KR101176544B1 - Grid for transmission electron microscope and manufacturing method thereof - Google Patents

Grid for transmission electron microscope and manufacturing method thereof Download PDF

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KR101176544B1
KR101176544B1 KR20100108341A KR20100108341A KR101176544B1 KR 101176544 B1 KR101176544 B1 KR 101176544B1 KR 20100108341 A KR20100108341 A KR 20100108341A KR 20100108341 A KR20100108341 A KR 20100108341A KR 101176544 B1 KR101176544 B1 KR 101176544B1
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graphene
metal catalyst
transmission electron
graphene film
grid structure
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KR20100108341A
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KR20120046601A (en
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이병주
정구환
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강원대학교산학협력단
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Abstract

Disclosed are a grid structure for transmission electron microscopy and a method of manufacturing the same. A method of manufacturing a grid structure includes forming a metal catalyst on a silicon wafer on which a silicon oxide film is formed, forming a graphene film by synthesizing graphene on the metal catalyst using a thermochemical vapor deposition process, and forming a graphene film from the metal catalyst. Separating the pin film and transferring the graphene film onto the grid mesh.

Description

Grid structure for transmission electron microscopy and its manufacturing method {GRID FOR TRANSMISSION ELECTRON MICROSCOPE AND MANUFACTURING METHOD THEREOF}

The present invention relates to a component used in a transmission electron microscope, and more particularly, to a grid structure for fixing a sample of a transmission electron microscope and a manufacturing method thereof.

An electron microscope is a device that enlarges an object using an electron beam instead of light, and has a much higher resolution and magnification than an optical microscope. In particular, a transmission electron microscope (TEM) can magnify a sample by 1,000 times or more, and can obtain structural information of a sample by using a diffraction pattern.

The sample to be analyzed is fixed on the grid structure. Typically the grid structure consists of a grid mesh woven of metal wires in the form of strings and blades. The spacing between the metal wires should be at least smaller than the diameter of the sample. Therefore, when the sample is a nanometer (nm) scale ultra-fine material, the grid mesh must also be woven at extremely fine intervals corresponding to the size of the sample, which is difficult to manufacture and expensive.

An object of the present invention is to provide a grid structure for transmission electron microscopy and a method of manufacturing the same, which stably supports an ultrafine sample without woven the grid mesh at extremely fine intervals, thereby facilitating observation of the ultrafine sample.

Grid structure for transmission electron microscopy according to an embodiment of the present invention is a grid mesh woven in the form of a grid, a graphene film positioned on the grid mesh to support the sample, and fixed to fix the edges of the grid mesh and graphene film It includes a holder.

The graphene film may include at least one of monolayer graphene, bilayer graphene, and multilayer graphene. At least two of the single layer graphene, the double layer graphene, and the multilayer graphene may be partially present on the graphene film.

In the method of manufacturing a grid structure for transmission electron microscopy according to an embodiment of the present invention, forming a metal catalyst on a silicon wafer on which a silicon oxide film is formed, and forming graphene on the metal catalyst using a thermochemical vapor deposition process. Synthesizing to form a graphene film, separating the graphene film from the metal catalyst, and transferring the graphene film onto the grid mesh.

The metal catalyst may include any one of a nickel (Ni) catalyst formed by electron beam deposition and a copper (Cu) catalyst in the form of a foil.

In the graphene film forming step, the silicon wafer on which the metal catalyst is formed is charged into a quartz tube, the inside of the quartz tube is vacuumed, and a mixed gas of argon (Ar) and hydrogen (H 2 ) is flowed to atmospheric pressure, Graphene may be synthesized by heating the inside of the quartz tube to a synthesis temperature and then inputting a source gas.

The method of manufacturing the grid structure may further include heat treating the metal catalyst before heating to a synthesis temperature and introducing the source gas. Heat treatment of the metal catalyst may be carried out for 5 to 60 minutes at a temperature of 900 ℃ to 1,100 ℃.

Graphene may be synthesized for 1 to 30 minutes at a synthesis temperature of 900 ℃ to 1,100 ℃. In the graphene synthesis, the source gas is methane (CH 4 ), and methane (CH 4 ) gas and hydrogen (H 2) gas may be introduced at a flow rate of 1 sccm to 30 sccm: 1500 sccm.

The method of manufacturing the grid structure may further include cooling the silicon wafer, the metal catalyst, and the graphene film after graphene synthesis. Argon (Ar) gas is injected into the quartz tube in the cooling step, the cooling rate may be 2 ℃ / min to 8 ℃ / min.

In the graphene film separation step, the silicon oxide film may be etched to separate the silicon wafer from the graphene film and the metal catalyst, and the graphene film may be left by removing the metal catalyst using an etchant of the metal catalyst.

In the transferring of the graphene film, the graphene film floating in the etchant of the metal catalyst may be collected and transferred onto the grid mesh.

In the present invention, by using a graphene film as a sample support instead of the grid mesh, it is possible to prevent the nanometer (nm) scale ultra-fine sample from escaping between the grid mesh, and to maintain the focal plane to maintain an accurate focal plane High resolution images of fine samples can be obtained.

1 is an exploded perspective view of a grid structure for transmission electron microscope observation according to an embodiment of the present invention.
Figure 2 is a perspective view of the bonded state of the grid structure for transmission electron microscopy according to an embodiment of the present invention.
3A to 3D are schematic perspective views illustrating a manufacturing process of the grid structure shown in FIG. 1.
Figure 4 is a graph showing the Raman spectrum measurement results of the graphene film of the completed grid structure according to an embodiment of the present invention.
5 is a transmission electron micrograph showing a graphene film of a grid structure manufactured according to an embodiment of the present invention.
FIG. 6 is a transmission electron micrograph showing a state where carbon nanotubes are disposed on the graphene film shown in FIG. 5.
7 is a transmission electron micrograph of a comparative example showing a state where carbon nanotubes are disposed on an amorphous carbon film.

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings so that those skilled in the art may easily implement the present invention. The present invention may be embodied in many different forms and is not limited to the embodiments described herein.

1 and 2 are an exploded perspective view and a coupled perspective view of a grid structure for transmission electron microscopy according to an embodiment of the present invention, respectively.

1 and 2, the grid structure 100 for transmission electron microscopy according to the present embodiment includes a grid mesh 10, a graphene film 20 positioned on the grid mesh 10, and a grid mesh 10. ) And a fixing holder 30 fixing the edge of the graphene film 20. The sample to be observed is disposed on the graphene film 20.

Graphene is a 0.35 nm thick two-dimensional film composed of a single layer of carbon atoms, which form a honeycomb structure in which carbon is connected like a net. Such graphene has high electrical and thermal conductivity, and mechanical strength is more than 200 times that of steel. In addition, graphene has good elasticity and does not lose its electrical conductivity when stretched or folded, and is chemically very stable.

The graphene film 20 includes at least one of single layer graphene, double layer graphene, and multilayer graphene, and at least two of the single layer graphene, the double layer graphene, and the multilayer graphene may be formed on the graphene film 20 according to the synthesis conditions. May be partially present. Since the graphene film 20 implements a large mechanical strength even at an extremely thin thickness, the graphene film 20 can stably support a sample to be observed, and can easily support an ultrafine sample having a nanometer (nm) scale without further processing.

The grid mesh 10 functions to support the graphene film 20 and the sample thereon. Since the actual sample is supported by the graphene film 20, the grid mesh 10 is installed at the minimum interval that the graphene film 20 can maintain flatness without sagging. The grid mesh 10 may be a structure in which a metal wire is woven in a lattice form, and has a sparse spacing structure having a wide spacing irrespective of the size of the sample.

In the grid structure 100 of the present exemplary embodiment, the graphene film 20 is used as the sample support instead of the grid mesh 10, thereby preventing the nanometer (nm) scale microscopic sample from escaping between the grid meshes 10. High resolution images of very fine samples can be obtained by maintaining an accurate focal plane.

The ultrafine sample on the nanometer (nm) scale may be carbon nanotubes, semiconductor nanowires, metal nanoparticles, or metal oxide nanoparticles. In addition, the ultrafine sample may be a biological material such as linear virus or particulate protein. The ultra-fine sample of the nanometer (nm) scale does not pass through the carbon net of the graphene film 20 and is thus stably placed on the graphene film 20.

The graphene film 20 may be synthesized on a silicon wafer on which a metal catalyst is formed, and then transferred onto the grid mesh 10 by the transfer method described below to form the grid structure 100. The grid structure 100 does not have to be manufactured at minute intervals to fit the grid mesh 10 to the sample size, and can easily analyze ultra-fine samples such as carbon nanotubes disposed on the graphene film 20 at high resolution. .

Next, the manufacturing method of the grid structure 100 is demonstrated.

3A to 3D are schematic perspective views illustrating a manufacturing process of the grid structure shown in FIG. 1.

Referring to FIG. 3A, a metal catalyst 50 is formed on a silicon wafer 40 on which a silicon oxide film is formed. The metal catalyst 50 may be a nickel (Ni) catalyst having a thickness of approximately 300 nm, and is formed by an electron beam (E-beam) deposition method. On the other hand, as the metal catalyst 50, a copper (Cu) foil of approximately 10 mu m thickness may be used.

Referring to FIG. 3B, the graphene film 20 is synthesized on the metal catalyst 50 using a thermal chemical vapor deposition facility.

To this end, the silicon wafer 40 on which the metal catalyst 50 is formed is placed in a quartz tube (not shown) of the thermochemical vapor deposition apparatus, and the base pressure is set to 5 × 10 −2 Torr to create a vacuum state. Subsequently, a mixed gas of argon (Ar) and hydrogen (H 2 ) is flowed to bring the pressure in the quartz tube to atmospheric pressure. At this time, the flow rate of argon (Ar) gas and hydrogen (H 2 ) gas may be 500sccm. Then, the temperature is raised to 20 ° C./min in the same atmosphere and heated to a synthesis temperature of 900 ° C. to 1,100 ° C., for example 1,000 ° C.

After reaching the synthesis temperature, the graphene film 20 is formed by synthesizing graphene for 1 minute to 30 minutes, for example, 5 minutes after the heat treatment step for 5 minutes to 60 minutes, for example, 30 minutes under the same conditions. Metal catalyst 50 in the heat treatment step varies with the polycrystalline thin film having excellent crystallinity, graphene synthesis of the raw material gas of methane (CH 4) to hydrogen (H 2) with a gas 1sccm to 30sccm: 1,500sccm, e.g. 5sccm The flow rate is 1,500 sccm.

When the graphene synthesis is completed, the silicon wafer 40, the metal catalyst 50, and the graphene film 20 are cooled. In this case, argon (Ar) gas is cooled by flowing 50 sccm, and a cooling rate may be 2 ° C./min to 8 ° C./min.

In the graphene synthesis process, the synthesis temperature, the synthesis time, and the ratio of methane (CH 4 ) and hydrogen (H 2 ) serve as the main variables for determining the number of layers of graphene to be synthesized. And the cooling rate also graphene in the composite single-layer and two-ply Yes acts as a synthesis parameter that can control the coverage of the pin. So if the synthesis temperature of pinmak 20 is less than 900 ℃ methane (CH 4) the thermal decomposition difficult of Graphene may not be synthesized or the graphene film 20 may be synthesized only on a portion of the metal catalyst 50. On the other hand, when the synthesis temperature of the graphene film 20 exceeds 1,100 ° C., the carbon solubility of the metal catalyst 50 may be increased, and thus, multilayer graphene having a large number of layers may be synthesized as a whole, and the process cost due to high temperature is increased.

If the metal catalyst 50 is not heat-treated or the heat treatment time of the metal catalyst 50 is less than 5 minutes, the grain size of the metal catalyst 50 is reduced, and the domain size of the graphene film 20 to be synthesized is also reduced. On the other hand, when the heat treatment time of the metal catalyst 50 exceeds 60 minutes, the polycrystalline thin film efficiency of the metal catalyst 50 does not increase, but only the process cost due to the high temperature is increased.

When the synthesis time of the graphene film 20 is less than 1 minute and the flow rate of methane (CH 4 ), which is a raw material gas, is smaller than the above range, the graphene film 20 may not be synthesized or may be synthesized only on a part of the metal catalyst 50. have. On the other hand, when the synthesis time of the graphene film 20 exceeds 30 minutes or the flow rate of methane (CH 4 ), the raw material gas, exceeds the above range, most of the graphene film 20 is formed of multi-layered graphene having a large number of layers to maintain high temperature. The process cost increases.

The cooling rate is related to the surface diffusion of the carbon atoms deposited on the metal catalyst 50 upon cooling. The deposited carbon atoms form partly multilayer graphene through surface diffusion, and form single or two layer graphene around the multilayer graphene. The proper cooling rate is a variable that maximizes the coverage of monolayer graphene. When the cooling rate is less than 2 ° C./min, the carbon atoms may move to the grain boundary of the metal catalyst 50 through surface diffusion, such that the graphene film 20 may not be synthesized. On the other hand, if the cooling rate exceeds 8 ℃ / min it is difficult to diffuse the surface of the carbon atoms can be reduced the area of the single layer or two-layer graphene film 20.

The graphene film 20 synthesized by the thermal chemical vapor deposition method as described above can control the coverage of each region to some extent according to the synthesis conditions, but partially monolayer graphene, bilayer graphene, and multilayers throughout the graphene film 20. Graphene can all be present. In the graphene film 20, both single layer graphene, double layer graphene, and multilayer graphene have no functional difference in supporting the sample.

Referring to FIG. 3C, the silicon oxide layer on the silicon wafer 40 is removed using a silicon oxide etchant. As the silicon oxide etching solution, a solution of potassium hydroxide (KOH) at 75 ° C. and 3 mol may be used. When the silicon oxide film is removed, the silicon wafer 40 is separated from the metal catalyst 50 and the graphene film 20.

The graphene film 20 is separated by etching the metal catalyst 50 using the metal catalyst etchant. In the case of the metal catalyst 50 formed of nickel (Ni), 1 mol of iron chloride (FeCl 3 ) solution may be used as the metal catalyst etchant. The graphene film 20 floats on the metal catalyst etchant. The graphene film 20 is floated and separated from the metal catalyst etch, and then transferred onto the grid mesh 10 (see FIG. 1). Through the above-described process, the grid structure 100 shown in FIGS. 1 and 2 is completed.

4 is a graph showing the Raman spectrum measurement results of the graphene film of the completed grid structure. Raman analysis is one of the analysis techniques that can distinguish the number of layers of graphene, referring to FIG. 4, it can be seen that single layer graphene and double layer graphene exist in the synthesized graphene film.

FIG 1,350cm -1 in the graph 4, 1,600cm -1, 2,700cm were three major peaks occur near 1, it is called a D-band, respectively, G-band, and G '(2D) band.

The D band is a peak due to sp3 type carbon bonds and is related to defects such as amorphous carbon or broken carbon-carbon bonds that may be present in carbon bodies such as carbon nanotubes and graphene. The G band is the peak associated with molecular vibrations between the carbon-carbon bonds of the carbon bodies with sp2 bonds. The G 'band is a peak due to secondary scattering in which two D-band phonons are emitted in an overtone of the D-band (2nd harmonic mode) .In the case of single-layer graphene, a single Lorentzian profile has a sharp left-right symmetrical shape Peaks appear.

In addition, the number of layers of graphene can be predicted from the intensity ratio of the G band and G 'band peaks. In the single layer graphene, the intensity of the G 'band peak appears higher than the G band peak, and the difference decreases as the number of layers increases. In the case of the multilayer graphene, the intensity of the G band peak is greater than that of the G' band peak.

5 is a transmission electron microscope (TEM) picture of a graphene film of the grid structure manufactured according to the above-described process, and FIG. 6 is a transmission electron microscope (TEM) showing a state where carbon nanotubes are disposed on the graphene film shown in FIG. 5. ) Photo. FIG. 7 is a transmission electron microscope (TEM) image showing a state where carbon nanotubes are disposed on an amorphous carbon film instead of a graphene film as a comparative example of the present embodiment.

6 and 7, a sharper, higher resolution image may be obtained in an embodiment in which carbon nanotubes are disposed on a graphene film (FIG. 6) than in a comparative example in which carbon nanotubes are disposed on an amorphous carbon film (FIG. 7). It can be confirmed. This difference in performance applies equally not only to carbon nanotubes, but also to all ultrafine samples on the nanometer (nm) scale.

While the present invention has been described in connection with what is presently considered to be practical exemplary embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, Of course.

100: grid structure 10: grid mesh
20: graphene film 30: fixed holder
40: silicon wafer 50: metal catalyst

Claims (14)

A grid structure mounted on a transmission electron microscope to support a sample to be observed,
Grid mesh woven in grid form;
A graphene film positioned on the grid mesh to support the sample; And
Fixed holder for fixing the edge of the grid mesh and the graphene film
Including,
The graphene film grid structure for transmission electron microscopy comprising at least one of a single layer graphene, two-layer graphene and multilayer graphene. delete The method of claim 1,
A grid structure for transmission electron microscopy in which at least two of the single layer graphene, the double layer graphene, and the multilayer graphene are partially present on the graphene film. Forming a metal catalyst on a silicon wafer on which a silicon oxide film is formed;
Forming a graphene film by synthesizing graphene on the metal catalyst using a thermochemical vapor deposition process;
Separating the graphene film from the metal catalyst; And
Transferring the graphene film onto a grid mesh
Method for producing a grid structure for transmission electron microscope observation comprising a. The method of claim 4, wherein
The metal catalyst is a method of manufacturing a grid structure for transmission electron microscopy comprising any one of a nickel (Ni) catalyst formed by an electron beam deposition method and a copper (Cu) catalyst in the form of a foil. The method of claim 4, wherein
In the graphene film forming step,
Charging the silicon wafer on which the metal catalyst was formed into a quartz tube,
After making the inside of the quartz tube in a vacuum state and flowing a mixed gas of argon (Ar) and hydrogen (H 2 ) to make an atmospheric pressure,
A method of manufacturing a grid structure for transmission electron microscopy, wherein the inside of the quartz tube is heated to a synthesis temperature, and then source gas is synthesized to synthesize the graphene. The method of claim 6,
A method of manufacturing a grid structure for transmission electron microscopy, further comprising the step of heat-treating the metal catalyst before heating to the synthesis temperature and introducing the source gas. The method of claim 7, wherein
The heat treatment of the metal catalyst is a method for producing a grid structure for transmission electron microscope observation is carried out for 5 to 60 minutes at a temperature of 900 ℃ to 1,100 ℃. The method of claim 6,
The graphene is a method for producing a grid structure for transmission electron microscopy is synthesized for 1 to 30 minutes at a synthesis temperature of 900 ℃ to 1,100 ℃. 10. The method of claim 9,
In the graphene synthesis, the raw material gas is methane (CH 4 ), and the methane (CH 4 ) gas and hydrogen (H 2 ) gas are injected at a flow rate of 1 sccm to 30 sccm: 1500 sccm. Way. The method of claim 6,
And cooling the silicon wafer, the metal catalyst, and the graphene film after the graphene synthesis. The method of claim 11,
Argon (Ar) gas is injected into the quartz tube in the cooling step, the cooling rate is 2 ℃ / min to 8 ℃ / min manufacturing method of the grid structure for transmission electron microscope observation. The method of claim 4, wherein
In the graphene membrane separation step,
Etching the silicon oxide film to separate the silicon wafer from the graphene film and the metal catalyst;
A method of manufacturing a grid structure for transmission electron microscopic observation, leaving the graphene film by removing the metal catalyst using an etchant of the metal catalyst. The method of claim 13,
In the step of transferring the graphene film,
A method for manufacturing a grid structure for transmission electron microscopy to collect the graphene film suspended in the etchant of the metal catalyst and to transfer it onto the grid mesh.
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WO2021256886A1 (en) * 2020-06-18 2021-12-23 한국화학연구원 Conductive substrate and method for analyzing analyte using same
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