KR101529510B1 - Apparatus and method for formation of nanowire - Google Patents

Apparatus and method for formation of nanowire Download PDF

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KR101529510B1
KR101529510B1 KR1020140011711A KR20140011711A KR101529510B1 KR 101529510 B1 KR101529510 B1 KR 101529510B1 KR 1020140011711 A KR1020140011711 A KR 1020140011711A KR 20140011711 A KR20140011711 A KR 20140011711A KR 101529510 B1 KR101529510 B1 KR 101529510B1
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South Korea
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powder
pore structure
gas
nanowire
region
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KR1020140011711A
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Korean (ko)
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백승수
박시정
최두진
박형호
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국방과학연구소
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B1/00—Nanostructures formed by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • B82B3/0095—Manufacture or treatments or nanostructures not provided for in groups B82B3/0009 - B82B3/009

Abstract

Disclosed in the present invention are an apparatus and a method for synthesizing a nanowire. The apparatus for synthesizing a nanowire includes: a synthetic tube; a heating body; and a gas supply portion for supplying reactant gas and diluted gas. The synthetic tube includes: a decomposition area formed to react a gaseous-phase reactant of a powder material produced by being heated by the heating body; and a deposition area separated from the decomposition area, maintained at lower temperatures than the decomposition area, reacting the gaseous-phase reactant and the reactant gas with a porous structure, and producing the nanowire. The method of synthesizing a nanowire comprises: a step of separately arranging the powder material and the porous structure inside the synthetic tube; a step of decompressing the synthetic tube and supplying the diluted gas; a step of heating and producing the gaseous-phase reactant of the powder material; a step of supplying the reactant gas to the synthetic tube; and a step of transferring the gaseous-phase reactant and the reactant gas to the porous structure by using the diluted gas, and forming the nanowire in the porous structure.

Description

≪ Desc / Clms Page number 1 > METHOD FOR FORMATION OF NANOWIRE < RTI ID =

The present invention relates to a device capable of forming nanowires on the surface and inner pores of a pore structure and a method of forming nanowires.

One-dimensional nanostructures exhibit superior physical properties and unique optical and electrical properties compared to bulk materials. For this reason, nanowire has received considerable attention recently and many related researches are under way.

Alumina has been used as a structural material because it has excellent strength, excellent thermal stability and chemical corrosion resistance as a traditional ceramic structural material, and it has better physical properties than bulk when it is synthesized with powder or nanowire. Has been studied. In particular, the alumina nanowire can be directly grown inside the pores of the pore structure by using the gas-solid growth method (VS growth method) to contribute to the improvement of the overall strength of the pore structure by structuring the network, Can be performed. For example, a porous ceramic filter or the like is used in a DPF of an automobile or the like. Such a porous ceramic filter can enhance the function of the filter by growing nanowires such as whiskers in the pores.

Synthesis technologies of nanowires are divided into gas-solid growth method (VS growth method) and gas-liquid-solid growth method (VLS growth method). In order to grow nanowires directly inside the pore structure, the reactive gas species must flow into the pores. At this time, it is necessary to disperse the catalyst inside the pores to grow the nanowires by the VLS growth method, and it is technically difficult to grow the nanowire by the VS growth method.

According to a conventional technique for synthesizing alumina nanowires, aluminum (Al) powder is used as the raw material. However, in the case of aluminum powder, the melting point is about 660 ° C, while the vaporization point is about 2520 ° C. Therefore, in most processes that are difficult to heat above 2000 ° C, the nanowires are formed at the periphery where the raw material of the powder is melted, and the deposition through the gas phase hardly occurs. However, since the vaporization of the raw material is essential for introducing the reaction gas-phase paper into the pore structure, it is technically and economically difficult to use the aluminum powder as it is in the process for forming the nanowire inside the pore structure.

Another conventional technique for synthesizing nanowires includes a method using a metal organic material powder such as aluminum isopropoxide. This is a method of preparing alumina nanowires by charging the raw material powder into a tube and then heating and vaporizing the raw material powder. However, since the temperature at which the metal organic compound powder is vaporized and the temperature at which the alumina nanowire is synthesized are greatly different, in order to prevent the exhaustion of the raw materials before the nanowire synthesis, Separate from the high temperature zone and give a temperature gradient. In this case, intensive vaporization can not be performed at a desired point of time and process control is difficult. In addition, metal organic compound powders such as aluminum isopropyl rubbers often contain oxygen atoms, which makes it difficult to control the amount of oxygen in the tubes. This is a significant drawback because alumina is affected by the composition and composition of the tube depending on the oxygen concentration in the tube. There is also a technology that can use a powder raw material such as aluminum chloride (AlCl) which does not contain oxygen, but this is also a disadvantage in that it is not easy to control the process and maintenance of the equipment due to the chlorine compound is difficult.

It is an object of the present invention to provide a nanowire synthesizing apparatus and a nanowire synthesis method capable of forming nanowires from a surface of a pore structure to pores therein.

Another object of the present invention is to propose a nanowire synthesizer and a nanowire synthesis method which can economically synthesize nanowires inside a pore structure using an inexpensive powder raw material.

It is another object of the present invention to disclose a nanowire synthesizing apparatus and nanowire synthesis method capable of protecting a pore structure from a high temperature during synthesis of nanowires.

According to another aspect of the present invention, there is provided a nanowire synthesizer including: a synthetic tube configured to receive a raw material powder and a pore structure; A heating element for heating the synthesis tube to form a temperature gradient in the interior of the synthesis tube and a gas supply connected to the inlet of the synthesis tube to supply the reaction gas and the dilution gas to the synthesis tube, A decomposition region formed so as to dispose the powder material between the inlet and the outlet of the synthesis tube and to react with the reactant gas of the powder raw material generated by heating by the heating element, The decomposition region and the decomposition region are separated from the decomposition region so as to be maintained at a temperature lower than the decomposition region. Defined between and includes a deposition area to be formed to produce a nanowire by reacting the porous structure, the said reactor associate with the reaction gas carried by the dilution gas.

According to one example relating to the present invention, the pressure inside the synthesis tube can be kept below 10 torr.

According to another embodiment of the present invention, the heating element is arranged to heat the decomposition area, and the temperature difference between the decomposition area and the deposition area may be 200 to 300 ° C.

When the decomposition region is heated by the heating element, the deposition region may be formed so that heat is transferred from the decomposition region to 1200 to 1500 ° C.

According to another embodiment of the present invention, the gas supply unit includes a reaction gas supply unit for supplying oxygen to the synthesis tube generated in the decomposition zone in the decomposition zone and reacting with the reaction gas of the reformer type, And a diluent gas supply portion for supplying at least one of hydrogen, argon, and helium to the synthesis tube to distribute gas from the decomposition region to the deposition region.

The reaction gas supply unit may be configured to supply the oxygen to the synthesis tube at a flow rate of 1 to 100 sccm.

The diluent gas supply unit may be configured to supply the diluent gas to the synthesis tube at a flow rate of 1 to 500 sccm.

Wherein the nanowire synthesizer further comprises a gas flow rate regulator configured to regulate a flow rate of gas supplied to the synthesis tube from the gas supply portion, wherein the gas flow rate regulator includes: A first gas flow rate regulating device installed in a pipe connecting the synthesis tube and the reactant gas feeder and a second gas flow rate adjuster installed in a pipe connecting the synthesis tube and the diluent gas feeder to regulate the flow rate of the diluent gas, Device.

Wherein the nanowire synthesizer further comprises an exhaust device connected to an outlet of the synthesis tube to discharge gases that have undergone reaction inside the synthesis tube to the outside of the synthesis tube, A vacuum pump connected to the outlet of the synthesis tube to discharge the byproduct produced after the reaction, the reaction gas not participating in the reaction and the diluent gas, and the damage of the vacuum pump due to the substance discharged from the outlet of the synthesis tube. And an alkaline trap installed in a pipe connecting the synthetic tube and the vacuum pump to prevent the synthetic tube.

The exhaust system further includes a bellows valve installed in a pipe connecting the vacuum pump and the synthesis tube to regulate the pressure of the vacuum pump and a bellows valve provided in the bellows valve to provide pressure information necessary for operating the bellows valve. And a vacuum gauge installed in a pipe connecting the alkali trap.

According to another embodiment of the present invention, the nanowire synthesizer further comprises a susceptor disposed within the synthesis tube to receive the powder material, wherein the susceptor is stable in temperature gradient of the synthesis tube And may be formed of aluminum oxide or silicon carbide as much as possible.

In order to achieve the above object, the present invention also discloses a nanowire synthesis method. The nanowire synthesis method includes the steps of disposing a powder raw material and a pore structure in a synthetic tube so as to be spaced apart from each other, reducing the pressure of the synthetic tube to a predetermined pressure and supplying a diluting gas to the synthetic tube, Heating the region in which the powder material is disposed to generate a reactant species of the powder material; supplying a reaction gas to be reacted with the kind of the reactor to a synthesis tube; and supplying the reactant species and the reactant gas To the pore structure to form nanowires in the pore structure.

According to an example of the present invention, the powder raw material may be a mixed powder of 10 to 90 parts by weight of aluminum powder and 10 to 90 parts by weight of aluminum oxide powder.

According to another example related to the present invention, the porous structure is of carbon (carbon), aluminum oxide (Al 2 O 3), silicon nitride (Si 3 N 4), silicon carbide (SiC), mullite (mullite), and zirconia ( zirconia).

According to another example of the present invention, the powder raw material is disposed between the inlet and the outlet of the synthesis tube, and the pore structure may be disposed between the powder raw material and the outlet so as to be spaced from the powder raw material.

The region where the pore structure is disposed may be 200 to 300 ° C lower than the region where the powder material is disposed.

The nanowire synthesis method may maintain the temperature of the region where the pore structure is arranged at a predetermined temperature so as to determine the shape of the nanowire.

When the region where the powder material is disposed is heated, the region where the pore structure is disposed may be set so that heat is transferred from the region where the powder material is disposed and heated to 1200 to 1500 ° C.

According to another embodiment of the present invention, the diluent gas includes at least one gas selected from the group consisting of hydrogen, argon, and helium, and may be supplied to the synthesis tube at a flow rate of 1 to 500 sccm.

According to another embodiment of the present invention, the reaction gas contains oxygen and may be supplied to the synthesis tube at a flow rate of 1 to 100 sccm.

According to another example of the invention, the pressure inside the synthesis tube can be kept below 10 torr.

According to the present invention having the above-described structure, the powdery raw material is disposed inside the synthetic tube, and the pore structure is disposed to be spaced apart from the powdery raw material, the reaction gas phase produced in the synthetic tube reacts with the reactive gas injected into the synthetic tube The diluent gas may be transported to the pore structure to synthesize nanowires in the pore structure.

In addition, the present invention can separate the decomposition region generated in the reactor type and the deposition region in which the nanowire is synthesized to form the nanowire not only on the surface of the pore structure but also in the pores therein.

Further, the present invention can protect the pore structure from a high temperature by arranging the pore structure in a deposition region which is a relatively low temperature region.

1 is a conceptual view of a nanowire synthesizing apparatus according to an embodiment of the present invention;
2 is a flow chart of a method of nanowire synthesis according to one embodiment of the present invention.
FIGS. 3A and 3B are photographs showing changes in the structural morphology of the nanowires formed by changing the deposition temperature in the nanowire synthesis method of the present invention. FIG.
4A and 4B are photographs showing results of a conventional nanowire synthesis method in which a decomposition region and a deposition region are not separated.
5A and 5B are a photograph of a surface and a cross-section of a pore structure on which nanowires are deposited by the nanowire synthesis method of the present invention, respectively.

Hereinafter, a nanowire synthesizing apparatus and a nanowire synthesizing method according to the present invention will be described in detail with reference to the drawings. In the present specification, the same or similar reference numerals are given to different embodiments in the same or similar configurations. As used herein, the singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise.

1 is a conceptual diagram of a nanowire synthesizing apparatus 100 according to an embodiment of the present invention.

The nanowire synthesizer 100 includes a synthesis tube 110, a heating body 120, and a gas supply unit 130.

The synthesis tube 110 is formed to accommodate the powder raw material 115 which is a raw material of nanowire synthesis and the pore structure body 117 which is a target of nanowire formation. The composite tube 110 is formed as a horizontal hot-wall-like tube-shaped chamber. The composite tube 110 may be formed of aluminum oxide (alumina) or mullite. The pressure inside the synthesis tube 110 for synthesis of the nanowires is preferably maintained at less than 10 torr.

In the present invention, the synthesis tube 110 has a decomposition region 111 in which a powder raw material 115 is disposed, and a deposition region 112 in which a pore structure 117 is disposed and spaced apart from the decomposition region 111.

The decomposition region 111 is formed so as to place the powder raw material 115 between the inlet 110a and the outlet 110b of the synthesis tube 110. [ The decomposition region 111 is formed to react with the reactant gas of the reactant species of the powder raw material 115 generated by heating by the heating body 120.

The deposition region 112 is formed between the decomposition region 111 and the outlet 110b so as to be kept at a temperature lower than the decomposition region 111 and away from the decomposition region 111. [ The deposition region 112 is formed to react the reactive species carried by the diluent gas and the reactive gas to the pore structure 117 to produce nanowires.

The heating body 120 is formed to surround at least a part of the outer circumferential surface of the synthetic tube 110 and heats the synthetic tube 110 to form a temperature gradient inside the synthetic tube 110. The heating element 120 may be formed of an electric heating element 120 that receives electricity to generate heat and may heat at least one region of the synthetic tube 110 to a temperature of 1000 ° C or higher.

The area of the synthetic tube 110 heated by the heating element 120 may be the decomposition area 111. [ When heat is supplied from the heating element 120, the decomposition region 111 is heated to a temperature of 1000 ° C or higher, and a temperature gradient is formed inside the synthesis tube 110. The temperature difference between the decomposition region 111 and the deposition region 112 can be 200 to 300 占 폚. For example, when the temperature of the decomposition region 111 is 1500 ° C., the temperature of the deposition region 112 may be 1200 to 1300 ° C., It is preferably maintained at 1500 ° C.

The gas supply part 130 is connected to the inlet 110a of the synthesis tube 110 to supply the reaction gas and the dilution gas to the synthesis tube 110. [ The gas supplying unit 130 includes a reactive gas supplying unit 131 and a diluting gas supplying unit 132.

The reaction gas supplier 131 supplies the synthesis tube 110 with oxygen to be reacted with the reactor type produced in the decomposition region 111. The reaction gas supply unit 131 may be configured to supply the oxygen to the synthesis tube 110 at a flow rate of 1 to 100 sccm.

The diluent gas supply unit 132 supplies at least one of hydrogen, argon, and helium to the synthesis tube 110 to transport the reactive gas species and reactive gas from the decomposition region 111 to the deposition region 112. The diluent gas supply unit 132 may be configured to supply the diluent gas to the synthesis tube 110 at a flow rate of 1 to 500.

The nanowire synthesizer 100 includes piping 191, 192, 193, 194, and 195 that connect the components of the gas flow rate regulator 140, the exhaust device, and the nanowire synthesizer 100, As shown in FIG.

The gas flow rate regulator 140 is configured to regulate the flow rate of the gas supplied to the synthesis tube 110 from the gas supplier 130 and includes a first gas flow rate regulator 141 for regulating the flow rate of the reactant gas, And a second gas flow rate regulating device 142 for regulating the flow rate of the gas.

The first gas flow rate regulator 141 is installed in a pipe 191 for connecting the synthesis tube 110 and the reactive gas supply unit 131 to regulate the flow rate of the reactive gas. The second gas flow rate regulator 142 is installed in the pipe 192 connecting the synthesis tube 110 and the diluent gas supply unit 132 to regulate the flow rate of the dilution gas.

The exhaust device is connected to the outlet 110b of the synthesis tube 110 so as to discharge the gases which have undergone the reaction inside the synthesis tube 110 to the outside of the synthesis tube 110. [ The exhaust system may include a vacuum pump 150, an alkali trap 160, a bellows valve 170 and a vacuum gauge 180.

The vacuum pump 150 is connected to the outlet 110b of the synthesis tube 110 to discharge the byproducts generated after the reaction in the synthesis tube 110, the reactive gas and the diluent gas which did not participate in the reaction. The alkali trap 160 is connected to the pipe 110 connecting the synthesis tube 110 and the vacuum pump 150 to prevent damage to equipment such as the vacuum pump 150 due to the material discharged from the outlet 110b of the synthesis tube 110 193 and 194 and a filter such as carbon felt is installed in the alkali trap 160 to filter the byproducts and the like generated in the synthesis tube 110.

The bellows valve 170 is a device for regulating the pressure of the vacuum pump 150.

A vacuum gauge 180 is provided between the bellows valve 170 and the alkali trap 160 to provide information about the pressure to be controlled by the bellows valve 170. By adjusting the pressure of the vacuum pump 150 with the bellows valve 170 based on the pressure information provided by the vacuum gauge 180, the pressure inside the synthesis tube 110 can be kept below the desired pressure of 10 torr.

The nanowire synthesizer 100 may further include a susceptor 116 disposed within the synthesis tube 110 to receive the powder material 115 and the susceptor 116 may be disposed within the synthesis tube 110 (Alumina) or silicon carbide (SiC) so as to be stable in the temperature gradient of the silicon carbide (SiC).

Hereinafter, a method of synthesizing nanowires using the nanowire synthesizer 100 will be described.

2 is a flow diagram of a nanowire synthesis method in accordance with an embodiment of the present invention.

Referring to FIG. 2, a nanowire synthesizer 100 is used to synthesize nanowires. The nanowire synthesizer 100 shown in FIG. 1 is referred to.

Methods for synthesizing nanowires include thermal chemical vapor deposition (CVD), carbothermal reduction process, metal oxidation, metal-organic chemical vapor deposition (MOCVD) A vapor phase precursor method, a laser ablation method, a method using an aluminum oxide template and a chemical vapor deposition method (AAO template + CVD), and a wet chemical method.

Among them, the present invention utilizes the thermal chemical vapor deposition method. The nanowire synthesis method proposed by the present invention comprises the steps of disposing the powder material 115 and the pore structure 117 in the interior of the synthesis tube 110 so as to be spaced apart from each other (S200) of reducing the pressure of the synthesis tube 110 to a predetermined pressure and supplying a dilution gas to the synthesis tube 110, (S400) of supplying a reaction gas to be reacted with the kind of the reactant to the synthesis tube (110) (S400); and a step And a step S500 of transferring the reactant species and the reactant gas to the pore structure 117 to form nanowires in the pore structure 117.

The step S100 of disposing the powder raw material 115 and the pore structure 117 in the interior of the synthesis tube 110 so as to be spaced apart from each other may include a step of forming a decomposition region 111, To separate the regions 112 from each other.

The powder raw material 115 is disposed in the decomposition region 111 of the synthesis tube 110. The powder raw material 115 is preferably a mixed powder of 10 to 90 parts by weight of aluminum (Al) powder and 10 to 90 parts by weight of aluminum oxide (Al 2 O 3 ) powder. When the aluminum powder alone is used, the melting point of aluminum is about 660 ° C, but the vaporization point is 2520 ° C, so an excessively high temperature is required to produce the reactor type. However, when the aluminum powder and the aluminum oxide powder are mixed, reaction gas phase paper of alumina nanowires such as aluminum (Al) or aluminum oxide (Al 2 O) can be produced at a pressure of 1 torr or lower and a temperature of 1400 ° C or higher .

The present invention is characterized in that nanowires are synthesized more easily and economically by lowering the production temperature of the reactor type through interfacial reaction between aluminum (Al) powder and aluminum oxide (Al 2 O 3 ) powder. The susceptor 116 on which the raw material powder is mounted can use a material that is stable at a target temperature such as aluminum oxide (Al 2 O 3 ) or silicon carbide (SiC).

The pore structure 117 is disposed in the deposition region 112 of the synthesis tube 110. The pore structure 117 may include at least one selected from the group consisting of carbon, aluminum oxide (Al 2 O 3 ), silicon nitride (Si 3 N 4 ), silicon carbide (SiC), mullite, and zirconia It can be one.

Subsequently, the vacuum pump 150 is operated to reduce the internal pressure of the synthesis tube 110 to a predetermined pressure or lower, and a diluent gas is supplied to the synthesis tube 110 (S200).

The pressure inside the synthesis tube 110 is preferably less than 10 torr, more preferably less than 1 torr.

The diluent gas includes at least one gas selected from the group consisting of hydrogen, argon, and helium, and may be supplied to the synthesis tube 110 at a flow rate of 1 to 500 sccm.

Next, the synthesis tube 110 is heated using the heating element 120 while the temperature of the synthesis tube 110 is measured through the thermocouple device to generate the reactor type of the powder material 115 (S300). The temperature inside the synthesis tube 110 can be heated to a target temperature, and the target temperature can be heated, for example, to 1400 to 1500 ° C. The temperature of the deposition region 112 where the pore structure 117 is disposed may be set to be lower by 200 to 300 ° C than the temperature of the decomposition region 111 where the powder material 115 is disposed, It can be heated to 1200 to 1500 ° C.

Then, a reaction gas to be reacted with the kind of the reactor is supplied to the synthesis tube 110 (S400). Oxygen is used as the reaction gas and the flow rate thereof is preferably from 1 to 100 sccm, more preferably from 1 to 10 sccm. When the flow rate of the reactive gas is more than 30 sccm, the film may be mainly deposited instead of the wire.

Finally, the reactor type and the reactant gas are transported to the pore structure 117 using a dilution gas to form nanowires in the pore structure 117 (S500). The shape of the nanowire may vary depending on the temperature of the deposition region 112 where the pore structure 117 is disposed. Accordingly, the nanowire synthesis method can maintain the temperature of the region where the pore structure 117 is disposed at a predetermined temperature to determine the shape of the nanowire.

Hereinafter, the nanowires synthesized using the nanowire synthesizer and nanowire synthesis method proposed in the present invention are compared with those produced by the prior art.

FIGS. 3A and 3B are photographs showing structural changes of a nanowire formed by varying the deposition temperature in the nanowire synthesis method of the present invention. FIG.

3A is a photograph showing nanowires synthesized in a pore structure when the temperature of the decomposition region is heated to 1500 ° C. When the decomposition region is 1500 ° C, the deposition region becomes 1300 ° C. When the decomposition region is 1500 ° C., nanowires of various diameters are synthesized and some of the tube-shaped wires are deposited.

3B is a photograph showing nanowires deposited on the pore structure when the temperature of the decomposition region is heated to 1400 캜. When the decomposition region is 1400 ° C, the deposition region becomes 1200 ° C. When the decomposition region is at 1400 ° C, nanowires having a diameter of 100 nm or less on average are synthesized and have a relatively uniform diameter. Therefore, when the decomposition region is 1400 ° C, it can be confirmed that the nanowire is suitable for growing the inside of the pore structure.

4A and 4B are photographs showing results of a conventional nanowire synthesis method in which a decomposition region and a deposition region are not separated.

4A is a photograph showing the result of arranging the pore structure in the decomposition region and heating the decomposition region to 1400 캜. When the nanowire synthesis is performed without separating the decomposition region and the deposition region, it can be confirmed that nanowires are not deposited inside the pores of the pore structure by synthesizing in film form instead of nanowire.

Fig. 4B is a photograph showing the result of arranging the pore structure in the decomposition region and heating the decomposition region to 1200 deg. 4A, it can be confirmed that the nanowires are not deposited.

The results of FIGS. 4A and 4B are comparative examples in which the decomposition region and the deposition region are separated from each other in the present invention. When the temperature at which the reaction gas paper is generated and the temperature at which the nanowires are synthesized are equal to each other, Do not.

5A and 5B are photographs of nanowires synthesized by the nanowire synthesizer and nanowire synthesis method proposed in the present invention.

5A and 5B are a photograph of a surface and a cross-section of a pore structure on which nanowires are deposited by the nanowire synthesis method of the present invention, respectively.

5A and 5B show the result of arranging the pore structure in the deposition region and heating the decomposition region to 1400 DEG C, in which case the temperature of the deposition region becomes 1200 DEG C. [ It can be confirmed that a large amount of nanowires are formed inside the pore structure by cooling and condensing the generated vapor phase paper in the decomposition region and decomposing the powder raw material in the deposition region.

The nanowires synthesized in the present invention are fine lines having diameters ranging from several tens to several hundreds of nanometers, and their growth direction is not constant, and their growth pattern is like a bush.

As described above, according to the present invention, the nanowire can be formed in the inner pores of the pore structure by separating the decomposition region and the deposition region of the powder raw material from the prior art. The nanowire can enhance the pore structure of the adiabatic pore structure, and the pore structure in which the nanowire is synthesized can be used for industrial high temperature filter, DPF, carrier filter and the like.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is evident that many alternatives, modifications and variations will be apparent to those skilled in the art. For example, alumina nanowires are formed as the nanowires to be formed in the pore structure, and thus the source material corresponding to the raw powder is also used. However, the present invention is not limited to the alumina nanowires, A wire can be formed according to the present invention. Also, it will be understood that the pore structure is also made of a cordierite honeycomb substrate, but any pore structure is possible.

The nanowire synthesizer and nanowire synthesis method described above are not limited to the configurations and the methods of the embodiments described above, but the embodiments may be modified so that all or some of the embodiments are selectively combined .

100: nanowire synthesizer 110: synthetic tube
120: heating element 130: gas supply part
140: Gas flow rate regulator 150: Vacuum pump
160: Alkaline trap 170: Bellows valve
180: Vacuum gauge

Claims (21)

delete delete delete delete delete delete delete delete delete delete delete Disposing the powder raw material and the pore structure in the interior of the synthesis tube so as to be spaced apart from each other;
Reducing the pressure of the synthesis tube to a predetermined pressure and supplying a dilution gas to the synthesis tube;
Heating the region where the powder material is disposed in the synthesis tube to 1400 ~ 1500 ° C to produce the reactor species of the powder material;
Supplying a reaction gas to be reacted with the reactor type to a synthesis tube; And
And transporting the reactant species and the reactant gas to the pore structure using the diluent gas to form nanowires in the pore structure,
The powder raw material includes aluminum (Al) powder, 10 to 90 parts by weight of aluminum oxide (Al 2 O 3) powder mixture of 10 to 90 parts by weight of the powder,
Wherein the pressure inside the synthesis tube is maintained at less than 10 torr. delete 13. The method of claim 12,
Wherein the pore structure is at least one selected from the group consisting of carbon, aluminum oxide (Al 2 O 3 ), silicon nitride (Si 3 N 4 ), silicon carbide (SiC), mullite, and zirconia ≪ / RTI > 13. The method of claim 12,
Wherein the powder feedstock is disposed between an inlet and an outlet of the synthesis tube and the pore structure is disposed between the powder feedstock and the outlet to be spaced from the powder feedstock. 16. The method of claim 15,
Wherein a region where the pore structure is disposed is 200 to 300 DEG C lower than a region where the powder material is disposed. 16. The method of claim 15,
Wherein the temperature of the region where the pore structure is arranged is maintained at a predetermined temperature so as to determine the shape of the nanowire. 18. The method of claim 17,
Wherein the region in which the pore structure is disposed is set to be heated to 1200 to 1500 ° C by transferring heat from a region where the powder material is disposed, when the region where the powder material is disposed is heated. 13. The method of claim 12,
Wherein the diluent gas comprises at least one gas selected from the group consisting of hydrogen (H 2 ), argon (Ar) and helium (He), and is supplied to the synthesis tube at a flow rate of 1 to 500 sccm. Synthesis method. 13. The method of claim 12,
Wherein the reaction gas comprises oxygen and is supplied to the synthesis tube at a flow rate of 1 to 100 sccm. delete
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20120119251A (en) * 2011-04-21 2012-10-31 연세대학교 산학협력단 Method for synthesizing nanowires without using catalysts and apparatus for the same
KR101360775B1 (en) * 2012-12-04 2014-02-12 연세대학교 산학협력단 Method and apparatus capable of synthesizing high density wires in pores and on surface of porous material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20120119251A (en) * 2011-04-21 2012-10-31 연세대학교 산학협력단 Method for synthesizing nanowires without using catalysts and apparatus for the same
KR101360775B1 (en) * 2012-12-04 2014-02-12 연세대학교 산학협력단 Method and apparatus capable of synthesizing high density wires in pores and on surface of porous material

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