CN103274394A - Method for preparing graphene by thermal decomposition - Google Patents
Method for preparing graphene by thermal decomposition Download PDFInfo
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- CN103274394A CN103274394A CN2013102242655A CN201310224265A CN103274394A CN 103274394 A CN103274394 A CN 103274394A CN 2013102242655 A CN2013102242655 A CN 2013102242655A CN 201310224265 A CN201310224265 A CN 201310224265A CN 103274394 A CN103274394 A CN 103274394A
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Abstract
The invention discloses a method for directly preparing a graphene powder by the utilization of a thermal decomposition precursor. According to the preparation method, carbohydrate hydrocarbon is used as a carbon source of graphene, and melamine and the like are used as a template. After uniformly mixed, the carbon source and the template react at a certain reaction temperature for a certain reaction time so as to obtain graphene. The mass ratio of the carbon source to the template is preferably within 1:1-1:100. The reaction temperature is preferably within 400-1200 DEG C. The reaction time is preferably within 0.1-24 h. The carbon source is widely selected. The method provided by the invention is used for preparation of graphene, requires simple steps, is easy to operate and is suitable for large-scale industrial production. In addition, the method has advantages of wide sources of the raw materials, high purity of the product, no by-product, no separation and purification technology, environmentally friendly technology and high yield.
Description
Technical field
The invention belongs to the carbon material preparing technical field, relate to the method that a kind of hydrocarbon polymer thermolysis prepares Graphene.
Background technology
Graphene (Graphene) is a kind of carbon material of novel two-dimensional structure, by sp
2Carbon atom is closely arranged the formation honey comb structure, is a kind of simple substance material of carbon of latest find.Graphene is the thinnest, material that physical strength is maximum known today, has good conduction, the capacity of heat transmission and optical property.These premium propertiess of Graphene make it in various fields potential application prospect be arranged, and become the focus of recent investigation of materials.
The research of Graphene and application have proposed an urgent demand to its preparation method.Preparation method of graphene mainly contains micromechanics and peels off methods such as method, thermal expansion graphite method, graphite oxide reduction method and gas chemistry sedimentation at present.Wherein, method peeled off by micromechanics and thermal expansion graphite method efficient is low, output is little, can only be limited to the laboratory small scale experiments; Though the graphite oxide reduction method can prepare in enormous quantities, redox processes is introduced a large amount of defectives, has a strong impact on its physics and chemical property, particularly conductivity; Chemical vapor deposition method complex process, the preparation condition harshness is unsuitable for low cost production in enormous quantities.Therefore, also there is certain difficulty in the large batch of Graphene product of low-cost acquisition at present.
Summary of the invention
The purpose of this invention is to provide a kind of simple to operate, environmental friendliness, transformation efficiency high can be used for the method that large-scale commercial production prepares Graphene.
Graphene preparation method provided by the present invention is that carbon source and template thermal degradation are directly prepared the Graphene powder, may further comprise the steps:
(1) carbon source and template is even according to mass ratio 1:1 to 1:100 ground and mixed;
(2) can to select chemical formulas such as glucose, fructose, maltose be Cn (H to carbon source
2O) saccharide compound of m;
(3) template can be selected the solid chemical compound that can decompose fully after the heating such as trimeric cyanamide, cyanamid dimerization, urea, bicarbonate of ammonia;
(4) carbon source and template are mixed after, be heated to 400-1200 ° of C, react after 0.1-24 hour, be cooled to room temperature and obtain the Graphene product.
The present invention uses saccharide compound to prepare Graphene as carbon source, by analytical procedures such as Raman, XRD, specific surface measurement, transmission electron microscopes, product is characterized, and has proved by present method to prepare the Graphene powder.
The invention provides a kind of method for preparing Graphene, compare with ordinary method, this preparation method has the following advantages:
(1) step is simple, and easy handling is fit to large-scale industrial production;
(2) raw material sources are extensive, can select kind many;
(3) productive rate is higher, and no coupling product does not have the purification step of separation;
(4) reaction conditions is gentle relatively, synthesis under normal pressure, and energy consumption is low.
Description of drawings
Fig. 1 is the Raman spectrogram of the Graphene product of the embodiment of the invention 1 preparation.
Fig. 2 is the XRD spectra of the Graphene product of the embodiment of the invention 1 preparation.
Fig. 3 is the transmission electron microscope photo of the Graphene product of the embodiment of the invention 1 preparation.
Fig. 4 is the Raman spectrogram of the Graphene product of the embodiment of the invention 2 preparations.
Fig. 5 is the XRD spectra of the Graphene product of the embodiment of the invention 2 preparations.
Fig. 6 is the transmission electron microscope photo of the Graphene product of the embodiment of the invention 2 preparations.
Fig. 7 is the Raman spectrogram of the Graphene product of the embodiment of the invention 3 preparations.
Fig. 8 is the XRD spectra of the Graphene product of the embodiment of the invention 3 preparations.
Fig. 9 is the Raman spectrogram of the Graphene product of the embodiment of the invention 4 preparations.
Figure 10 is the XRD spectra of the Graphene product of the embodiment of the invention 4 preparations.
Embodiment
The present invention will be further described below by specific embodiment.
Embodiment 1:
With 1.0 gram glucose and 6.0 gram trimeric cyanamide ground and mixed evenly after, the crucible and put into retort furnace of packing into, temperature programming to 800 ° C reaction 2 hours, reaction finishes the back and is cooled to room temperature naturally, collects product in the crucible.Under these conditions, the output of Graphene is 0.4 gram; The Raman spectrum (see figure 1) shows G peak, D peak and the 2D peak that this sample has grapheme material and has; The nitrogen adsorption analysis shows that its specific surface area is 580m
2/ g illustrates that the Graphene product has bigger specific surface area; From the XRD figure (see figure 2) of product as can be known, product has the diffraction peak of the peculiar broadening of Graphene; Fig. 3 is shown as the transmission electron microscope photo of product, can know and see that the Graphene product is the tulle shape.
Embodiment 2:
With 1.0 gram glucose and 40.0 gram trimeric cyanamide ground and mixed evenly after, the crucible and put into retort furnace of packing into, temperature programming to 800 ° C reaction 2 hours, reaction finishes the back and is cooled to room temperature naturally, collects product in the crucible.Under these conditions, the output of Graphene is 0.2 gram; The Raman spectrum (see figure 4) shows G peak, D peak and the 2D peak that this sample has grapheme material and has; The nitrogen adsorption analysis shows that its specific surface area is 980m
2/ g illustrates that the Graphene product has bigger specific surface area; From the XRD figure (see figure 5) of product as can be known, product has the diffraction peak of the peculiar broadening of Graphene.Fig. 6 is shown as the transmission electron microscope photo of product, can know and see that the Graphene product is the tulle shape.
Embodiment 3:
With 1.0 gram fructose and 6.0 gram trimeric cyanamide ground and mixed evenly after, the crucible and put into retort furnace of packing into, temperature programming to 800 ° C reaction 2 hours, reaction finishes the back and is cooled to room temperature naturally, collects product in the crucible.Under these conditions, the output of Graphene is 0.4 gram; The Raman spectrum (see figure 7) shows that this sample has characteristic peak that grapheme material has; Its specific surface area is 592m
2/ g illustrates that the Graphene product has bigger specific surface area; The XRD figure (see figure 8) of product shows the diffraction peak of the peculiar broadening of Graphene.
Embodiment 4:
With 1.0 gram glucose and 10.0 gram urea ground and mixed evenly after, the crucible and put into retort furnace of packing into, temperature programming to 800 ° C reaction 2 hours, reaction finishes the back and is cooled to room temperature naturally, collects product in the crucible.Under these conditions, the output of Graphene is 0.3 gram; The Raman spectrum (see figure 9) shows G peak, D peak and the 2D peak that this sample has grapheme material and has; Its specific surface area is 520m
2/ g; The XRD figure (see figure 10) shows that product has the diffraction peak of the peculiar broadening of Graphene.
Claims (5)
1. a thermal decomposition method prepares the method for Graphene, it is characterized in that carbon source and template are mixed post-heating by the certain mass ratio decomposes the preparation Graphene.
2. method according to claim 1 is characterized in that carbon source is that chemical formula is Cn (H
2O) saccharide compound of m is as glucose, fructose, maltose etc.
3. method according to claim 1 is characterized in that template is the solid chemical compound that can decompose fully after the heating such as trimeric cyanamide, cyanamid dimerization, urea, bicarbonate of ammonia.
4. method according to claim 1 is characterized in that the mass ratio of carbon source and template is between 1:1-1:100.
5. method according to claim 1, it is characterized in that carbon source and template mix after, be heated to 400-1200 ° of C, react after 0.1-24 hour, be cooled to room temperature and obtain the Graphene product.
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| CN2013102242655A CN103274394A (en) | 2013-06-07 | 2013-06-07 | Method for preparing graphene by thermal decomposition |
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| CN2013102242655A CN103274394A (en) | 2013-06-07 | 2013-06-07 | Method for preparing graphene by thermal decomposition |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103840158A (en) * | 2014-03-21 | 2014-06-04 | 新疆大学 | Preparation method for graphene/molybdenum disulfide composite material |
| CN105621393A (en) * | 2014-11-28 | 2016-06-01 | 中国科学院大连化学物理研究所 | Functionalized graphene material, and preparation method and application thereof |
| CN108117064A (en) * | 2018-03-01 | 2018-06-05 | 上海理工大学 | A kind of preparation method of fold graphene |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674321A (en) * | 2011-03-10 | 2012-09-19 | 中国科学院金属研究所 | Graphene foam with three dimensional fully connected network and macroscopic quantity preparation method thereof |
| WO2013028826A2 (en) * | 2011-08-25 | 2013-02-28 | Wisconsin Alumni Research Foundation | Barrier guided growth of microstructured and nanostructured graphene and graphite |
| CN103086359A (en) * | 2011-11-01 | 2013-05-08 | 海洋王照明科技股份有限公司 | Method for continuously preparing graphene |
-
2013
- 2013-06-07 CN CN2013102242655A patent/CN103274394A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674321A (en) * | 2011-03-10 | 2012-09-19 | 中国科学院金属研究所 | Graphene foam with three dimensional fully connected network and macroscopic quantity preparation method thereof |
| WO2013028826A2 (en) * | 2011-08-25 | 2013-02-28 | Wisconsin Alumni Research Foundation | Barrier guided growth of microstructured and nanostructured graphene and graphite |
| CN103086359A (en) * | 2011-11-01 | 2013-05-08 | 海洋王照明科技股份有限公司 | Method for continuously preparing graphene |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103840158A (en) * | 2014-03-21 | 2014-06-04 | 新疆大学 | Preparation method for graphene/molybdenum disulfide composite material |
| CN105621393A (en) * | 2014-11-28 | 2016-06-01 | 中国科学院大连化学物理研究所 | Functionalized graphene material, and preparation method and application thereof |
| CN108117064A (en) * | 2018-03-01 | 2018-06-05 | 上海理工大学 | A kind of preparation method of fold graphene |
| CN108117064B (en) * | 2018-03-01 | 2021-07-09 | 上海理工大学 | Preparation method of folded graphene |
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Application publication date: 20130904 |