KR20130134123A - Boron-doped reduction graphine of adjusting physical properties of semiconductor and electric conductivity, and preparation thereof - Google Patents
Boron-doped reduction graphine of adjusting physical properties of semiconductor and electric conductivity, and preparation thereof Download PDFInfo
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- KR20130134123A KR20130134123A KR1020120057407A KR20120057407A KR20130134123A KR 20130134123 A KR20130134123 A KR 20130134123A KR 1020120057407 A KR1020120057407 A KR 1020120057407A KR 20120057407 A KR20120057407 A KR 20120057407A KR 20130134123 A KR20130134123 A KR 20130134123A
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Abstract
Description
The present invention relates to a reduced graphene doped with a boron dopant adjustable in the semiconductor properties and electrical conductivity and a production method thereof, preferably a mass production method.
Graphene, the hottest issue in the world, is attracting the attention of many researchers because of its new and superior properties since its discovery in 2004. In particular, the Nobel Prize for Physics in 2010 has been awarded to two Nobel Prize winners who have separated the unit graphene for the first time and attract a great deal of interest from researchers worldwide as well as the general public.
Graphene is the thinnest of all known materials, yet it is the strongest and most flexible material, as well as the best able to conduct electricity and heat. To apply graphene effectively, it is a big topic of graphene research to develop a technology capable of mass production of graphene with good quality and control of physical properties and an application device suitable for the physical properties of graphene.
The superior properties of graphene, such as high electron mobility, thermal conductivity, strong mechanical properties, flexibility, and stretchability, can be explained by the peculiar properties of the electrons present therein. So three of four carbon outermost electrons dog that make up the pin is sp 2 hybrid orbital (sp 2 hybrid orbitals) to form the strong covalent bond of one electron rest forms a σ bond is different carbon π bonds in the peripheral It forms a hexagonal honeycomb two-dimensional structure. The band structure of this graphene is very different from that of a general parabolic solid band structure. Graphene is not an insulator in that it is not a metal such as graphite and there is no bandgap because there is no electron density at the Fermi level. The addition of a small amount of charge makes it easy to transform into a conductor, which in this sense has been given the name semi-metal. In addition, unlike common metals, it is known to have bipolar characteristics that can easily change the type of charge carriers depending on how the doping is done.
Meanwhile, in order to apply graphene to electronic devices, there is a demand for a method of precisely controlling charge in a channel region. In the case of organic molecules and alkali metals, the charge is shifted depending on the relative position of the fermi level with the doping element adsorbed on the graphene surface, so that the majority carrier and Efforts are underway to control the concentration.
Recently, as new graphene synthesis methods for large area / mass production have been developed, the applicability to various electronic devices has increased. Many recent studies have reported that a transparent conductive film can be produced by transferring a graphene sheet to a glass film or a plastic film. Such transparent thin films are expected to be used in solar cells or electronic paper, transparent electronic devices, flexible devices.
However, graphene with such various functionalities is difficult to mass-produce due to the poor balance of yield and quality of known production methods. It is known to be unique. Therefore, many researchers have studied the method for the large area of graphene and the methods to control the electrical properties, the most representative of which is to replace the carbon atom with an element such as boron or nitrogen, Doping method by element.
The doping method mainly used until now is the chemical vapor deposition method (CVC) using the most representative metal catalyst. In the above method, graphene is grown by depositing dissolved carbon on the surface using a metal such as a copper thin film having low solubility in carbon as a catalyst, and using this method, a relatively high proportion of single layer graphene is used. It can be synthesized in area and has wide application potential because it is possible to melt the metal catalyst and transfer it to another substrate. In addition, although it has been reported to have a high charge mobility (-4,000 cm 2 / Vs), the chemical vapor deposition method has the disadvantage that all must be manufactured at a very high temperature (~ 1,000 ℃) and vacuum conditions (10 -3 torr), There is a limit to the synthesis of low-cost graphene material.
In addition, studies have been reported to doping during the synthesis of graphene using the arc discharge method of the Republic of Korea. When an electric discharge occurs in the presence of diborane or pyridine, graphene doped with boron and nitrogen can be obtained, respectively. However, after graphene production, a complex purification process is required to obtain high purity.
On the other hand, the closest approach to the two goals of large-scale growth and mass production of graphene is chemical synthesis through oxidation-reduction of graphite. The method of oxidizing graphite has been studied a lot, starting with Brodie in the 19th century, and among them, researchers have used the method proposed by Hummers.
Graphite oxide (graphite oxide) oxidized with strong acid and oxidizing agent has strong hydrophilicity, so that water molecules can be easily inserted between the surfaces, which increases the interplanar spacing to 6 to 12Å It can be easily peeled off using. Since the graphene oxide sheet thus obtained is present in the form of a hydroxyl group and an epoxy group bonded to the surface and a carboxyl group at the edge, most of the graphene oxide sheet loses its inherent properties. However, if graphene oxide is reduced again to remove functional groups including oxygen, it shows similar characteristics to graphene, and researches that can completely remove functional groups through reduction reactions are actively conducted.
A typical reduction method is the exposure of liquid or gaseous hydrazine to graphene oxide (VC Tung et al, Nature Nanotechnology, 2008). In this case, it has been reported that toxic gases are generated during the reduction process and nitrogen atoms are still present. As well as adsorbed on the surface of the pin sheet, there is a disadvantage that the electrical properties are degraded by impurities generated during the reduction process.
In addition to the hydrazine, a number of methods using a reducing agent such as sodium borohydrate (NaBH 4 ), sodium borohydrate (NaBH 4 ), sulfuric acid (H 2 SO 4 ), and the like are known. There are problems such as constraints on the use of silver reducing agents, low efficiency and impurity inclusion.
Another reduction method has been developed using a mixture of iodine and acetic acid to reduce impurities, reduce in the gas phase and liquid phase, and reduce the toxic gas at low temperature. (Korean Patent No. 10-1048490).
The chemical graphene synthesis method has a disadvantage in that the physical properties of the graphene is lower than other methods, but it is easy to functionalize, mass production and large area, and has a big advantage that it is hardly restricted by the type or structure of the substrate. Although research to use is being actively conducted, the process method is not only difficult, but also expensive, and because a small amount of doped graphene is obtained, there is a problem to be widely used in various industrial fields, and thus a new mass synthesis of graphene for commercialization There is a need for a method.
In order to solve the above problems, the present inventors have prepared boron-doped reduced graphene whose semiconductor physical properties and electrical conductivity can be controlled, and not only reduce the cost by simplifying the process method but also enable mass synthesis. The invention was completed.
An object of the present invention is to provide a method for producing reduced graphene that can control the semiconductor properties and electrical conductivity doped boron on the graphene oxide.
In order to achieve the above object, the present invention provides a method of producing reduced graphene, preferably a mass production method, which is capable of controlling the semiconductor properties and electrical conductivity of the boron-doped graphene oxide,
(a) adding boron oxide to graphene oxide to obtain a dispersion;
(b) removing the solvent of the graphene oxide and boron oxide dispersion prepared in step (a) to obtain a solid mixture; And
(c) heat-treating the solid mixture obtained in step (b) to obtain reduced graphene doped with boron; it provides a method for producing boron-doped reduced graphene comprising a.
As a result of measuring the electrical conductivity of the boron-doped reduced graphene according to the present invention, the electrical conductivity is very good, the stability is increased, and p-type characteristics, so that it can be useful as a graphene semiconductor, The manufacturing method of the reduced graphene according to the present invention can be used in the production of graphene semiconductor because it is environmentally friendly, the manufacturing method is reduced by simplifying the process method, mass synthesis is easy, and the semiconductor physical properties and electrical conductivity can be adjusted. ..
1 is a schematic diagram showing a method of producing boron-doped reduced graphene of one embodiment according to the present invention.
Figure 2 is a graph showing the results of the component analysis of boron-doped reduced graphene of one embodiment according to the present invention.
Figure 3 is a graph comparing the electrical conductivity of boron doped reduced graphene and boron doped reduced graphene according to an embodiment of the present invention.
4 is a view showing the output characteristics of the boron-doped reduced graphene of one embodiment according to the present invention.
5 is a view showing the conductivity of boron-doped reduced graphene of one embodiment according to the present invention.
Hereinafter, the present invention will be described in detail.
The present invention provides reduced graphene that can control semiconductor properties and electrical conductivity doped with boron on graphene oxide.
As a result of measuring the electrical conductivity of the boron-doped reduced graphene according to the present invention, it was confirmed that the electrical conductivity increases very well as the heat treatment temperature is increased (Experimental Example 2), and also the reduced graphene according to the present invention. Denotes the p-type characteristic as shown in the output voltage and conduction characteristic graphs (Experimental Example 3). Therefore, the reduced graphene of the present invention can be usefully used as a graphene semiconductor because it is possible to control the semiconductor properties and electrical conductivity.
In addition, the present invention is a method of producing reduced graphene, preferably a mass production method, which can control the semiconductor properties and electrical conductivity doped boron on the graphene oxide,
(a) adding boron oxide to graphene oxide to obtain a dispersion;
(b) removing the solvent of the graphene oxide and boron oxide dispersion prepared in step (a) to obtain a solid mixture; And
(c) heat-treating the solid mixture obtained in step (b) to obtain reduced graphene doped with boron; providing a method for producing boron-doped reduced graphene, including (see FIG. 1 ).
Hereinafter, the manufacturing method according to the present invention will be described in detail.
In the method of producing boron-doped reduced graphene according to the present invention, step (a) is a step of adding boron oxime to graphene oxide and then mixing to obtain a dispersion.
At this time, the content of boron oxide is preferably used more than the graphene oxide content so that boron can be doped to the entire graphene oxide.
On the other hand, the dispersion of the present invention can be mixed using a microwave or ultrasonic waves, but is not limited thereto.
When preparing the dispersion using the microwave or ultrasonic waves, the dispersion of boron oxide and graphene oxide in the dispersion can be increased to uniformly doped boron.
In addition, step (b) is a step of obtaining a solid mixture by removing the solvent of the graphene oxide and boron oxide dispersion obtained in the step (a).
Step (b) is preferably performed immediately after step (a), but is not limited thereto.
At this time, the method of removing the solvent may be lyophilization, reduced pressure filtration, vacuum drying, heat drying, centrifugal concentrator, etc., preferably freeze-drying in liquid nitrogen may be used.
When the solvent is removed by the lyophilization method, the generation of impurities generated during the reduction process may be lowered.
In addition, the step (c) is a step of obtaining the reduced graphene doped with boron by heat-treating the graphene oxide and boron oxide solid mixture obtained in the step (b) under a nitrogen atmosphere.
At this time, the heat treatment temperature is 300 to 1500 ° C, preferably 600 to 1200 ° C.
In the case of outside the above range, in particular, at a temperature of less than 600 ℃ has a problem of low electrical conductivity, and if it exceeds 1200 ℃ there is a problem in that the degradation of the carbon structure is degraded graphene quality.
The heat treatment may be performed in a tube furnace, but is not limited thereto.
Meanwhile, in preparing boron-doped reduced graphene according to the present invention, the graphene oxide used may be purchased and used, and may be prepared using a conventionally known Hummer's method, but not limited thereto. Do not.
The manufacturing method of the reduced graphene according to the present invention can be used in the production of graphene semiconductor because it is environmentally friendly, the manufacturing method is reduced by simplifying the process method, mass synthesis is easy, and the semiconductor physical properties and electrical conductivity can be adjusted. .
Hereinafter, the present invention will be described in detail with reference to Production Examples, Examples and Experimental Examples.
The following Preparation Examples, Examples and Experimental Examples are merely illustrative of the present invention, the present invention is not limited by the following Preparation Examples, Examples and Experimental Examples, the following Preparation Examples, Examples and Experimental Examples are just present invention It is provided to make the disclosure of the present invention complete, and to fully inform the scope of the invention to those skilled in the art.
< Manufacturing example 1> Graphene oxide Produce
23 mL of 98% sulfuric acid was added to 0.85 g of expandable graphite, followed by stirring for 8 hours to insert the graphite. Then, after adding 3 g of potassium permanganate, the mixture was heated and stirred at 36 ° C. for 30 minutes and 70 ° C. for 45 minutes, and 45 mL of distilled water was added thereto, followed by further stirring at 100 ° C. for 30 minutes to perform oxidation. It was. Thereafter, distilled water and hydrogen peroxide were added to terminate the reaction.
5% hydrochloric acid was added to the reaction, washed through centrifugation, and washed twice more with distilled water using centrifugation. The graphite oxide thus obtained was removed impurities by dialysis in distilled water for one week, and then treated with ultrasonic waves to obtain graphene oxide.
< Example 1> Boron Doped restoration Grapina Produce
Step 1: Graphene oxide and Boron oxide Preparation of dispersion
Boron oxide was added to the graphene oxide obtained in Preparation Example 1, followed by mixing using ultrasonic waves to obtain a dispersion of graphene oxide-boron oxide.
Step 2: Graphene oxide and Boron oxide Preparation of Solid Mixture
The mixture of
Step 3: Boron Doped restoration Grapina Produce
The graphene oxide-boron oxide solid mixture obtained in
< Comparative Example 1> Reduced graphene Produce
Except for not adding boron oxide instead of adding boron oxide in
< Experimental Example 1> X-ray Photoelectron spectroscopy Component Analysis
In order to analyze the components of the boron-doped graphene according to the present invention was analyzed by X-ray photoelectron molecular method (XPS). The results are shown in Table 1 and FIG. 2 .
As shown in Table 1 and Figure 2, the graphene according to the present invention was confirmed that the higher the heat treatment temperature is reduced, the lower the proportion of oxygen and the higher the proportion of doped boron (see Figure 2). ).
< Experimental Example 2> Conductivity measurement
The following experiment was performed to compare the electrical conductivity of boron-doped graphene and boron-doped reduced graphene according to the present invention.
Electrical conductivity was measured by a four-point probe method using a current supply meter (Keithley, Model 6280) and a voltmeter (Keithley, Model 2182A). The results are shown in Table 2 and FIG. 3 .
Electrical Conductivity (S / cm)
Electrical Conductivity (S / cm)
As shown in Table 2, in the case of boron doped graphene (Comparative Example 1), it was confirmed that the effect of increasing the electrical conductivity is low, but in the case of boron doped graphene according to the present invention, the heat treatment temperature is Higher electrical conductivity was found to increase very well from about 1 S / cm to 45 S / cm. As a result, it was confirmed that the doping degree of boron affects the electrical conductivity (see FIG. 3 ).
< Experimental Example 3> output characteristics ( output characteristics ) And conduction characteristics ( transfer characteristics measurement
In order to determine the output characteristics and conduction characteristics of boron-doped graphene according to the present invention, the following experiment was performed.
Output and conduction characteristics were measured using an IV analyzer. The results are shown in FIGS . 4 to 5 , respectively.
result
(1) output characteristics
As shown in Figure 4, the boron-doped reduced graphene according to the present invention was confirmed that the slope of the graph is lowered as the output voltage increases from -2v to 2v.
(2) conduction characteristics
As shown in Figure 5, the boron-doped reduced graphene according to the present invention was found to decrease I ds (A) as the V gs (v) value increases.
Therefore, as a result of measuring the electrical conductivity of the boron-doped reduced graphene according to the present invention, the electrical conductivity is very excellent, the stability is increased, and it can be usefully used as a graphene semiconductor because it exhibits p-type characteristics. In addition, the manufacturing method of the reduced graphene according to the present invention is environmentally friendly, the process cost is reduced by simplifying the process method, mass synthesis is easy, and can be useful in the production of graphene semiconductor because it can control the semiconductor properties and electrical conductivity Can be.
Claims (5)
(a) adding boron oxide to graphene oxide to obtain a dispersion;
(b) removing the solvent of the graphene oxide and boron oxide dispersion prepared in step (a) to obtain a solid mixture; And
(c) heat-treating the solid mixture obtained in step (b) to obtain reduced graphene doped with boron; production method of boron-doped reduced graphene comprising a.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103949234A (en) * | 2014-04-23 | 2014-07-30 | 上海荣富新型材料有限公司 | Preparation method of boron-doped graphene/TiO2 nanorod photocatalytic material |
| CN104291329A (en) * | 2014-09-28 | 2015-01-21 | 北京理工大学 | Graphene sponge and preparation method thereof |
| WO2015105861A1 (en) * | 2014-01-08 | 2015-07-16 | Gordon Chiu | A hydrophobic and oleophilic sponge-like compositions |
| CN109835892A (en) * | 2018-12-13 | 2019-06-04 | 华侨大学 | A kind of preparation method of Boron doped semiconductor graphite |
| CN110577210A (en) * | 2018-06-07 | 2019-12-17 | 山东欧铂新材料有限公司 | preparation method of powder of graphene and graphene derivative |
| KR20200087902A (en) * | 2019-01-11 | 2020-07-22 | 전남대학교산학협력단 | Method for producing graphene having uniform nano-sized pores |
| CN114682244A (en) * | 2022-06-01 | 2022-07-01 | 浙江晟格生物科技有限公司 | Recovery method of lactose isomerization composite catalyst |
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2012
- 2012-05-30 KR KR1020120057407A patent/KR20130134123A/en not_active Application Discontinuation
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015105861A1 (en) * | 2014-01-08 | 2015-07-16 | Gordon Chiu | A hydrophobic and oleophilic sponge-like compositions |
| CN103949234A (en) * | 2014-04-23 | 2014-07-30 | 上海荣富新型材料有限公司 | Preparation method of boron-doped graphene/TiO2 nanorod photocatalytic material |
| CN104291329A (en) * | 2014-09-28 | 2015-01-21 | 北京理工大学 | Graphene sponge and preparation method thereof |
| CN110577210A (en) * | 2018-06-07 | 2019-12-17 | 山东欧铂新材料有限公司 | preparation method of powder of graphene and graphene derivative |
| CN110577210B (en) * | 2018-06-07 | 2023-04-25 | 山东欧铂新材料有限公司 | Preparation method of graphene and graphene derivative powder |
| CN109835892A (en) * | 2018-12-13 | 2019-06-04 | 华侨大学 | A kind of preparation method of Boron doped semiconductor graphite |
| KR20200087902A (en) * | 2019-01-11 | 2020-07-22 | 전남대학교산학협력단 | Method for producing graphene having uniform nano-sized pores |
| CN114682244A (en) * | 2022-06-01 | 2022-07-01 | 浙江晟格生物科技有限公司 | Recovery method of lactose isomerization composite catalyst |
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