CN109650902A - A kind of preparation method of the graphene-based ceramic composite of high tenacity biomimetic features - Google Patents
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Abstract
The invention discloses a kind of preparation methods of graphene-based ceramic composite of high tenacity biomimetic features; this method prepares layered porous ceramic idiosome using electrostatic field freeze-drying; and pass through vacuum immersion process; so that graphene is impregnated into completely in the hole of prefabricated embryo; after inert gas shielding microwave sintering; graphene is crystallized to and is coated on ceramic crystal surface, microcosmic continuously distributed stratiform is formed and imitates the graphene-based ceramic composite of clam shell feature.The composite ceramic material has high-compactness and fracture toughness compared with traditional ceramics material, while cooperateing with graphene excellent properties, significantly improves the thermally conductive and electric property of the material, has huge application value in fields such as traffic, building, space flight, military projects.
Description
Technical field
The present invention relates to a kind of preparation methods of graphene-based ceramic composite, belong to the preparation of ceramic material material
And applied technical field.
Background technique
Imitative clam shell feature research for ceramic material, general use roll film, tape casting, centrifugal casting, electrophoretic deposition
Fine not enough, substantially simple parallel layers folded structures are designed Deng, structure, interface layer status influences the strength of materials
It is very big, it is easy to situations such as causing layer to crack, in the fabrication process there are many more problem have it is to be solved.
Summary of the invention
The invention discloses a kind of graphene-based ceramic composites of high tenacity biomimetic features.The preparation method passes through graphite
Alkene crystallizes and is coated on ceramic crystal surface, and it is compound to form high-compactness, high rigidity, the imitative concba lamellar structure of high-fracture toughness
Material greatly improves cracking caused by being mismatched by boundary layer bond strength, the disadvantages such as intensity is low, in addition, may additionally facilitate graphite
Alkene cooperates with ceramic material to promote the heating conduction and electric property of composite material, in mobile communication, military affairs, ship, aviation boat
There is huge application potential in the fields such as it.
The technical scheme is that be achieved:
A kind of preparation method of the graphene-based ceramic composite of high tenacity biomimetic features, the specific steps are as follows:
Step 1: preparing ceramic slurry and graphene slurry respectively；
Step 2: preparing layer using electrostatic field freeze-drying using the preparation-obtained ceramic slurry of step 1 as raw material
Shape porous ceramics idiosome obtains the prefabricated embryo of the three-dimensional netted ceramic material framework of aperture；
Step 3: by vacuum immersion process, the three-dimensional netted ceramic material bone of the aperture that step 2 is prepared
The prefabricated embryo of frame is infiltrated in the preparation-obtained graphene slurry of step 1, so that graphene is impregnated into the hole of prefabricated embryo completely
In；
Step 4: using the prefabricated embryo for being impregnated with graphene in inert gas shielding microwave sintering step 3, graphene knot
Brilliant and cladding is embedded in ceramic crystal surface, forms the microcosmic graphene-based ceramic composite of continuously distributed biomimetic features.
Further, the ceramic powder that ceramic slurry is prepared in step 1 is one of silicon carbide, silicon nitride, and be averaged grain
Diameter is 200nm~5 μm.
Further, ceramic slurry prepared in step 1, solvent use water, and ceramic solid content is 10~50%；Point
Powder, to one of isooctyl phenyl ether, adds mass fraction using dodecyl sodium sulfate, ammonium polyacrylate, polyethylene glycol
Amount is 0.1~0.5%；Binder uses one of polytetrafluoroethylene (PTFE), polyvinyl alcohol, polyurethane, and addition mass fraction amount is 1
~5%.
Further, graphene slurry prepared in step 1, solvent use water, and graphene solid content is 1~3%；
Graphene horizontal direction is having a size of 5~15 μm, and vertical direction is with a thickness of 0.6~1.5nm.
Further, electrostatic field direction set in electrostatic field freeze-drying described in step 2 and cryogenic temperature side
To vertical, electric field strength is 5 × 104~9 × 104V/m；Set unidirectional cryogenic temperature is -70~-10 DEG C, and dry pressure is
20~80Pa.
Further, ceramic slurry described in step 1 and graphene slurry are prepared using ball-milling method or sand-blast.
Further, inert gas described in step 4 is argon gas.
Further, microwave sintering temperature described in step 4 is 1500 DEG C -1700 DEG C.
The present invention first passes through electrostatic field freeze-drying and makes the prefabricated embryo one-pass molding of the continuously distributed ceramic material of stratiform, keeps away
Stress match between layers is exempted from.In preparation process that electrostatic field direction is vertical with cryogenic temperature direction, ice crystal is along temperature
It grows while spending gradient direction growth also along electrostatic field direction, by the traction of electric field action, grows into inclined microcosmic
Porous stent structure layer.Again by graphene infiltrate in ordered porous support frame be embedded in and it is sintered combined, ultimately form height
Consistency, high rigidity, the complete macroscopic view of high-fracture toughness imitate clam shell feature.
Graphene-based ceramic composite prepared by the present invention, graphene is by vacuum immersion technique, and uniformly penetrating is simultaneously
Crystallization is coated on ceramic crystal surface, interior after microwave pressure sintering in conjunction with the imitative shell layered framework unique structural feature of ceramics
Dense structure, portion, interface are generated without brittlement phase.Therefore graphene-based ceramic composite forms the multistage toughening machine of different scale
System, improves boundary layer to toughening effects such as deviation, the bridge joints of crackle.In addition, the electricity for cooperateing with graphene excellent, calorifics (are led
Hot coefficient theoretical value 5300W/mK), mechanical property (stretch modulus theoretical value 130GPa), the heating conduction and electricity of the composite material
Performance is learned also to be greatly improved.
The beneficial effects of the present invention are: graphene-based ceramic composite disclosed by the invention is freeze-dried using electrostatic field
Method prepares layered porous ceramic material framework, then graphene is embedded in compound, formation high-compactness, high rigidity, high-fracture toughness
Imitative concba lamellar structure composite material.This method is used to non-toxic, pollution-free, friendly the water of environment and ethyl alcohol as molten
Agent, by modulating associated technical parameters, pore size, stomata pattern and the pore size distribution of controllable producing porous ceramic, to obtain not
With the prefabricated embryo of mechanical property requirements.Electrostatic field freeze-drying make the prefabricated embryo of the continuously distributed ceramic material of stratiform once at
Type avoids Stress match between layers, meanwhile, vacuum immersion technique is passed through as weak interface layer by graphene,
Closely knit infiltration insertion in ceramic material can get so that crackle deviation repeatedly in weak interface layer, consumes a large amount of energy to failure
The laminated ceramic composite of high tenacity and breaking strength.In addition, the electricity for cooperateing with graphene excellent, calorifics (thermal coefficient reason
By value 5300W/mK), mechanical property (stretch modulus theoretical value 130GPa), it can be achieved that dimensional effect, skin effect and component effect
The combination answered, the heating conduction and electric property of the composite material are also greatly improved.
Specific embodiment
The present invention is described in detail with reference to embodiments, but the present embodiment cannot be used for the limitation present invention, all
Using similar method and its similar variation of the invention, protection scope of the present invention should all be included in.
Embodiment 1
Prepare 3w.t.% graphene slurry, wherein graphene horizontal direction is having a size of 5 μm, vertical direction with a thickness of
1.5nm.Graphene slurry is uniformly mixed using ball-milling method, drum's speed of rotation 400r/min, is ground 2 hours.In 1w.t.%
0.1w.t.% dodecyl sodium sulfate is added in polytetrafluoroethyl-ne aqueous solution, after fully dispersed, add 50w.t.% and is averaged grain
Diameter is 5 μm of silicon nitride ceramics.Ceramic slurry is uniformly mixed using ball-milling method, drum's speed of rotation 400r/min, grinding 2 is small
When.Ceramic slurry is injected in flat plate mold and is freeze-dried, sets electrostatic field intensity as 5 × 104V/m, unidirectional freezing temperature
Degree is -10 DEG C, and dry pressure is 20Pa.Vacuum immersion takes out after having prepared graphene slurry after silicon nitride ceramic plate is dry
Prefabricated board carries out microwave sintering under protection of argon gas, and 1500 DEG C of sintering temperature.
Embodiment 2
Prepare 1w.t.% graphene slurry, wherein graphene horizontal direction is having a size of 15 μm, vertical direction with a thickness of
0.6nm.Graphene slurry is uniformly mixed using ball-milling method, drum's speed of rotation 400r/min, is ground 2 hours.In 5w.t.%
0.5w.t.% ammonium polyacrylate is added in aqueous emulsion of polyurethane, after fully dispersed, adding 50w.t.% average grain diameter is
500nm silicon carbide ceramics powder.Ceramic slurry is uniformly mixed using ball-milling method, drum's speed of rotation 400r/min, grinding 2 is small
When.Ceramic slurry is injected in flat plate mold and is freeze-dried, sets electrostatic field intensity as 9 × 104V/m, unidirectional freezing temperature
Degree is -70 DEG C, and dry pressure is 80Pa.Vacuum immersion takes out after having prepared graphene slurry after silicon carbide ceramics plate is dry
Prefabricated board carries out microwave sintering under protection of argon gas, and 1700 DEG C of sintering temperature.
Embodiment 3
Prepare 3w.t.% graphene slurry, wherein graphene horizontal direction is having a size of 10 μm, vertical direction with a thickness of
1.5nm.Graphene slurry is uniformly mixed using ball-milling method, drum's speed of rotation 400r/min, is ground 2 hours.In 3w.t.%
0.3w.t.% polyethylene glycol is added in polyvinyl alcohol water solution to isooctyl phenyl ether, after fully dispersed, adds 35w.t.%
Average grain diameter is 200nm silicon carbide ceramics powder.Ceramic slurry is uniformly mixed using ball-milling method, drum's speed of rotation 400r/
Min is ground 2 hours.Ceramic slurry is injected in flat plate mold and is freeze-dried, sets electrostatic field intensity as 9 × 104V/m,
Unidirectional cryogenic temperature is -50 DEG C, and dry pressure is 80Pa.Vacuum immersion is in having prepared graphene slurry after silicon carbide ceramics plate is dry
After material, takes out prefabricated board and carry out microwave sintering under protection of argon gas, 1700 DEG C of sintering temperature.
Embodiment 4
Prepare 1w.t.% graphene slurry, wherein graphene horizontal direction is having a size of 5 μm, vertical direction with a thickness of
1.2nm.Graphene slurry is uniformly mixed using ball-milling method, drum's speed of rotation 400r/min, is ground 2 hours.In 1w.t.%
0.3w.t.% dodecyl sodium sulfate is added in polytetrafluoroethyl-ne aqueous solution, after fully dispersed, add 10w.t.% and is averaged grain
Diameter is 5 μm of silicon nitride ceramics.Ceramic slurry is uniformly mixed using ball-milling method, drum's speed of rotation 400r/min, grinding 2 is small
When.Ceramic slurry is injected in flat plate mold and is freeze-dried, sets electrostatic field intensity as 7 × 104V/m, unidirectional freezing temperature
Degree is -30 DEG C, and dry pressure is 30Pa.Vacuum immersion takes out after having prepared graphene slurry after silicon nitride ceramic plate is dry
Prefabricated board carries out microwave sintering under protection of argon gas, and 1500 DEG C of sintering temperature.
Embodiment 5
Prepare 2w.t.% graphene slurry, wherein graphene horizontal direction is having a size of 10 μm, vertical direction with a thickness of
1.2nm.Graphene slurry is uniformly mixed using ball-milling method, drum's speed of rotation 400r/min, is ground 2 hours.In 1w.t.%
0.3w.t.% polyethylene glycol is added in polyvinyl alcohol water solution to isooctyl phenyl ether, after fully dispersed, adds 30w.t.%
Average grain diameter is 1 μm of silicon nitride ceramic.Ceramic slurry is uniformly mixed using ball-milling method, drum's speed of rotation 400r/min,
Grinding 2 hours.Ceramic slurry is injected in flat plate mold and is freeze-dried, sets electrostatic field intensity as 7 × 104V/m, unidirectionally
Cryogenic temperature is -50 DEG C, and dry pressure is 50Pa.Vacuum immersion is in having prepared graphene slurry after silicon nitride ceramic plate is dry
Afterwards, it takes out prefabricated board and carries out microwave sintering under protection of argon gas, 1500 DEG C of sintering temperature.
Following table is the graphene-based ceramic composite performance of high tenacity biomimetic features prepared by 5 embodiments:
| Main component | Bending strength (MPa) | Consistency (%) | |
| Standard silicon nitride ceramics | Silicon nitride | 391 | / |
| Standard silicon carbide ceramics | Silicon carbide | 224 | / |
| Embodiment 1 | Silicon nitride | 535 | 96.5 |
| Embodiment 2 | Silicon carbide | 386 | 97.2 |
| Embodiment 3 | Silicon carbide | 463 | 98.0 |
| Embodiment 4 | Silicon nitride | 495 | 96.0 |
| Embodiment 5 | Silicon nitride | 810 | 97.5 |
As can be seen from the table, composite material prepared by embodiment has an excellent mechanical property, bending strength with
Intrinsic ceramic material improves consistency, the crystallinity of material by the process optimization compared to being obviously improved, composite material
It fracture toughness and thermally conductive is expected to further to be promoted with electric conductivity.
Claims (8)
1. a kind of preparation method of the graphene-based ceramic composite of high tenacity biomimetic features, it is characterised in that: specific steps are such as
Under:
Step 1: preparing ceramic slurry and graphene slurry respectively；
Step 2: using the preparation-obtained ceramic slurry of step 1 as raw material, it is more using electrostatic field freeze-drying preparation stratiform
Hole ceramic idiosome obtains the prefabricated embryo of the three-dimensional netted ceramic material framework of aperture；
Step 3: by vacuum immersion process, the three-dimensional netted ceramic material framework of the aperture that step 2 is prepared is pre-
Embryo processed is infiltrated in the preparation-obtained graphene slurry of step 1, so that graphene is impregnated into completely in the hole of prefabricated embryo；
Step 4: graphene crystallizes simultaneously using the prefabricated embryo for being impregnated with graphene in inert gas shielding microwave sintering step 3
Cladding is embedded in ceramic crystal surface, forms the microcosmic graphene-based ceramic composite of continuously distributed biomimetic features.
2. a kind of preparation method of graphene-based ceramic composite of high tenacity biomimetic features according to claim 1,
Be characterized in that: the ceramic powder that ceramic slurry is prepared in step 1 is one of silicon carbide, silicon nitride, and average grain diameter is
200nm~5 μm.
3. a kind of preparation method of graphene-based ceramic composite of high tenacity biomimetic features according to claim 1,
Be characterized in that: prepared ceramic slurry in step 1, solvent use water, and ceramic solid content is 10~50%；Dispersing agent uses
To one of isooctyl phenyl ether, adding mass fraction amount is 0.1 for dodecyl sodium sulfate, ammonium polyacrylate, polyethylene glycol
~0.5%；Binder uses one of polytetrafluoroethylene (PTFE), polyvinyl alcohol, polyurethane, and addition mass fraction amount is 1~5%.
4. a kind of preparation method of graphene-based ceramic composite of high tenacity biomimetic features according to claim 1,
Be characterized in that: prepared graphene slurry in step 1, solvent use water, and graphene solid content is 1~3%；Graphene water
Square to having a size of 5~15 μm, vertical direction is with a thickness of 0.6~1.5nm.
5. a kind of preparation method of graphene-based ceramic composite of high tenacity biomimetic features according to claim 1,
Be characterized in that: set electrostatic field direction is vertical with cryogenic temperature direction in electrostatic field freeze-drying described in step 2,
Electric field strength is 5 × 104~9 × 104V/m；Set unidirectional cryogenic temperature is -70~-10 DEG C, dry pressure is 20~
80Pa。
6. a kind of preparation method of graphene-based ceramic composite of high tenacity biomimetic features according to claim 1,
Be characterized in that: ceramic slurry described in step 1 and graphene slurry are prepared using ball-milling method or sand-blast.
7. a kind of preparation method of graphene-based ceramic composite of high tenacity biomimetic features according to claim 1,
Be characterized in that: inert gas described in step 4 is argon gas.
8. a kind of preparation method of graphene-based ceramic composite of high tenacity biomimetic features according to claim 1,
Be characterized in that: microwave sintering temperature described in step 4 is 1500 DEG C -1700 DEG C.
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| CN111825459B (en) * | 2019-04-23 | 2021-05-18 | 中国科学院金属研究所 | Silicon carbide/graphene bionic composite material for bulletproof armor and preparation method thereof |
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| CN110526695A (en) * | 2019-09-11 | 2019-12-03 | 三峡大学 | A kind of graphene for injection molding/Ceramic Composite particle and preparation method thereof |
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| CN110552129B (en) * | 2019-09-27 | 2022-09-23 | 宁波曙翔新材料股份有限公司 | High-density quartz/quartz composite material and preparation method thereof |
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