CN104478458B - A kind of preparation method of Graphene ball toughness reinforcing SiCN pottery - Google Patents
A kind of preparation method of Graphene ball toughness reinforcing SiCN pottery Download PDFInfo
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Abstract
The preparation method of a kind of Graphene ball toughness reinforcing SiCN pottery, relates to SiCN ceramic preparation.1) prepare graphene oxide dehydrated alcohol dispersion liquid: joined by ethanol solution in graphene oxide, container closure, then container is put into ultrasonic disperse in ultrasonic machine, obtain graphene oxide dehydrated alcohol dispersion liquid；2) mixed solution of graphene oxide dehydrated alcohol dispersion liquid and polysilazane is prepared: in polysilazane solution, add step 1) gained graphene oxide dehydrated alcohol dispersion liquid, add cumyl peroxide, container closure, then stirring, ultrasonic, obtain the mixed solution of graphene oxide dehydrated alcohol dispersion liquid and polysilazane；3) Graphene ball toughness reinforcing SiCN pottery is prepared: by step 2) gained mixed solution carries out heat cross-linking in an inert atmosphere; flaxen liquid is made to become the polysilazane solid of black; clay into power again, and be hot pressed into biscuit, more i.e. obtain product after being pyrolyzed under inert gas shielding by biscuit.
Description
Technical field
The present invention relates to SiCN ceramic preparation, especially relate to the preparation method of a kind of Graphene ball toughness reinforcing SiCN pottery.
Background technology
The SiCN pottery utilizing the pyrolysis preparation of polymer precursor polysilazane has the excellences such as high temperature resistant, corrosion-resistant, antioxidation
Performance, and preparation technology is easy, it is strong to design, forming temperature is low, but intensity and hardness are the most relatively low, thus limits SiCN
Pottery application in the presence of a harsh environment.Graphene is a kind of with carbon atom SP2Hybrid orbital composition hexagon is the list of honeycomb lattice
The new material of lamellar structure, is the thinnest, the hardest the most known nano material.Therefore, Graphene is studied in recent years
Personnel apply the mechanical performance improving material widely.
Research currently, with respect to Graphene ball was only reported on the document and patent of minority.Such as: Chinese patent
CN103121672A uses electrostatic spraying processes through electrostatic spray process, Graphene precursor solution to be formed microspheroidal drop, then
Described microspheroidal drop is inputted solidification liquid by the method collected by wet method, prepares Graphene microsphere.Simply report a kind of Graphene
The preparation method of microsphere, the method preparation process is complicated, also fails to apply in practice.
How while Graphene ball preparation method is prepared in simplification Graphene ball be applied to SiCN pottery toughness reinforcing in improve
The mechanical performance of SiCN pottery, has not yet to see.
Summary of the invention
It is an object of the invention to provide preparation process simple, compressive property, a kind of Graphene ball of reduction fragility can be significantly improved
The preparation method of toughness reinforcing SiCN pottery.
The present invention comprises the following steps:
1) graphene oxide dehydrated alcohol dispersion liquid is prepared
Ethanol solution is joined in graphene oxide, container closure, then container is put into ultrasonic disperse in ultrasonic machine,
To graphene oxide dehydrated alcohol dispersion liquid；
2) mixed solution of graphene oxide dehydrated alcohol dispersion liquid and polysilazane is prepared
Step 1 is added in polysilazane solution) gained graphene oxide dehydrated alcohol dispersion liquid, add peroxidating diisopropyl
Benzene (DCP), container closure, then stirring, ultrasonic, obtain the mixing of graphene oxide dehydrated alcohol dispersion liquid and polysilazane
Solution；
3) Graphene ball toughness reinforcing SiCN pottery is prepared
By step 2) gained mixed solution carries out heat cross-linking in an inert atmosphere, makes flaxen liquid become the poly-silicon nitrogen of black
Alkane solid, then clays into power, and is hot pressed into biscuit, then obtains amorphous stone after being pyrolyzed under inert gas shielding by biscuit
The composite ceramics that ink alkene ball is ceramic with SiCN, the most described Graphene ball toughness reinforcing SiCN pottery.
In step 1) in, described graphene oxide is preferably single-layer graphene oxide；The power of described ultrasonic disperse can be 220～
250W；The time of described ultrasonic disperse can be 1～2h；Graphene oxide in described graphene oxide dehydrated alcohol dispersion liquid with
The proportioning of ethanol solution can be (0.5～2) mg: 1ml, and wherein, graphene oxide is calculated by mass, ethanol solution
In terms of volume；Preferably 1mg: 1ml.
In step 2) in, in described mixed solution, in mass ratio, the ratio of polysilazane content and graphene oxide content can
Being 1: (0.1～1), polysilazane can be 1 with the ratio of cumyl peroxide: (0.002～0.004)；Described stirring time
Between can be 1～2h；The described ultrasonic time can be 30～60min.
In step 3) in, described inert atmosphere can use nitrogen or argon；Described heat cross-linking temperature can be 160～450 DEG C；Institute
Stating Ball-milling Time can be 30～60min；The temperature of described hot pressing can be 50～100 DEG C, and the pressure of hot pressing can be 10～20MPa；
The temperature of described pyrolysis can be 1000～1500 DEG C, and pyrolysis time can be 1～8h.
Compare with prior art, present invention have the advantage that
The present invention is with SiCN pottery as parent phase, and Graphene ball is for strengthening phase.Do not changing SiCN and Graphene network structure
Under premise, SiCN pottery and Graphene ball is made to be combined by high temperature sintering.Mechanism is: be uniformly embedded into by Graphene ball
In SiCN network structure, using Graphene ball as strengthening phase.The compressive property of SiCN pottery can be improved, reduce fragility.This
Bright raw materials used wide material sources, easily obtain.Preparation method, condition are the simplest.Course of reaction is easily controllable, and ceramic yield is high.
The Graphene ball toughness reinforcing SiCN pottery of preparation is higher than SiCN ceramic hardness, and wearability is good.
Accompanying drawing explanation
Fig. 1 is the SEM photograph (1000 times) of the Graphene ball toughness reinforcing SiCN pottery section prepared by the embodiment of the present invention 1.
Fig. 2 is the SEM photograph (3000 times) of the Graphene ball toughness reinforcing SiCN pottery section prepared by the embodiment of the present invention 1.
Detailed description of the invention
The present invention will be further described to combine accompanying drawing by the following examples.
Embodiment 1
The present embodiment prepares Graphene ball toughness reinforcing SiCN pottery, comprises the following steps:
1, by beaker respectively with deionized water and dehydrated alcohol ultrasonic cleaning 2 times, dry.It is the electronic balance of 0.1mg by precision
Weigh the graphene oxide of 5mg in beaker.Measure 5ml dehydrated alcohol in beaker with graduated cylinder, seal rapidly.Put into ultrasonic
Obtaining graphene oxide dehydrated alcohol dispersion liquid A with the power ultrasonic 30min of 220W in cleaning machine, concentration is 1mg/ml.
2, with electronic balance weighing 3g polysilazane in beaker, measure 1ml dispersion liquid A with graduated cylinder and join polysilazane
In liquid, stir 30min, obtain mixed solution B.
3, mixed solution B is joined in the container that masking foil folds, put in tube furnace, cross-link in the atmosphere of nitrogen.
Crosslinking temperature is 300 DEG C, and heating rate is 0.5 DEG C/min, obtains black solid after crosslinking curing.
4, black solid pulverizer is broken into powder, with electronic balance weighing 2g powder, puts into ball milling in agate jar
30min.The powder obtained crosses 250 mesh sieves.
5, adding in hot pressing die with electronic balance weighing 0.2mg powder, temperature is 80 DEG C, and pressure is 15MPa.Justified
Shape biscuit of ceramics.
6, biscuit of ceramics sheet is sintered.Spread, at clean corundum crucible inner bottom part, the powder that a little ball milling is good, then will press
Biscuit of ceramics sheet put in crucible, then crucible put in high temperature process furnances be sintered, in high-purity N2With 0.5 under atmosphere
DEG C/programming rate of min, from room, progressively temperature rise, to 800 DEG C, naturally cools to room temperature after 800 DEG C of insulation 4h, obtains brown
Ceramic disks.
7, the ceramic disks obtained is annealed.High temperature process furnances is sintered, high-purity N2With 0.5 DEG C/min under atmosphere
Programming rate, rise to 1000 DEG C from room temperature, 1000 DEG C insulation 4h after naturally cool to room temperature, finally give black ceramic circle
Sheet, i.e. Graphene ball toughness reinforcing SiCN pottery.
The Graphene ball toughness reinforcing SiCN Ceramic manufacturing obtained is become standard sample, by the Young's modulus of dynamic method test sample.Its
Young's modulus is 110GPa, and the Young's modulus not adding the SiCN pottery of Graphene is 75GPa.Equally, Graphene ball increases
The hardness of tough SiCN pottery is 10.6GPa, and the SiCN ceramic hardness being not added with Graphene is 9.5GPa.Young's modulus and hardness
Improve mainly due to Graphene ball be embedded in uniformly SiCN pottery network structure in (seeing Fig. 1), make Young's modulus and
Hardness increases.
Embodiment 2
The present embodiment prepares Graphene ball toughness reinforcing SiCN pottery, comprises the following steps:
1, by beaker respectively with deionized water and dehydrated alcohol ultrasonic cleaning 2 times, dry.It is the electronic balance of 0.1mg by precision
Weigh the graphene oxide of 10mg in beaker.Measure 5ml dehydrated alcohol in beaker with graduated cylinder, seal rapidly.Put into super
Obtaining graphene oxide dehydrated alcohol dispersion liquid A with the power ultrasonic 30min of 220W in sound cleaning machine, concentration is 2mg/ml.
2, with electronic balance weighing 3g polysilazane in beaker, measure 1ml dispersion liquid A with graduated cylinder and join polysilazane
In liquid, stir 1h, ultrasonic 30min, obtain mixed solution B.
3, mixed solution B is joined in the container that masking foil folds, put in tube furnace, cross-link in the atmosphere of nitrogen.
Crosslinking temperature is 300 DEG C, and heating rate is 0.5 DEG C/min, obtains black solid after crosslinking.
4, black solid pulverizer is broken into powder, with electronic balance weighing 2g powder, puts into ball milling in agate jar
30min.The powder obtained crosses 250 mesh sieves.
5, adding in hot pressing die with electronic balance weighing 0.2mg powder, temperature is 80 DEG C, and pressure is 15MPa.Justified
Shape biscuit of ceramics.
6, biscuit of ceramics sheet is sintered.Bottom clean corundum crucible, spread the powder that a little ball milling is good, then will press
Biscuit of ceramics sheet is put in crucible, then is put in high temperature process furnances by crucible and be sintered, in high-purity N2With 0.5 DEG C/min under atmosphere
Programming rate, from room temperature progressively temperature rise to 800 DEG C, 800 DEG C insulation 4h after naturally cool to room temperature, obtain brown pottery
Disk.
7, the ceramic disks obtained is annealed.High temperature process furnances is sintered, high-purity N2With 0.5 DEG C/min under atmosphere
Programming rate, rise to 1000 DEG C from room temperature, 1000 DEG C insulation 4h after naturally cool to room temperature, finally give amorphous state black
Ceramic disks, i.e. Graphene ball toughness reinforcing SiCN pottery.
The Graphene ball toughness reinforcing SiCN Ceramic manufacturing obtained is become standard sample, by the Young's modulus of dynamic method test sample.Its
Young's modulus is 119GPa, and the Young's modulus not adding the SiCN pottery of Graphene is 75GPa.Equally, with Graphene ball
The hardness of compound SiCN pottery is 14.7GPa, and the SiCN ceramic hardness being not added with Graphene is 9.5GPa.Same Young mould
The raising of amount and hardness is embedded in the network structure of SiCN pottery (seeing Fig. 2) mainly due to, Graphene ball uniformly,
Young's modulus and hardness is made to increase.
Embodiment 3
The present embodiment prepares Graphene ball toughness reinforcing SiCN pottery, comprises the following steps:
1, by beaker respectively with deionized water and dehydrated alcohol ultrasonic cleaning 2 times, dry.It is the electronic balance of 0.1mg by precision
Weigh the graphene oxide of 10mg in beaker.Measure 5ml dehydrated alcohol in beaker with graduated cylinder, seal rapidly.Put into super
Obtaining graphene oxide dehydrated alcohol dispersion liquid A with the power ultrasonic 30min of 220W in sound cleaning machine, concentration is 2mg/ml.
2, with electronic balance weighing 3g polysilazane in beaker, measure 1ml dispersion liquid A with graduated cylinder and join polysilazane
In liquid, stir 1h, ultrasonic 30min, obtain mixed solution B.
3, mixed solution B is joined in the container that masking foil folds, put in tube furnace, cross-link in the atmosphere of nitrogen.
Crosslinking temperature is 400 DEG C, and heating rate is 0.5 DEG C/min, obtains black solid after crosslinking.
4, black solid pulverizer is broken into powder, with electronic balance weighing 2g powder, puts into ball milling in agate jar
30min.The powder obtained crosses 250 mesh sieves.
5, adding in hot pressing die with electronic balance weighing 0.2mg powder, temperature is 100 DEG C, pressure 15MPa.Obtain circle
Biscuit of ceramics.
6, biscuit of ceramics sheet is sintered.Bottom clean corundum crucible, spread the powder that a little ball milling is good, then will press
Biscuit of ceramics sheet is put in crucible, then is put in high temperature process furnances by crucible and be sintered, in high-purity N2With 0.5 DEG C/min under atmosphere
Programming rate, from room temperature progressively temperature rise to 800 DEG C, 800 DEG C insulation 4h after naturally cool to room temperature, obtain brown pottery
Disk.
7, the ceramic disks obtained is annealed.High temperature process furnances is sintered, high-purity N2With 0.5 DEG C/min under atmosphere
Programming rate, rise to 1100 DEG C from room temperature, 1100 DEG C insulation 4h after naturally cool to room temperature, finally give amorphous state black
Ceramic disks, i.e. Graphene ball toughness reinforcing SiCN pottery.
Embodiment 4
The present embodiment prepares Graphene ball toughness reinforcing SiCN pottery, comprises the following steps:
1, by beaker respectively with deionized water and dehydrated alcohol ultrasonic cleaning 2 times, dry.It is the electronic balance of 0.1mg by precision
Weigh the graphene oxide of 5mg in beaker.Measure 5ml dehydrated alcohol in beaker with graduated cylinder, seal rapidly.Put into ultrasonic
Obtaining graphene oxide dehydrated alcohol dispersion liquid A with the power ultrasonic 30min of 230W in cleaning machine, concentration is 1mg/ml.
2, with electronic balance weighing 3g polysilazane in beaker, measure 1ml dispersion liquid A with graduated cylinder and join polysilazane
In liquid, stir 1h, ultrasonic 1h, obtain mixed solution B.
3, mixed solution B is joined in the container that masking foil folds, put in tube furnace, cross-link in the atmosphere of nitrogen.
Crosslinking temperature is 400 DEG C, and heating rate is 0.5 DEG C/min, obtains black solid after crosslinking.
4, black solid pulverizer is broken into powder, with electronic balance weighing 2g powder, puts into ball milling in agate jar
30min.The powder obtained crosses 250 mesh sieves.
5, adding in hot pressing die with electronic balance weighing 0.2mg powder, temperature is 100 DEG C, pressure 10MPa.Obtain circle
Biscuit of ceramics.
6, biscuit of ceramics sheet is sintered.Bottom clean corundum crucible, spread the powder that a little ball milling is good, then will press
Biscuit of ceramics sheet is put in crucible, then is put in high temperature process furnances by crucible and be sintered, in high-purity N2With 0.5 DEG C/min under atmosphere
Programming rate, from room temperature progressively temperature rise to 800 DEG C, 800 DEG C insulation 4h after naturally cool to room temperature, obtain brown pottery
Disk.
7, the ceramic disks obtained is annealed.High temperature process furnances is sintered, high-purity N2With 0.5 DEG C/min under atmosphere
Programming rate, rise to 1000 DEG C from room temperature, 1000 DEG C insulation 4h after naturally cool to room temperature, finally give amorphous state black
Ceramic disks, i.e. Graphene ball toughness reinforcing SiCN pottery.
Claims (10)
1. the preparation method of a Graphene ball toughness reinforcing SiCN pottery, it is characterised in that comprise the following steps:
1) graphene oxide dehydrated alcohol dispersion liquid is prepared
Ethanol solution is joined in graphene oxide, container closure, then container is put into ultrasonic disperse in ultrasonic machine, obtain graphene oxide dehydrated alcohol dispersion liquid；
2) mixed solution of graphene oxide dehydrated alcohol dispersion liquid and polysilazane is prepared
Step 1 is added in polysilazane solution) gained graphene oxide dehydrated alcohol dispersion liquid, add cumyl peroxide, container closure, then stirring, ultrasonic, obtain the mixed solution of graphene oxide dehydrated alcohol dispersion liquid and polysilazane；
3) Graphene ball toughness reinforcing SiCN pottery is prepared
By step 2) gained mixed solution carries out heat cross-linking in an inert atmosphere; flaxen liquid is made to become the polysilazane solid of black; then clay into power; and it is hot pressed into biscuit; the composite ceramics of amorphous Graphene ball and SiCN pottery, the most described Graphene ball toughness reinforcing SiCN pottery is obtained after being pyrolyzed under inert gas shielding by biscuit again.
The preparation method of a kind of toughness reinforcing SiCN of Graphene ball the most as claimed in claim 1 pottery, it is characterised in that in step 1) in, described graphene oxide is single-layer graphene oxide.
The preparation method of a kind of toughness reinforcing SiCN of Graphene ball the most as claimed in claim 1 pottery, it is characterised in that in step 1) in, the power of described ultrasonic disperse is 220～250W；The time of described ultrasonic disperse is 1～2h.
The preparation method of a kind of toughness reinforcing SiCN of Graphene ball the most as claimed in claim 1 pottery, it is characterized in that, in step 1) in, graphene oxide in described graphene oxide dehydrated alcohol dispersion liquid is (0.5～2) mg: 1mL with the proportioning of ethanol solution, wherein, graphene oxide is calculated by mass, and ethanol solution is in terms of volume.
The preparation method of a kind of toughness reinforcing SiCN of Graphene ball the most as claimed in claim 4 pottery, it is characterized in that, graphene oxide in described graphene oxide dehydrated alcohol dispersion liquid is 1mg: 1mL with the proportioning of ethanol solution, wherein, graphene oxide is calculated by mass, and ethanol solution is in terms of volume.
The preparation method of a kind of toughness reinforcing SiCN of Graphene ball the most as claimed in claim 1 pottery, it is characterized in that, in step 2) in, in described mixed solution, in mass ratio, polysilazane content is 1 with the ratio of graphene oxide content: (0.1～1), and polysilazane is 1 with the ratio of cumyl peroxide: (0.002～0.004).
The preparation method of a kind of toughness reinforcing SiCN of Graphene ball the most as claimed in claim 1 pottery, it is characterised in that in step 2) in, the time of described stirring is 1～2h；The described ultrasonic time is 30～60min.
The preparation method of a kind of toughness reinforcing SiCN of Graphene ball the most as claimed in claim 1 pottery, it is characterised in that in step 3) in, described inert atmosphere uses nitrogen or argon.
The preparation method of a kind of toughness reinforcing SiCN of Graphene ball the most as claimed in claim 1 pottery, it is characterised in that in step 3) in, described heat cross-linking temperature is 160～450 DEG C；Described claying into power is clayed into power for ball, and Ball-milling Time is 30～60min.
The preparation method of a kind of toughness reinforcing SiCN of Graphene ball the most as claimed in claim 1 pottery, it is characterised in that in step 3) in, the temperature of described hot pressing is 50～100 DEG C, and the pressure of hot pressing is 10～20MPa；The temperature of described pyrolysis is 1000～1500 DEG C, and pyrolysis time is 1～8h.
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| CN104944960B (en) * | 2015-07-01 | 2017-05-24 | 山东大学 | Method for preparing ferric acetylacetonate-containing silicon carbonitride ceramic by precursor conversion method |
| CN105732064A (en) * | 2016-02-24 | 2016-07-06 | 厦门大学 | Method for preparing cylindrical graphene reinforced SiCN ceramic temperature sensor |
| CN105801152B (en) * | 2016-02-24 | 2019-01-29 | 厦门大学 | Square graphite alkene enhances SiCN ceramic temperature sensor and preparation method thereof |
| CN107056284B (en) * | 2017-02-28 | 2020-06-23 | 安徽拓吉泰新型陶瓷科技有限公司 | Zirconia ceramic mobile phone backboard and preparation method thereof |
| CN108387141B (en) * | 2018-03-06 | 2020-08-18 | 绍兴文理学院 | Preparation method of composite bulletproof ceramic plate |
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| CN103288466B (en) * | 2013-03-08 | 2014-08-20 | 西北工业大学 | Preparation method of in-situ synthesized carbon nano-tube modified SiCN ceramic matrix composite material |
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