CN110482864A - A kind of doped graphite ene-type glass ceramics additive and preparation method thereof - Google Patents
A kind of doped graphite ene-type glass ceramics additive and preparation method thereof Download PDFInfo
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- CN110482864A CN110482864A CN201910880928.6A CN201910880928A CN110482864A CN 110482864 A CN110482864 A CN 110482864A CN 201910880928 A CN201910880928 A CN 201910880928A CN 110482864 A CN110482864 A CN 110482864A
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- glass ceramics
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
- C03C14/004—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of particles or flakes
Abstract
The invention discloses a kind of doped graphite ene-type glass ceramics additives and preparation method thereof, belong to glass ceramics technical field.A kind of doped graphite ene-type glass ceramics additive, including following raw materials according: ZrO2, graphene, Sb2O3、CeO2And ethyl alcohol, wherein ZrO2: Sb2O3: CeO2: graphene=1~2:1:2~3:3~5, ethyl alcohol are added by 8~10 times of remaining raw material.The present invention is using graphene as raw material, chemical modification preparation glass ceramics additive is carried out to it, this glass additive raw material uses wet grinding grinding and mixing, graphene is changed into graphene oxide to be coated on other inorganic material surfaces using hydro-thermal reaction, become porous material using vacuum drying, being ground into fine powder improves its specific surface area, to be conducive to improve the mechanical property and stability of glass ceramics, so that glass ceramics has a extensive future.
Description
Technical field
The invention belongs to glass ceramics technical fields, and in particular to a kind of doped graphite ene-type glass ceramics additive and its
Preparation method.
Background technique
Glass ceramics, be by high temperature melt, molding, heat treatment and what manufactured a kind of crystal phase was combined with glass phase answer
There is condensation material high mechanical strength, thermal expansion to form the superiority such as adjustable, heat shock resistance, resistant to chemical etching, low-dielectric loss
Can, it is widely used in the fields such as machine-building, electronics and microelectronics, chemistry, industry and building.But domestic glass ceramics produces work
Skill there are qualities it is poor, yield rate is low the problems such as.
Graphene is one kind by sp2The two-dimentional monoatomic layer structure that carbon atom is constituted with honeycomb lattice has tough, steady
Calmly, many advantages, such as good conductivity, high thermal conductivity, it is widely used in electronics industry and military field.
Patent application CN105271759A provides a kind of preparation method of glass ceramics, and this method is by graphene oxide
Mix after crushing with acrylic resin, alcohols, carbonized under inert atmosphere, first carbon microspheres, then by carbon microspheres be added it is other at
Water quenching obtains devitrified glass at glass particle after after heating three times after dividing melting.The preparation method is micro- with the charcoal of preparation
Ball is that subsequent devitrified glass makes one of raw material, and glass ceramics additive of the invention is as devitrified glass production raw material aspect
Research report not yet disclose at present；Simultaneously additive of the invention for glass ceramics production can substantially improve its stability and
Related mechanical property.
Summary of the invention
Based on above-mentioned problem, the present invention provides a kind of doped graphite ene-type glass ceramics additive and its preparation side
Method carries out chemical modification preparation glass ceramics additive, to it using graphene as raw material so as to improve the mechanical property of glass ceramics
Energy and stability.
The technical solution adopted by the invention is as follows:
A kind of doped graphite ene-type glass ceramics additive, including following raw materials according: ZrO2, graphene, Sb2O3、CeO2And second
Alcohol, wherein ZrO2: Sb2O3: CeO2: graphene=1~2:1:2~3:3~5, ethyl alcohol are added by 8~10 times of remaining raw material.
Further, a kind of doped graphite ene-type glass ceramics additive, including following raw materials according: ZrO2, graphite
Alkene, Sb2O3、CeO2And ethyl alcohol, wherein ZrO2: Sb2O3: CeO2: graphene=2:1:3:5, ethyl alcohol by remaining raw material 10 extraordinarily
Enter.
A kind of preparation method of doped graphite ene-type glass ceramics additive, including the following steps:
S1, by graphene, ZrO2、Sb2O3、CeO2, ethyl alcohol be added in ball mill in the ratio and carry out wet-milling for 24 hours, obtain
Mixed liquor；
S2, it the mixed liquor is put into ptfe autoclave carries out hydro-thermal reaction；
S3, to S2 after, gains are centrifuged at a high speed, must be precipitated, by sediment progress vacuum refrigeration do
Dry, grinding crosses 400 meshes to get glass ceramics additive.
Further, the hydrothermal temperature is 120~180 DEG C, the reaction time 16~for 24 hours.
Further, the high-speed separation rate is 8000rpm.
In conclusion by adopting the above-described technical solution, the beneficial effects of the present invention are: the present invention provides a kind of doping
Graphite ene-type glass ceramics additive and preparation method thereof carries out chemical modification to it and prepares glass pottery using graphene as raw material
Porcelain additive, this glass additive raw material use wet grinding grinding and mixing, graphene are changed into oxidation using hydro-thermal reaction
Graphene becomes porous material to be coated on other inorganic material surfaces, using vacuum drying, is ground into fine powder and changes
It is apt to its specific surface area, to be conducive to improve the mechanical property and stability of glass ceramics, so that the application prospect of glass ceramics
It is wide.
Specific embodiment
Embodiment of the present invention can be replaced by the difference of specific range based on the above technical solution,
Available numerous embodiment, therefore, several embodiments as described below are only merely the more excellent reality in numerous embodiment
Example is applied, any technology replacement done in above-mentioned technical proposal all belongs to the scope of protection of the present invention.
Embodiment 1
A kind of doped graphite ene-type glass ceramics additive, including following raw materials according: ZrO2, graphene, Sb2O3、CeO2And second
Alcohol, wherein ZrO2: Sb2O3: CeO2: graphene=2:1:3:5, ethyl alcohol are added by 10 times of remaining raw material.
A kind of preparation method of doped graphite ene-type glass ceramics additive, including the following steps:
S1, by graphene, ZrO2、Sb2O3、CeO2, ethyl alcohol be added in ball mill in the ratio and carry out wet-milling for 24 hours, obtain
Mixed liquor；
S2, it the mixed liquor is put into ptfe autoclave carries out hydro-thermal reaction, hydrothermal temperature 160
DEG C, reaction time 20h；
S3, to S2 after, by gains carry out high speed 8000rpm centrifuge separation, must precipitate, sediment is subjected to vacuum
Freeze-drying, grinding cross 400 meshes to get glass ceramics additive.
Embodiment 2
A kind of doped graphite ene-type glass ceramics additive, including following raw materials according: ZrO2, graphene, Sb2O3、CeO2And second
Alcohol, wherein ZrO2: Sb2O3: CeO2: graphene=1:1:2:3, ethyl alcohol are added by 8 times of remaining raw material.
A kind of preparation method of doped graphite ene-type glass ceramics additive, including the following steps:
S1, by graphene, ZrO2、Sb2O3、CeO2, ethyl alcohol be added in ball mill in the ratio and carry out wet-milling for 24 hours, obtain
Mixed liquor；
S2, it the mixed liquor is put into ptfe autoclave carries out hydro-thermal reaction, hydrothermal temperature 120
DEG C, reaction time 16h；
S3, to S2 after, by gains carry out high speed 8000rpm centrifuge separation, must precipitate, sediment is subjected to vacuum
Freeze-drying, grinding cross 400 meshes to get glass ceramics additive.
Embodiment 3
A kind of doped graphite ene-type glass ceramics additive, including following raw materials according: ZrO2, graphene, Sb2O3、CeO2And second
Alcohol, wherein ZrO2: Sb2O3: CeO2: graphene=1.5:1:2.5:4, ethyl alcohol are added by 9 times of remaining raw material.
A kind of preparation method of doped graphite ene-type glass ceramics additive, including the following steps:
S1, by graphene, ZrO2、Sb2O3、CeO2, ethyl alcohol be added in ball mill in the ratio and carry out wet-milling for 24 hours, obtain
Mixed liquor；
S2, it the mixed liquor is put into ptfe autoclave carries out hydro-thermal reaction, hydrothermal temperature 150
DEG C, reaction time 18h；
S3, to S2 after, by gains carry out high speed 8000rpm centrifuge separation, must precipitate, sediment is subjected to vacuum
Freeze-drying, grinding cross 400 meshes to get glass ceramics additive.
Embodiment 4
A kind of doped graphite ene-type glass ceramics additive, including following raw materials according: ZrO2, graphene, Sb2O3、CeO2And second
Alcohol, wherein ZrO2: Sb2O3: CeO2: graphene=1:1:2:3, ethyl alcohol are added by 8 times of remaining raw material.
A kind of preparation method of doped graphite ene-type glass ceramics additive, including the following steps:
S1, by graphene, ZrO2、Sb2O3、CeO2, ethyl alcohol be added in ball mill in the ratio and carry out wet-milling for 24 hours, obtain
Mixed liquor；
S2, it the mixed liquor is put into ptfe autoclave carries out hydro-thermal reaction, hydrothermal temperature 180
DEG C, the reaction time is for 24 hours；
S3, to S2 after, by gains carry out high speed 8000rpm centrifuge separation, must precipitate, sediment is subjected to vacuum
Freeze-drying, grinding cross 400 meshes to get glass ceramics additive.
Embodiment 5
A kind of doped graphite ene-type glass ceramics additive, including following raw materials according: ZrO2, graphene, Sb2O3、CeO2And second
Alcohol, wherein ZrO2: Sb2O3: CeO2: graphene=2:1:3:5, ethyl alcohol are added by 8 times of remaining raw material.
A kind of preparation method of doped graphite ene-type glass ceramics additive, including the following steps:
S1, by graphene, ZrO2、Sb2O3、CeO2, ethyl alcohol be added in ball mill in the ratio and carry out wet-milling for 24 hours, obtain
Mixed liquor；
S2, it the mixed liquor is put into ptfe autoclave carries out hydro-thermal reaction, hydrothermal temperature 180
DEG C, the reaction time is for 24 hours；
S3, to S2 after, by gains carry out high speed 8000rpm centrifuge separation, must precipitate, sediment is subjected to vacuum
Freeze-drying, grinding cross 400 meshes to get glass ceramics additive.
Embodiment 6
Glass ceramics additive is with embodiment 1, the glass ceramics additive and SiO that will be prepared2、Al2O3Co2O3With 2:5:
The ratio of 1.5:1 first melts after-pouring and forms to obtain glass ceramics.Melting process is divided into three sections: 4h is kept the temperature at 1350 DEG C of first segment,
Second segment is warming up to 1450 DEG C of heat preservation 1.5h, and third section is warming up to 1580 DEG C of heat preservation 2h after-pouring moldings.
Embodiment 7
With embodiment 6, the difference is that: glass ceramics additive is the same as embodiment 2.
Embodiment 8
With embodiment 6, the difference is that: glass ceramics additive is the same as embodiment 3.
Embodiment 9
With embodiment 6, the difference is that: glass ceramics additive is the same as embodiment 4.
Embodiment 10
With embodiment 6, the difference is that: glass ceramics additive is the same as embodiment 5.
Comparative example 1
With embodiment 6, the difference is that, no glass ceramics additive.
Comparative example 2
With embodiment 6, the difference is that, participation of the glass ceramics additive without graphene.
Correlated performance test is carried out to glass ceramics obtained by embodiment and comparative example, the results are shown in Table 1.
1 the performance test results of table
The invention is not limited to specific embodiments above-mentioned.The present invention, which expands to, any in the present specification to be disclosed
New feature or any new combination, and disclose any new method or process the step of or any new combination.
Claims (5)
1. a kind of doped graphite ene-type glass ceramics additive, which is characterized in that including following raw materials according:
ZrO2, graphene, Sb2O3、CeO2And ethyl alcohol, wherein ZrO2: Sb2O3: CeO2: graphene=1~2:1:2~3:3~5,
Ethyl alcohol is added by 8~10 times of remaining raw material.
2. a kind of doped graphite ene-type glass ceramics additive as described in claim 1, which is characterized in that including following original
Material: ZrO2, graphene, Sb2O3、CeO2And ethyl alcohol, wherein ZrO2: Sb2O3: CeO2: graphene=2:1:3:5, ethyl alcohol press remaining
10 times of additions of raw material.
3. a kind of preparation method of doped graphite ene-type glass ceramics additive as claimed in claim 1 or 2, feature exist
In, including the following steps:
S1, by graphene, ZrO2、Sb2O3、CeO2, ethyl alcohol be added in ball mill in the ratio and carry out wet-milling for 24 hours, must mix
Liquid；
S2, it the mixed liquor is put into ptfe autoclave carries out hydro-thermal reaction；
S3, to S2 after, gains are centrifuged at a high speed, must be precipitated, by sediment carry out vacuum freeze drying, grind
Mill crosses 400 meshes to get glass ceramics additive.
4. a kind of preparation method of doped graphite ene-type glass ceramics additive as claimed in claim 3, which is characterized in that institute
Stating hydrothermal temperature is 120~180 DEG C, the reaction time 16~for 24 hours.
5. a kind of preparation method of doped graphite ene-type glass ceramics additive as claimed in claim 3, which is characterized in that institute
Stating high-speed separation rate is 8000rpm.
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| CN201910880928.6A CN110482864A (en) | 2019-09-18 | 2019-09-18 | A kind of doped graphite ene-type glass ceramics additive and preparation method thereof |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140158906A1 (en) * | 2012-12-06 | 2014-06-12 | Charles Hillel Rosendorf | Method and equipment for quantum vacuum energy extraction |
| CN105084769A (en) * | 2014-05-08 | 2015-11-25 | 海南大学 | Preparation method of graphene/quartz glass block |
| CN105271759A (en) * | 2015-09-30 | 2016-01-27 | 江苏耀兴安全玻璃有限公司 | Preparation method of glass ceramic |
| ES2597157A1 (en) * | 2015-06-09 | 2017-01-16 | Consejo Superior De Investigaciones Científicas (Csic) | Graphene hybrid materials and coatings (Machine-translation by Google Translate, not legally binding) |
| CN107129156A (en) * | 2017-06-06 | 2017-09-05 | 广东环境保护工程职业学院 | A kind of graphene devitrified glass and preparation method thereof |
| CN108164149A (en) * | 2018-01-16 | 2018-06-15 | 王明国 | A kind of glass ceramics for adulterating graphene oxide and preparation method thereof |
-
2019
- 2019-09-18 CN CN201910880928.6A patent/CN110482864A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140158906A1 (en) * | 2012-12-06 | 2014-06-12 | Charles Hillel Rosendorf | Method and equipment for quantum vacuum energy extraction |
| CN105084769A (en) * | 2014-05-08 | 2015-11-25 | 海南大学 | Preparation method of graphene/quartz glass block |
| ES2597157A1 (en) * | 2015-06-09 | 2017-01-16 | Consejo Superior De Investigaciones Científicas (Csic) | Graphene hybrid materials and coatings (Machine-translation by Google Translate, not legally binding) |
| CN105271759A (en) * | 2015-09-30 | 2016-01-27 | 江苏耀兴安全玻璃有限公司 | Preparation method of glass ceramic |
| CN107129156A (en) * | 2017-06-06 | 2017-09-05 | 广东环境保护工程职业学院 | A kind of graphene devitrified glass and preparation method thereof |
| CN108164149A (en) * | 2018-01-16 | 2018-06-15 | 王明国 | A kind of glass ceramics for adulterating graphene oxide and preparation method thereof |
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