silica-graphene composite ceramic core material by mass percent 94%~99.4% quartz glass
Powder, 0.5%~3% cristobalite powder, 0.1%~3% Graphene powder and the plasticising for accounting for powder gross mass 15%~24%
Agent is composed.
Currently preferred technical solution are as follows: graphene is modified graphene and graphene oxide.
Currently preferred technical solution are as follows: fused silica powder by 200 mesh, 325 mesh and 500 mesh fused silica powder group
At.
Currently preferred technical solution are as follows: fused silica powder, cristobalite powder and Graphene powder by three-dimensional material mixer into
Row mixing.
A kind of preparation method of silica-graphene composite ceramic core, comprising the following steps:
1) it mixes powder: weighing fused silica powder, cristobalite powder, Graphene powder in proportion and form mixed powder, by mixed powder
It is put into three-dimensional material mixer and carries out mixed powder, be uniformly mixed, the ceramic powder of uniform component；
2) ingredient: weighing plasticizer in proportion, adds it to and is heated to melting in de-airing mixer.Step is added in substep
1) ceramic powder made from, stirs evenly, and after ceramic powder is all added, stirring stops stirring for 24 hours and after vacuumizing 2h, obtains
Obtain ceramic core slurry；
3) it forms: ceramic core slurry is put into ceramic core press injector, it is consistent with pressure injection technological temperature to material temperature
When, by ceramic core slurry pressure injection into required mold, hygrometric state ceramic core is made；
4) it roasts: hygrometric state ceramic core is fitted into the burning alms bowl equipped with alumina packing, be then put into aluminium oxide burning alms bowl
It is roasted in box roaster.Sintering schedule: 400 DEG C are warming up to 0.1 DEG C/min~3 DEG C/min heating rate, with 0.5
DEG C/min~5 DEG C/min heating rate is warming up to 900 DEG C~1000 DEG C, with the heating of 2 DEG C/min~5 DEG C/min heating rate
To 1180 DEG C~1250 DEG C, 2h~8h is kept the temperature, is cooled to 900 DEG C~1000 with 0.5 DEG C/min~1 DEG C/min rate of temperature fall
DEG C, it then cools to room temperature with the furnace, obtains silica-graphene composite ceramic core.
The invention has the following beneficial effects:
A kind of silica-graphene composite ceramic core of the invention and preparation method thereof, will have excellent mechanical performance
And the grapheme material of hot property introduces high silicon ceramic core material system.Grapheme material improve ceramic core ratio of briquetting and
Elevated temperature strength, ceramic core ratio of briquetting >=90% of the invention, elevated temperature strength 25MPa~40MPa, erosion rate >=0.18g/
min。
Detailed description of the invention
Fig. 1 silica-graphene composite ceramic core scanning electron microscope diagram.
Specific embodiment
For that can further appreciate that the contents of the present invention, feature and effect, the following examples are hereby given, and cooperates attached drawing detailed
It is described as follows.It should be noted that the present embodiment be it is descriptive, be not restrictive, cannot thus limit guarantor of the invention
Protect range.
A kind of silica-graphene composite ceramic core material, silica-graphene composite ceramic core material is by quality
The fused silica powder of percentage 94%~99.4%, 0.5%~3% cristobalite powder, 0.1%~3% Graphene powder and
The plasticizer combinations for accounting for powder gross mass 15%~24% form.
Currently preferred technical solution are as follows: graphene is modified graphene and graphene oxide.
Currently preferred technical solution are as follows: fused silica powder by 200 mesh, 325 mesh and 500 mesh fused silica powder group
At.
Currently preferred technical solution are as follows: fused silica powder, cristobalite powder and Graphene powder by three-dimensional material mixer into
Row mixing.
A kind of preparation method of silica-graphene composite ceramic core, comprising the following steps:
1) it mixes powder: weighing fused silica powder, cristobalite powder, Graphene powder in proportion and form mixed powder, by mixed powder
It is put into three-dimensional material mixer and carries out mixed powder, be uniformly mixed, the ceramic powder of uniform component；
2) ingredient: weighing plasticizer in proportion, adds it to and is heated to melting in de-airing mixer.Step is added in substep
1) ceramic powder made from, stirs evenly, and after ceramic powder is all added, stirring stops stirring for 24 hours and after vacuumizing 2h, obtains
Obtain ceramic core slurry；
3) it forms: ceramic core slurry is put into ceramic core press injector, it is consistent with pressure injection technological temperature to material temperature
When, by ceramic core slurry pressure injection into required mold, hygrometric state ceramic core is made；
4) it roasts: hygrometric state ceramic core is fitted into the burning alms bowl equipped with alumina packing, be then put into aluminium oxide burning alms bowl
It is roasted in box roaster.Sintering schedule: 400 DEG C are warming up to 0.1 DEG C/min~3 DEG C/min heating rate, with 0.5
DEG C/min~5 DEG C/min heating rate is warming up to 900 DEG C~1000 DEG C, with the heating of 2 DEG C/min~5 DEG C/min heating rate
To 1180 DEG C~1250 DEG C, 2h~8h is kept the temperature, is cooled to 900 DEG C~1000 with 0.5 DEG C/min~1 DEG C/min rate of temperature fall
DEG C, it then cools to room temperature with the furnace, obtains silica-graphene composite ceramic core.
In addition, currently preferred, the chemical composition of plasticizer materials successively includes: paraffin 93% according to mass percent
~97%, beeswax 1.5%~2%, polyethylene 1%~3%, modified graphene 0.5%~2%.Its function and effect are as follows: improve
The thermophilic performance and dimensional stability of paraffinic base plasticizer materials, press ceramic core moulding rate is high, and graphene increases in paraffinic base
It is uniformly mixed in modeling agent, to obtain good fluidity, the high graphene of ratio of briquetting enhances paraffinic base plasticizer materials.With routine paraffin wax
Base plasticizer materials are compared, and being shunk using the ceramic core element embryo of graphene enhancing paraffinic base plasticizer materials preparation is reduced
30%, plain embryo room temperature intensity improves 50%, plain embryo size non-deformability and improves 20%, and ratio of briquetting improves 60%, ceramic core
Plain embryo contraction can be controlled in 0.1~0.3%, and plain embryo room temperature intensity is up to 10MPa or more, and deformation rate is lower than 10%, and ratio of briquetting is high
Up to 90% or more.
In addition, currently preferred, modified graphene uses matured product in the prior art.
Graphene enhancing alumina based ceramic core in order to more clearly describe the present invention and preparation method thereof, mentions below
For several embodiments:
Embodiment 1
A kind of silica-graphene composite ceramic core material, according to the chemical composition of mass percent are as follows: 200 purposes
Fused silica powder 47%, 325 mesh fused silica powders 12%, 500 mesh fused silica powders 35%, cristobalite powder 3%, Graphene powder
3%.Addition accounts for the plasticizer of powder gross mass 15%.The preparation method of ceramic core, comprising:
1) it mixes powder: according to above-mentioned mass percent, fused silica powder, cristobalite powder, Graphene powder being formed into mixed powder,
Mixed powder is put into three-dimensional material mixer and carries out mixed powder, is uniformly mixed, the ceramic powder of uniform component；
2) ingredient: weighing plasticizer in proportion, adds it to and is heated to melting in de-airing mixer, and then substep is added
Ceramic powder made from step 1), stirs evenly, and after ceramic powder is all added, stirring stops stirring for 24 hours and after vacuumizing 2h
It mixes, obtains ceramic core slurry；
3) it forms: ceramic core slurry is put into ceramic core press injector, it is consistent with pressure injection technological temperature to material temperature
When, by ceramic core slurry pressure injection into required mold, hygrometric state ceramic core is made；
4) it roasts: hygrometric state ceramic core is fitted into the burning alms bowl equipped with alumina packing, be then put into aluminium oxide burning alms bowl
It is roasted in box roaster.Sintering schedule: 400 DEG C are warming up to the heating rate of 0.1 DEG C/min；With 0.5 DEG C/min's
Heating rate is warming up to 900 DEG C；1250 DEG C are warming up to the heating rate of 2 DEG C/min, 2h is kept the temperature, with the cooling of 0.5 DEG C/min
Rate is cooled to 900 DEG C, then cools to room temperature with the furnace, obtains silica-graphene composite ceramic core.
Use silica manufactured in the present embodiment-graphene composite ceramic core ratio of briquetting for 95.5%, elevated temperature strength is
39.2MPa, erosion rate 0.24g/min.
Embodiment 2
A kind of silica-graphene composite ceramic core material, according to the chemical composition of mass percent are as follows: 200 purposes
Fused silica powder 45%, 325 mesh fused silica powders 13%, 500 mesh fused silica powders 38%, cristobalite powder 2%, Graphene powder
2%.Addition accounts for the plasticizer of powder gross mass 17%.
The preparation method of ceramic core, comprising:
1) it mixes powder: according to above-mentioned mass percent, fused silica powder, cristobalite powder, Graphene powder being formed into mixed powder,
Mixed powder is put into three-dimensional material mixer and carries out mixed powder, is uniformly mixed, the ceramic powder of uniform component；
2) ingredient: weighing plasticizer in proportion, adds it to and is heated to melting in de-airing mixer, and then substep is added
Ceramic powder made from step 1), stirs evenly, and after ceramic powder is all added, stirring stops stirring for 24 hours and after vacuumizing 2h
It mixes, obtains ceramic core slurry；
3) it forms: ceramic core slurry is put into ceramic core press injector, it is consistent with pressure injection technological temperature to material temperature
When, by ceramic core slurry pressure injection into required mold, hygrometric state ceramic core is made；
4) it roasts: hygrometric state ceramic core is fitted into the burning alms bowl equipped with alumina packing, be then put into aluminium oxide burning alms bowl
It is roasted in box roaster.Sintering schedule: 400 DEG C are warming up to the heating rate of 0.5 DEG C/min；With the liter of 1 DEG C/min
Warm rate is warming up to 920 DEG C；1220 DEG C are warming up to the heating rate of 2.2 DEG C/min, 3h is kept the temperature, with the cooling of 0.6 DEG C/min
Rate is cooled to 920 DEG C, then cools to room temperature with the furnace, obtains silica-graphene composite ceramic core.
Use silica manufactured in the present embodiment-graphene composite ceramic core ratio of briquetting for 93.5%, elevated temperature strength is
33.4MPa, erosion rate 0.24g/min.
Embodiment 3
A kind of silica-graphene composite ceramic core material, according to the chemical composition of mass percent are as follows: 200 purposes
Fused silica powder 39%, 325 mesh fused silica powders 29%, 500 mesh fused silica powders 29%, cristobalite 2%, Graphene powder 1%.
Addition accounts for the plasticizer of powder gross mass 19%.
The preparation method of ceramic core, comprising:
1) it mixes powder: according to above-mentioned mass percent, fused silica powder, cristobalite powder, Graphene powder being formed into mixed powder,
Mixed powder is put into three-dimensional material mixer and carries out mixed powder, is uniformly mixed, the ceramic powder of uniform component；
2) ingredient: weighing plasticizer in proportion, adds it to and is heated to melting in de-airing mixer, and then substep is added
Ceramic powder made from step 1), stirs evenly, and after ceramic powder is all added, stirring stops stirring for 24 hours and after vacuumizing 2h
It mixes, obtains ceramic core slurry；
3) it forms: ceramic core slurry is put into ceramic core press injector, it is consistent with pressure injection technological temperature to material temperature
When, by ceramic core slurry pressure injection into required mold, hygrometric state ceramic core is made；
4) it roasts: hygrometric state ceramic core is fitted into the burning alms bowl equipped with alumina packing, be then put into aluminium oxide burning alms bowl
It is roasted in box roaster.Sintering schedule: 400 DEG C are warming up to the heating rate of 0.8 DEG C/min；With 1.5 DEG C/min's
Heating rate is warming up to 940 DEG C；1200 DEG C are warming up to the heating rate of 2.4 DEG C/min, 4h is kept the temperature, with the drop of 0.7 DEG C/min
Warm rate is cooled to 960 DEG C, then cools to room temperature with the furnace, obtains silica-graphene composite ceramic core.
Use silica manufactured in the present embodiment-graphene composite ceramic core ratio of briquetting for 93.5%, elevated temperature strength is
30.7MPa, erosion rate 0.23g/min.
Embodiment 4
A kind of silica-graphene composite ceramic core material, according to the chemical composition of mass percent are as follows: 200 purposes
Fused silica powder 36%, 325 mesh fused silica powders 12%, 500 mesh fused silica powders 50%, cristobalite 1%, Graphene powder
0.1%.Addition accounts for the plasticizer of powder gross mass 20%.
The preparation method of ceramic core, comprising:
1) it mixes powder: according to above-mentioned mass percent, fused silica powder, cristobalite powder, Graphene powder being formed into mixed powder,
Mixed powder is put into three-dimensional material mixer and carries out mixed powder, is uniformly mixed, the ceramic powder of uniform component；
2) ingredient: weighing plasticizer in proportion, adds it to and is heated to melting in de-airing mixer, and then substep is added
Ceramic powder made from step 1), stirs evenly, and after ceramic powder is all added, stirring stops stirring for 24 hours and after vacuumizing 2h
It mixes, obtains ceramic core slurry；
3) it forms: ceramic core slurry is put into ceramic core press injector, it is consistent with pressure injection technological temperature to material temperature
When, by ceramic core slurry pressure injection into required mold, hygrometric state ceramic core is made；
4) it roasts: hygrometric state ceramic core is fitted into the burning alms bowl equipped with alumina packing, be then put into aluminium oxide burning alms bowl
It is roasted in box roaster.Sintering schedule: 400 DEG C are warming up to the heating rate of 1.5 DEG C/min；With 2.5 DEG C/min's
Heating rate is warming up to 980 DEG C；1180 DEG C are warming up to the heating rate of 2.6 DEG C/min, 6h is kept the temperature, with the drop of 0.8 DEG C/min
Warm rate is cooled to 980 DEG C, then cools to room temperature with the furnace, obtains silica-graphene composite ceramic core.
Use silica manufactured in the present embodiment-graphene composite ceramic core ratio of briquetting for 90.5%, elevated temperature strength is
25.1MPa, erosion rate 0.30g/min.
Finally it should be noted that: above embodiments only technical solution and feature to illustrate the invention, its object is to
Fields personage is allowed to can understand the content of the present invention and implement it accordingly, it is not intended to limit the scope of the present invention.
Any modification or equivalent replacement without departing from the spirit and scope of the present invention, should all cover protection scope of the present invention it
It is interior.
Claims (5)
1. a kind of silica-graphene composite ceramic core material, it is characterised in that: the silica-graphene composite ceramics
Core material by mass percent 94%~99.4% fused silica powder, 0.5%~3% cristobalite powder, 0.1%~3%
Graphene powder and account for the plasticizer combinations of powder gross mass 15%~24% and form.
2. a kind of silica-graphene composite ceramic core according to claim 1, it is characterised in that: the graphene
For modified graphene and graphene oxide.
3. a kind of silica-graphene composite ceramic core according to claim 1, it is characterised in that: the quartz glass
Glass powder is made of the fused silica powder of 200 mesh, 325 mesh and 500 mesh.
4. a kind of silica-graphene composite ceramic core according to claim 1, it is characterised in that: the quartz glass
Glass powder, cristobalite powder are mixed with Graphene powder by three-dimensional material mixer.
5. a kind of preparation method of silica as described in claim 1-graphene composite ceramic core, it is characterised in that: packet
Include following steps:
1) it mixes powder: weighing fused silica glass powder, cristobalite powder, Graphene powder in proportion and form mixed powder, by mixed powder
It is put into three-dimensional material mixer and carries out mixed powder, be uniformly mixed, the ceramic powder of uniform component；
2) ingredient: weighing plasticizer in proportion, adds it to and is heated to melting in de-airing mixer.Step 1) system is added in substep
The ceramic powder obtained, stirs evenly, and after ceramic powder is all added, stirring stops stirring for 24 hours and after vacuumizing 2h, is made pottery
Porcelain type core slurry；
3) it forms: ceramic core slurry is put into ceramic core press injector, it, will when material temperature is consistent with pressure injection technological temperature
Hygrometric state ceramic core is made into required mold in ceramic core slurry pressure injection；
4) it roasts: hygrometric state ceramic core is fitted into the burning alms bowl equipped with alumina packing, be then put into aluminium oxide burning alms bowl box
It is roasted in roaster.Sintering schedule: being warming up to 400 DEG C with 0.1 DEG C/min~3 DEG C/min heating rate, with 0.5 DEG C/
Min~5 DEG C/min heating rate is warming up to 900 DEG C~1000 DEG C, is warming up to 2 DEG C/min~5 DEG C/min heating rate
1160 DEG C~1250 DEG C, 2 DEG C~8 DEG C are kept the temperature, is cooled to 900 DEG C~1000 with 0.5 DEG C/min~1 DEG C/min rate of temperature fall
DEG C, it then cools to room temperature with the furnace, obtains silica-graphene composite ceramic core.
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| CN110280724A (en) * | 2019-07-25 | 2019-09-27 | 盐城泰欧昌机械有限公司 | A kind of high efficiency and heat radiation core pins |
| CN112222362A (en) * | 2020-09-10 | 2021-01-15 | 中国科学院金属研究所 | Silicon-based ceramic core resistant to cold and hot impact, high-temperature creep and easy to remove and preparation process thereof |
| CN115322009A (en) * | 2021-05-10 | 2022-11-11 | 中国科学院上海硅酸盐研究所 | Large-size silicon-based ceramic core and preparation method thereof |
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