CN112778005A - Graphene porous ceramic and preparation process thereof - Google Patents
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Abstract
The invention provides a graphene porous ceramic which comprises the following raw materials in parts by weight: 35-40 parts of silicon dioxide, 20-25 parts of calcium oxide, 3-5 parts of boron oxide, 5-8 parts of sodium oxide, 8-10 parts of silicon carbide and 25-30 parts of graphene. The invention also provides a preparation process of the graphene porous ceramic, which comprises the following steps: preparing porous pottery, preparing porous graphene, and blowing graphene powder onto the surface of the porous pottery to form the graphene porous pottery. According to the graphene porous ceramic and the preparation process thereof, after the graphene porous ceramic is manufactured, the graphene layer and the ceramic layer are connected more tightly, the phenomenon that the graphene layer falls off is avoided, and the service life of the graphene porous ceramic is guaranteed.
Description
Technical Field
The invention relates to the field of graphene, in particular to graphene porous ceramic and a preparation process thereof.
Background
The graphene has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future. The physicists Andeli Gem and Constantin Nuowuskov of Manchester university in England successfully separate graphene from graphite by a micromechanical stripping method, so that the Nobel prize in 2010 is obtained together, the common powder production methods of graphene are a mechanical stripping method, an oxidation-reduction method and a SiC epitaxial growth method, and the film production method is a Chemical Vapor Deposition (CVD) method. 31 months in 2018, the production line of the first full-automatic mass-production graphene organic solar optoelectronic device in China is started in the lotus in Shandong, the project mainly produces the graphene organic solar cell (called graphene OPV) capable of generating power under weak light, and the three solar power generation problems of application limitation, sensitivity to angle and difficulty in modeling are solved;
graphene porous pottery is an application of graphene, however, most of graphene in the existing graphene porous pottery is directly mixed with porous pottery, so that the performance of graphene and porous pottery is influenced mutually, the application of graphene and porous pottery is not facilitated, and some graphene is adhered to the porous pottery, but the adhesion degree of graphene and porous pottery is not enough, so that the phenomenon that graphene falls off easily occurs along with the lapse of time.
Disclosure of Invention
The invention mainly aims to provide a graphene porous ceramic and a preparation process thereof, which can effectively solve the problems in the prior art.
In order to achieve the purpose, the invention adopts the technical scheme that:
the graphene porous ceramic comprises the following raw materials in parts by weight: 35-40 parts of silicon dioxide, 20-25 parts of calcium oxide, 3-5 parts of boron oxide, 5-8 parts of sodium oxide, 8-10 parts of silicon carbide and 25-30 parts of graphene.
The graphene porous ceramic provided by the invention comprises a ceramic material layer and a graphene layer, wherein the ceramic material layer is a central layer, the graphene layer is a surface layer, and the graphene layer coats the ceramic material layer.
Preferably, the thickness of the ceramic material layer is 5-6 mm, and the thickness of the graphene layer is 2-3 mm.
The invention also aims to provide a preparation method of the graphene porous ceramic, which comprises the following steps:
preparing porous ceramics:
weighing raw materials of silicon dioxide, calcium oxide, boron oxide, sodium oxide and silicon carbide according to a predetermined mass part ratio, mixing and grinding, and sieving with a 300-400-mesh sieve;
adding the sieved powder into a shaping mold, and putting the molding mold into a kiln for calcination to form porous ceramics;
preparing porous graphene:
weighing graphene according to a predetermined mass part, grinding, and sieving with a 200-250 mesh sieve;
chemically treating graphene by a catalytic etching method to form porous graphene powder;
preparing a finished product:
and blowing the signed graphene powder to the surface of the prepared porous ceramic to form the graphene porous ceramic.
Preferably, the calcination in the above steps is a high-temperature hot-pressing sintering process, the sintering temperature is 500-950 ℃, and the calcination pressure is 250-300 kilopascals.
Preferably, the shaping mold in the above step adopts a double-mold inter-engaging structure, and the double molds are a sub mold and a female mold respectively; the surface equidistance of submodule is provided with a plurality of archs, the surface equidistance of master model is provided with a plurality of shrinkage pools, protruding on the submodule with shrinkage pool on the master model corresponds each other, just the arch is less than the diameter of shrinkage pool, bellied length is less than the degree of depth of shrinkage pool.
Preferably, the process conditions of the step of preparing the finished product are as follows: the two-stage high temperature environment comprises a first stage of continuous 3-5 hours at a temperature of 80-200 ℃, and a second stage of continuous 2-3 hours at a temperature of 200-500 ℃.
Preferably, the preparation method of the graphene porous ceramic further comprises a cooling and/or polishing step.
Preferably, the step of cooling is to cool the graphene porous ceramic obtained in the step of preparing the finished product in a sand cooling mode;
preferably, the polishing is to polish the surface of the prepared graphene porous ceramic.
Compared with the prior art, the invention has the following beneficial effects:
the graphene porous ceramic prepared by the invention,
according to the graphene porous ceramic prepared by the method, the plurality of concave holes are formed in the front surface of the ceramic material layer at equal intervals, and the plurality of protrusions are formed in the rear surface at equal intervals, so that after the graphene porous ceramic is manufactured, the graphene layer is connected with the ceramic material layer more tightly, the phenomenon that the graphene layer falls off is avoided, and the service life of the graphene porous ceramic is guaranteed. Simultaneously, because in the preparation process, the surface of submodule is provided with a plurality of archs, and corresponding master model surface is provided with a plurality of shrinkage pools and makes and accomplish the back when graphite alkene porous pottery, demonstrates the form that interlocks each other and overlap, can not influence respective performance each other between graphite alkene layer and the pottery material layer, does benefit to the utilization of graphite alkene porous pottery.
Drawings
Fig. 1 is a process flow diagram for preparing graphene porous ceramics provided by the invention.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1
Weighing raw materials for later use: 350 g of silicon dioxide, 200 g of calcium oxide, 40 g of boron oxide, 50 g of sodium oxide, 100 g of silicon carbide and 300 g of graphene.
Preparing the graphene porous ceramic according to the following steps:
preparing porous ceramics:
mixing and grinding silicon dioxide, calcium oxide, boron oxide, sodium oxide and silicon carbide, and sieving with a 300-400-mesh sieve;
adding the mixed and ground raw materials into a shaping mold, wherein the shaping mold adopts a double-mold mutual clamping structure, the double molds are respectively a sub mold and a female mold, a plurality of bulges are arranged on the surface of the sub mold at equal intervals, a plurality of concave holes are arranged on the surface of the female mold at equal intervals, the bulges on the sub mold correspond to the concave holes on the female mold, the bulges are smaller than the diameters of the concave holes, and the lengths of the bulges are smaller than the depths of the concave holes;
placing the shaping mold added with the raw materials into a kiln to calcine in a high-temperature hot-pressing sintering mode, wherein the sintering temperature is 500-950 ℃, and the calcining pressure is 250-300 Kpa, and forming porous ceramics after calcining;
preparing porous graphene:
grinding graphene, and sieving with a 200-250 mesh sieve;
chemically processing graphene by a catalytic etching method to form porous graphene powder;
preparing a finished product:
blowing the prepared graphene powder to the surface of the prepared porous ceramic in a sectional type high-temperature environment, and carrying out two-stage high-temperature treatment, wherein the first stage lasts for 3-5 hours at the temperature of 80-200 ℃, and the second stage lasts for 2-3 hours at the temperature of 200-500 ℃ to form the graphene porous ceramic.
After the graphene porous ceramic is formed through the steps, cooling and polishing can be performed, wherein the cooling is realized by adopting sandy soil; polishing is to polish the surface of the graphene porous ceramic.
The graphene porous ceramic obtained by the preparation method comprises a ceramic layer and a graphene layer, wherein the ceramic layer is a central layer, and the graphene layer is a surface layer; the thickness of the ceramic layer is about 5mm, and the thickness of the graphene layer is about 2 mm.
Example 2
Weighing raw materials for later use: wherein, the silicon dioxide is 400 g, the calcium oxide is 250 g, the boron oxide is 50 g, the sodium oxide is 80 g, the silicon carbide is 90 g, and the graphene is 250 g.
The specific steps of the method for preparing the graphene porous ceramic from the raw materials are the same as those in example 1, and the thickness of the ceramic layer in the prepared graphene porous ceramic is about 5mm, and the thickness of the graphene layer is about 3 mm.
Example 3
Weighing raw materials for later use: 380 g of silicon dioxide, 240 g of calcium oxide, 35 g of boron oxide, 75 g of sodium oxide, 100 g of silicon carbide and 280 g of graphene.
The specific steps of the method for preparing the graphene porous ceramic from the raw materials are the same as those in example 1, and the thickness of the ceramic layer in the prepared graphene porous ceramic is about 6mm, and the thickness of the graphene layer is about 3 mm.
The compression resistance tests of the graphene porous ceramics prepared in the first embodiment, the second embodiment and the third embodiment show that the graphene porous ceramics prepared in the first embodiment has the strongest compression resistance, and the graphene layer and the ceramic layer are bonded most tightly, so that the service life is longest; the graphene porous ceramic of the second embodiment has good compression resistance, and the graphene layer and the ceramic layer are tightly bonded, so that the service life is long; the third embodiment is weaker in compression resistance than the first embodiment and the second embodiment, the graphene layer and the ceramic layer are relatively loose in adhesion, and the service life is relatively short. The analysis of the material is mainly caused by different proportions of silicon dioxide/calcium oxide in the raw materials of the three porous ceramics, and in the first to third embodiments, the proportions of the silicon dioxide/calcium oxide are respectively 1.75, 1.6 and 1.58, which show a gradually decreasing trend, which shows that the ceramic sintered by the material with high silicon-calcium ratio has high glass phase content, so that the compressive property is good, and the graphene is bonded with the ceramic more firmly.
Meanwhile, compared with the product prepared by the direct mixing or adhering method in the prior art, the graphene porous ceramic material prepared by the method provided by the invention has the advantages that the pressure resistance is improved by more than 20%, and the service life of the product is also improved by more than 30%.
According to the method, the porous graphene powder is blown on the surface of the ceramic material layer in an air blowing mode, so that the uniformity of the graphene layer is higher, the uniformity of the graphene powder is guaranteed, the graphene powder is blown in a two-stage high-temperature environment in a stage-by-stage mode, the blowing environment temperature of the first stage is 80-200 ℃, the blowing environment temperature of the second stage is 200-500 ℃, the fusion of the graphene powder and the ceramic material is tighter, and the quality of the graphene porous ceramic is improved.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The graphene porous ceramic is characterized by comprising the following raw materials in parts by mass:
2. the graphene porous according to claim 1, characterized in that: the graphene porous ceramic comprises a ceramic material layer and a graphene layer, wherein the ceramic material layer is a central layer, the graphene layer is a surface layer, and the graphene layer covers the ceramic material layer.
3. The graphene porous ceramic of claim 1, wherein: the thickness of the pottery material layer is 5-6 mm, and the thickness of the graphene layer is 2-3 mm.
4. The preparation process of the graphene porous ceramic as claimed in claim 1, which is characterized by comprising the following steps: preparing porous ceramics:
weighing raw materials of silicon dioxide, calcium oxide, boron oxide, sodium oxide and silicon carbide according to a predetermined mass part ratio, mixing and grinding, and sieving with a 300-400-mesh sieve;
adding the sieved powder into a shaping mold, and putting the molding mold into a kiln for calcination to form porous ceramics; preparing porous graphene:
weighing graphene according to a predetermined mass part, grinding, and sieving with a 200-250 mesh sieve;
chemically treating graphene by a catalytic etching method to form porous graphene powder; preparing a finished product:
and blowing the prepared graphene powder to the surface of the prepared porous ceramic to form the graphene porous ceramic.
5. The process according to claim 4, characterized in that: the calcination adopts a high-temperature hot-pressing sintering process, the sintering temperature is 500-950 ℃, and the calcination pressure is 250-300 kilopascals.
6. The process according to claim 4, characterized in that: the shaping mold adopts a double-mold mutual clamping structure, and the double molds are a sub mold and a female mold respectively; the surface equidistance of submodule is provided with a plurality of archs, the surface equidistance of master model is provided with a plurality of shrinkage pools, protruding on the submodule with shrinkage pool on the master model corresponds each other, just the arch is less than the diameter of shrinkage pool, bellied length is less than the degree of depth of shrinkage pool.
7. The process according to claim 4, wherein: the process conditions of the step of preparing the finished product are as follows: two-stage high temperature treatment, the first stage is carried out at 80-200 ℃ for 3-5 hours, and the second stage is carried out at 200-500 ℃ for 2-3 hours.
8. The process according to claim 4, wherein: further comprising a cooling or polishing step.
9. The process according to claim 8, wherein: and the cooling is to cool the graphene porous ceramics obtained in the step of preparing the finished product in a sand cooling mode.
10. The process according to claim 8, wherein: and the polishing is to polish the surface of the prepared graphene porous ceramic.
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Address after: 518100 workshop B, No.2, Gongye 3rd road, Langxin community, Shiyan street, Bao'an District, Shenzhen City, Guangdong Province Applicant after: Shenzhen zhuolineng Technology Co.,Ltd. Address before: 518100 the 1st, 2nd, 3rd, 4th and 5th floors of workshop B, No.2, Gongye 3rd road, Langxin community, Shiyan street, Bao'an District, Shenzhen City, Guangdong Province are located in the workshop 4-3 of tongfuyu Industrial Zone, Aiqun Road, Shangwu community, Shiyan street, which is engaged in production and business activities Applicant before: Shenzhen zhuolineng Technology Co.,Ltd. |
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Application publication date: 20210511 |