KR20170107736A - Synthetic method for graphene composites and nonomethal using graphene oxide - Google Patents
Synthetic method for graphene composites and nonomethal using graphene oxide Download PDFInfo
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- KR20170107736A KR20170107736A KR1020160031434A KR20160031434A KR20170107736A KR 20170107736 A KR20170107736 A KR 20170107736A KR 1020160031434 A KR1020160031434 A KR 1020160031434A KR 20160031434 A KR20160031434 A KR 20160031434A KR 20170107736 A KR20170107736 A KR 20170107736A
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- C—CHEMISTRY; METALLURGY
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- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/145—After-treatment of oxides or hydroxides, e.g. pulverising, drying, decreasing the acidity
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The present invention relates to a method of manufacturing a nano metal and a method of manufacturing a graphene composite, which comprises mixing and dispersing a nano metal oxide in a liquid phase graphene oxide, drying the mixture, and a thermal reduction step, Thereby solving the problem of aggregation of particles.
In addition, the nanomaterial manufacturing method according to the present invention can produce a composite of nanomaterial and graphene together.
Description
The present invention relates to a method for producing a graphene composite using graphene oxide and a method for producing a nano metal. More particularly, the present invention relates to a method for producing a nano-metal oxide composite powder by mixing and drying a nano-metal oxide and a liquid-phase graphene oxide dispersion to prepare a nano-metal oxide composite powder coated with a graphene oxide and heat- .
Because of its physical and chemical properties, nanometals have been widely applied in the fields of electronics, optics, catalysts and biotechnology. However, as the size of the metal powder decreases, the surface energy increases and the powder becomes unstable. When stored in air, the surface continuously oxidizes or spontaneously ignites. Therefore, various researches have been conducted in order to manufacture a nano-sized metal powder having a large activity and effectively treat the produced powder without contamination.
The most important factor in the production of nano-metal powders is to produce powders of uniform purity of high purity. Physical production methods such as mechanical pulverization for pulverizing bulk metals, chemical production methods such as liquid phase reduction method in which a precipitant or a reducing agent is added to metal salts . However, the conventional chemical manufacturing method has a problem in that the process is very complicated or the yield is very low, and a new manufacturing method has been required.
There is a one-pot synthesis method using a polymer represented by polyvinylpyrrolidone (PVP) as a method of simplifying the kind and process of a chemical substance. However, when the nanoparticle is manufactured at a high temperature, There is a problem in that the yield is low due to aggregation in order to obtain stability, and there is a problem that the polymer melts at a high temperature and becomes fluid, resulting in a tendency of agglomeration among the particles.
Korean Patent Laid-Open Publication No. 2003-0030729 provides a method of forming a metal-surfactant complex by reacting a metal precursor with a surfactant and decomposing the complex at a high temperature to produce uniform metal and alloy nanoparticles. There is a problem that the time is long and the yield is low.
On the other hand, as a conventional reduction method of metals, there is a iron ore cutting process as part of a process capable of mass production. The ironmaking process is a process of making pig iron by removing iron oxide from iron ore by burning coke in blast furnace. The coke is a heat source that dissolves iron ore, which is a compound of iron and oxygen, in the blast furnace, It plays a role.
More specifically, the coke is burned by the hot air flowing into the bottom of the blast furnace, and the carbon monoxide (CO) generated in the process is reduced to iron ore to produce molten iron. In this process, the coke plays a role as a heat source for melting iron ore And iron oxide which is iron oxide.
The inventors of the present invention have focused on the reduction method of the above-mentioned manufacturing process and have studied a method of reducing metal oxides at a temperature lower than that of coke using graphene oxide. In addition to simplifying the manufacturing process of nano metal powder, So that the present invention has been accomplished.
The present invention provides a method for producing a nano-metal by preparing a nano-metal oxide composite powder coated with a graphene oxide so that the metal oxide can be reduced at a low temperature, The purpose.
It is still another object of the present invention to provide a method for producing a graphene composite by preparing the graphene oxide-coated nano-metal oxide composite powder and reducing the graphene oxide.
In order to accomplish the object of the present invention, there is provided a method of manufacturing a semiconductor device, comprising: preparing a nano-metal oxide; Mixing and dispersing the nano-metal oxide in a liquid phase graphene oxide dispersion; Drying the mixture to produce a nano-metal oxide composite powder coated with graphene oxide; And reducing the oxygen of the nano-metal oxide by heat-treating the composite powder under reducing conditions; And a method for manufacturing the nano metal.
The nano-metal oxide may have an average diameter of 5 to 10 nm, and the nano-metal oxide may be any one of a transition metal oxide, a transition metal oxide, and an alloy.
The graphene oxide is contained in a weight ratio of 0.01 to 10% with respect to the nano-metal oxide composite powder, and the heat treatment temperature is 200 to 1,500 ° C or less.
The present invention also relates to a process for preparing a liquid crystalline graphene oxide dispersion comprising mixing and dispersing a nanocrystal oxide and a liquid phase graphene oxide dispersion; Drying the mixture to produce a nano-metal oxide composite powder coated with graphene oxide; And heat treating the composite powder to reduce the graphene oxide; Wherein the grains of the nano-metal oxide have a particle size of 5 to 100 nm and the heat treatment temperature is 200 to 1,500 ° C. The present invention also provides a method for producing graphene composites containing graphene.
According to the nano-metal manufacturing method and the graphene composite manufacturing method of the present invention, it is possible not only to simplify the manufacturing process of the nano-metal, but also to solve the nano-particle agglomeration problem in the polymer-based reduction method.
Further, it is possible to provide a method of further obtaining a graphene composite in which metal oxides can be reduced at a temperature lower than that of using coke or graphite, and the coating properties of nanoparticles are complemented through graphene coating.
FIG. 1 is a flowchart illustrating a method of manufacturing a nano metal and a method of manufacturing a graphene composite according to an embodiment of the present invention. Referring to FIG.
Hereinafter, a method of manufacturing a nano metal and a method of manufacturing a graphene composite according to a preferred embodiment of the present invention will be described in detail with reference to the accompanying drawings.
FIG. 1 is a flow chart showing a method of manufacturing a nano metal and a method of manufacturing a graphene composite according to an embodiment of the present invention, wherein a nano metal oxide and a liquid graphene oxide dispersion are prepared (S110) (S120), and the mixture is dried to produce a nano-metal oxide composite powder coated with a graphene oxide (S130). The composite powder is heat-treated under reducing conditions to produce oxygen of the nano- Reduction or graphene oxide is reduced (S140).
In the step of preparing the nano-metal oxide and the liquid-phase graphene oxide dispersion (S110), the nano-metal oxide may be in the form of a powder, and the graphene oxide may be in the form of a slurry dispersed in water.
The nano-metal oxide may be any of the nano-metal oxides to be reduced. However, the nano-metal oxide may be any one selected from the group consisting of transition metal oxides, transition metal oxides, and alloys containing metal ions suitable for thermal reduction or chemical reduction do.
In addition, the nano-metal oxide may have a different diameter depending on the purpose of the nano-metal to be produced, but preferably has an average diameter of 5 to 100 nm. When the average diameter is less than 5 nm, the activity of the powder is high and stable reaction is difficult. When the average diameter is more than 100 nm, there is a problem that the utilization of the produced nanometal is lowered.
The graphene oxide is thermodynamically stable as compared with graphene composed only of carbon, becomes hydrophilic through oxygen functional groups, and can be mass-produced in a stable dispersion form. In addition, reducing agents and high heat can be treated to remove oxygen functional groups. Therefore, it is prepared as a liquid phase dispersed in water to enable stable reaction.
The graphene oxide may be prepared by a modified Hummers method, a Hummers method, a Brodie method, a Hofman & Frenzel method, a Hamdi method, or a Staus method. In the present embodiment, the Modified Hummers method is used. Specifically, 50 g of micro graphite powder and 40 g of NaNO 3 are placed in a 200 mL H 2 SO 4 solution, and while cooling, 250 g of KMnO 4 is slowly added over 1 hour. Then slowly add 5 L of 4-7 % H 2 SO 4 over 1 hour and add H 2 O 2 . The precipitate was then centrifuged and washed with 3% H 2 SO 4 - 0.5% H 2 O 2 And washed with distilled water, a yellowish brown graphene oxide aqueous solution is obtained.
The nano-metal oxide prepared in the liquid phase graphene oxide dispersion is mixed and dispersed (S120). The dispersion method of the mixture may be any method as long as the particles can be dispersed evenly. Preferably, the dispersion method is a ball milling method, A dispersion method, a sink mixer method, a mixer method, and a stirling method.
Wherein the gravimetric weight ratio of the graphene oxide is 0.01 to 10% by weight of the nano-metal oxide and the graphene oxide composite. When it is less than 0.01%, the nano-metal oxide can not be sufficiently reduced, and when it exceeds 10%, there is a problem that the economical efficiency is deteriorated.
The dispersed mixture is prepared as a nano-metal oxide composite coated with graphene oxide through a drying process (S130). The nano-metal oxide powder is coated with graphene oxide and is produced as a composite powder. The drying process may be any one as long as it does not cause other chemical reactions including thermal drying, hot air drying, and the like.
The nano-metal oxide composite powder coated with the prepared graphene oxide is heat-treated at a reducing condition (S140) to produce a nano-metal in which the nano-metal oxide is reduced through thermal reduction, or to produce a graphene composite in which graphene oxide is reduced do.
If the temperature is lower than 200 ° C., the reduction reaction will not occur. If the temperature is higher than 1500 ° C., the nano-metal oxide may aggregate due to melting of the nano-metal oxide.
In the reduction reaction, the carbon of the graphene oxide is consumed and the oxygen atom of the metal oxide is easily dropped, so that the metal oxide is reduced. Also, as the graphene oxide is reduced under the heating condition, the graphene oxide-coated nano-metal oxide composite can be produced as a graphene-coated graphene composite.
In the preparation of the graphene composite, a graphene complex can be formed by a reaction with the hydrophilic group or the adsorbed water on the surface of the graphene oxide. Thus, it is possible to produce a composite in combination with various solvents other than the aqueous solvent Do.
Although the present invention has been described in detail with reference to the above embodiments, it is needless to say that the present invention is not limited to the above-described embodiments, and various modifications may be made without departing from the spirit of the present invention.
Claims (6)
Mixing and dispersing the nano-metal oxide in a liquid phase graphene oxide dispersion;
Drying the mixture to produce a nano-metal oxide composite powder coated with graphene oxide; And
Subjecting the composite powder to heat treatment under reducing conditions to reduce oxygen of the nano-metal oxide; ≪ / RTI >
Drying the mixture to produce a nano-metal oxide composite powder coated with graphene oxide; And
Heat treating the composite powder to reduce graphene oxide; A graphene-containing graphene composite manufacturing method comprising:
Wherein the particles of the nano-metal oxide are 5 to 100 nm and the heat treatment temperature is 200 to 1,500 ° C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102011800B1 (en) | 2018-04-18 | 2019-08-19 | 주식회사 크레진 | Manufacturing method for nano-sized magnetic graphene powder composite |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102011800B1 (en) | 2018-04-18 | 2019-08-19 | 주식회사 크레진 | Manufacturing method for nano-sized magnetic graphene powder composite |
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