KR101808405B1 - High-efficiency automatic control sampler for nano particle by vapor phase-synthesis and method using the same - Google Patents

Abstract

The present invention relates to a method of synthesizing nanoparticles by gas phase synthesis by pyrolyzing raw materials of nanoparticles using an electric furnace or the like as a heat source and increasing the amount of nanoparticles synthesized using nanotubes It is a technique to increase the synthesis amount and recovery rate of continuously produced nanoparticles by using a cooling tube and a filter type automatic collecting device in collecting the nanoparticles. It is a technique to increase the synthesis amount of nanoparticles in the vapor phase synthesis process, A method and an apparatus for improving the efficiency of cooling the particles and greatly increasing the collection efficiency and recovery of the synthesized particles by using a collection device equipped with an automatic control device.

Description

TECHNICAL FIELD [0001] The present invention relates to a high-efficiency, large-scale vapor-phase synthetic nanoparticle automatic control collecting apparatus and a collecting method thereof. BACKGROUND ART [0002]

The present invention relates to a mass synthesis of nanoparticles by a gas phase synthesis method and a high efficiency collection and recovery method of synthesized particles. More specifically, the present invention relates to a method of collecting nanoparticles in a gas phase synthesis process, And an object of the present invention is to provide a method and apparatus for greatly increasing the collection efficiency and recovery of synthesized particles by using a collection device equipped with an automatic control device.

Nanotechnology, which has been the subject of discussion in the 21st century, is a collective term for technologies for making, manipulating, or analyzing materials at the nanometer (10 ^-9 m) level. Double nanoparticles have an increased ratio of surface to mass of particles compared to existing materials and materials, that is, the surface area per unit mass increases, thereby improving the performance of the particles and changing the physical properties such as decreasing the melting point of the particles. It is different from case. As a result, it has been applied to various fields such as materials manufacturing, electronics, medicine, biotechnology, environment and energy, and has become a main research topic of many researchers.

As a method for producing nanoparticles, liquid phase method, supercritical fluid method, and vapor phase method are widely used. In general, as a method for producing nanoparticles in general, a method of recovering nanoparticles by inducing a chemical reaction in a liquid phase is mainly used, and recently, techniques such as a high speed particle beam and a plasma gas evaporation technique are also performed. However, in the case of a high-speed particle beam, it requires a high level of technological power to generate nanoparticles in a supersonic nozzle by expanding and cooling the gas through a supersonic nozzle, and in the case of plasma gas evaporation, metal nanoparticles of several tens of nanometers It is difficult to synthesize small metal nanoparticles of 30 nm or less in a large amount.

Accordingly, in addition to the above-described methods, a vapor phase synthesis technique for inducing vaporization of a precursor material of nanoparticles and then rapidly condensing particles after production of particles due to collision between gas molecules in a high-temperature reactor has attracted attention recently. However, the recovery of nanoparticles is also very low due to particle collection by simple condensation, which leads to industrialization. Meanwhile, a number of known documents for addressing the above problems are as follows.

Korean Patent Laid-Open Publication No. 2006-0112546 discloses a method for producing silicon carbide which comprises: a vaporization step of vaporizing a precursor containing iron (Fe) and silicon (Si); A simultaneous reaction step of transferring the vaporized vaporized material in the vaporization step to the transfer gas to simultaneously charge the reaction gas in the reaction vessel where the pyrolysis reaction takes place; And a condensing / recovering step of recovering and recovering the coated nano powder formed in the simultaneous reaction step. Particularly, the vaporized iron-based vaporized material is transferred to a transfer gas in the vaporizing step to be first injected into a reactor in which a pyrolysis reaction takes place, A delayed reaction step of transferring the vaporized silicon-based vapor to the transfer gas and charging the vaporized silicon-based vapor to the reaction furnace in the vaporization step; And a condensing / recovering step of recovering and recovering the coated nano powder formed in the delayed reaction step. Advantages of manufacturing nano metal powder coated with silicon having various phases and sizes with this configuration Discloses a silica-coated nano iron powder horse-making process by chemical vapor deposition.

Korean Unexamined Patent Publication No. 2012-0054254 discloses a process for producing a manganese precursor and a titanium precursor vaporizing portion; A carrier gas supply line for supplying a carrier gas for transferring the vaporized precursor vaporized in the vaporizing portion to the reaction portion, to the vaporizing portion; An oxygen supply line for supplying an oxygen supply source to the reaction section; A reaction part for synthesizing a manganese oxide-titania catalyst by reacting the precursor vapor and the oxygen source; And a collecting part for collecting and recovering the oxidized manganese-titania catalyst synthesized in the reaction part. In particular, the present invention relates to an apparatus for producing a manganese oxide-titania catalyst comprising a precursor vaporizer (a manganese precursor and a titanium precursor vaporizer) A reaction step of transferring the reaction product to a reaction part, a reaction step of synthesizing a manganese oxide-titania catalyst by reacting the precursor vapor and the oxygen source transferred to the reaction part, And a collecting step of collecting and recovering the synthesized manganese oxide-titania catalyst, characterized by the production of a manganese oxide-titania catalyst having a small number of process steps, each process being continuous, mass production of the catalyst is possible, Titania catalyst capable of producing a manganese oxide-titania catalyst having high decomposition efficiency of an organic compound and the like.

In Korean Patent No. 10-1282142, a first precursor supply unit for vaporizing a first precursor and supplying it to a reaction unit; A second precursor supply unit for vaporizing the second precursor and supplying it to the reaction unit; A reaction unit for synthesizing the first precursor and the second precursor vapor to produce composite nanoparticles; An oxygen supply line for supplying an oxygen supply source to the reaction section; And a collecting unit for collecting the complex nanoparticles generated in the reaction unit, wherein the reaction unit comprises: a first rectilinear flow channel for generating nanoparticles from the first precursor vaporized material supplied from the first precursor supply unit; A curved flow path communicating with the linear flow path and allowing the nanoparticles generated in the first linear flow path to flow into the second linear flow path in a curved flow direction; A U-shaped reaction chamber having a second rectilinear flow path for synthesizing particles and a second precursor vaporizer supplied from the second precursor supply unit to produce composite nanoparticles; A second precursor inlet flow path for joining the second precursor vaporized material supplied from the second precursor supply section to the second linear flow path of the U-shaped reaction chamber; And a heat supply means for supplying heat to the U-shaped reaction chamber, and a method of manufacturing the same, wherein the U-shaped reaction chamber is vapor-phase synthesized in stages to prevent coagulation phenomena, And complex nano-particles having a high specific surface area can be easily produced.

Korean Patent Laid-Open Publication No. 2010-0109762 discloses a known residual chemical and by-product exhaust apparatus in which particles of a certain mass or more contained in exhaust gas are collected in powder form on a vacuum pipe connecting a processor chamber and a vacuum pump, And a trap for allowing a part of the exhaust gas to be discharged to the bypass through the gas bypass space formed between the inner and outer cylinders when the internal conductance is reduced to a predetermined value or less. When the conductance of the piping is reduced, a part of the gas corresponding to the reduced amount is continuously supplied to the vacuum pump side through the gas bypassing discharge space portion formed between the inner and outer tubes, thereby reducing the conductance of the vacuum piping If the production process chamber is affected or the trap is replaced It is possible to prevent the state where the conductance in the original vacuum pipe is lowered from affecting the production process for a long time, thereby remarkably improving the pumping ability of the vacuum pump and greatly improving the operation rate of the equipment. Discloses a residual chemical and by-product collecting apparatus in a semiconductor process using particle inertia that can significantly reduce the production cost.

In Cho et al., "Intraparticle structures of composite TiO 2 / SiO 2 nanoparticles prepared by varying precursor mixing modes in vapor phase", Journal of Materials Science, June 2003, Vol. 38, Issue 12, pp 2619-2625, using the method, the titania in the reaction region of the vacuum induction and then walk volatilization of the precursor materials to a high temperature inside the reactor - the composite nanoparticles TiO ₂ -SiO ₂ having a different structure to the technique for manufacturing the silicon nano-composite catalyst TTIP And TEOS were prepared by mixing various reactants in the equimolar vapor phase hydrolysis of TEOS. The structures of the titania core were composed of oxide (TS) surrounded by silica cell or oxide Structure. ≪ / RTI >

However, the use of thermophoresis and a straight tube as the gas-phase synthesized particle collection method lowers the cooling efficiency of the high-temperature particles or impregnates a part of the nanoparticles on the wall of the collection tube, . Also, since it is composed of a non-magnetic capture system, it is a method of capturing nanoparticles synthesized after the system is stopped from time to time, and it has limitations in mass production and collection for commercialization.

Korea Patent Publication No. 2006-0112546 Korea Patent Publication No. 2012-0054254 Korean Registered Patent Korean Patent No. 10-1282142 Korea Patent Publication No. 2010-0109762

Journal of Materials Science, June 2003, Vol.38, Issue 12, pp 2619-2625

Disclosure of Invention Technical Problem [8] Accordingly, the present invention has been made keeping in mind the above problems occurring in the prior art,

The nanoparticle collection process using nanoparticles using large number of nanoparticles and the automatic collection control device can synthesize a large amount of nanoparticles in a short time compared to the conventional single tube and thermophoretic collection, and the recovery rate can be greatly increased. In the case of using a single reactor tube, the heat transfer efficiency inside the reactor tube is lowered as the precursor feed rate is increased. On the other hand, when the multi tube is used, the heat transfer and heat conduction efficiency inside the reactor tube increases, It can be synthesized in a large amount. Therefore, the nanoparticles produced in large quantities are intended for the purification of air that adsorbs or oxidizes atmospheric pollutants contained in domestic / foreign industrial facility flue gas.

 Therefore, it is possible to synthesize nanoparticles by vapor phase synthesis by pyrolyzing the raw material of nanoparticles by using electric furnace as a heat source, and to increase the amount of nanoparticles to be synthesized by using multitubes in the synthesis of nanoparticles, It is a technology to increase the synthesis amount and recovery rate of continuously produced nanoparticles by using a cooling tube and filter type automatic collecting device during particle collection. It is a technique to increase the synthesis amount of nanoparticles by using multi- And to provide a method and an apparatus for enhancing the cooling efficiency and greatly increasing the collection efficiency and recovery of synthesized particles by using a collection device equipped with an automatic control device.

To this end, the present invention provides an apparatus for automatically controlling high-efficiency vapor-phase synthesis nano-particles, comprising: a vaporizer (100) for vaporizing a precursor material; A reaction tube (200) including a reaction tube (210) composed of a plurality of tubes in which vaporized vaporized substances in the vaporizer are transferred to a carrier gas to cause a thermal decomposition reaction; A condenser 300 for condensing high-temperature nanoparticles formed in the reaction furnace; And a particle collecting device (400) for collecting the nanoparticles condensed in the condenser by using a filter.

Also, in the reactor, a dispersion plate 220 for inducing a constant flow of the vaporized material may be installed at a predetermined position of the reaction tube.

In addition, the reactor may surround the reaction tube to heat the reaction tube, or may further include a heating medium 230 at the center of the reaction tube section.

The reaction tube may be composed of two or more tubes and may be disposed at a uniform interval on the cross section of the reaction tube, or may be arranged radially spaced from the center of the cross section.

Further, the dispersion plate may be installed at one or more of the front end, the rear end of the reaction tube, and the reaction tube surrounded by the heating medium.

Further, a metal bar 211 having a high thermal conductivity may be additionally provided at the center of the cross section of the reaction tube in order to increase the heating effect and prevent the breakage of the reaction tube.

The condenser includes a condensing outer tube 310 through which a cooling fluid circulates, a cooling fluid inlet 320 through which the cooling fluid is introduced into the outer tube, a cooling fluid outlet 330 through which the cooling fluid formed in the outer tube is discharged, It may be in the form of a double tube for increasing the cooling efficiency including the condensed inner tube 340 and the temperature control device 350 having a polygonal or ball shape for increasing the contact cross sectional area of the cooling fluid.

Further, the surface of the inner tube of condensation may be selectively formed with fins or wrinkles to enhance heat transfer.

The particle collecting device includes a collecting pipe 410, and a bag filter pipe 420 formed at an end of the collecting pipe. A collecting filter 430 formed between the bag filter tube and the collecting tube, a compression gas inlet 440 connected to one end of the collecting tube and the other end connected to the bag filter tube, A nano particle inflow part 450 through which a carrier gas containing nanoparticles cooled from the condenser flows, nanoparticles introduced into the nanoparticle inflow part are collected in a bag filter 421, And a second exhaust pipe (470) for exhausting the compressed gas to collect the nanoparticles collected in the bag filter by the collecting filter, wherein the compressed gas inlet, the nanoparticle inlet, A valve may be formed in the first exhaust pipe and the second exhaust pipe.

In addition, the compressed gas inlet may further include an injection nozzle 441 for injecting the compressed gas into the bag filter.

When the pressure of the bag filter pressure gauge 422 provided inside the bag filter tube rises above a predetermined pressure, the injection condition of the compressed gas in the particle collecting device is set so that injection And a pressure control unit 480 for controlling the valve.

Also, the vaporizer may include a bubbler 110 in which a precursor is accommodated and vaporized, and a thermostat 120 for heating the bubbler.

The bubbler is cylindrical with a diameter of 150 mm and can contain a single precursor material in a single stage inside the reactor. Also, the oil bath may include heat ray and the oil used may be a heat-resistant silicone oil such as Shin-Etsu KF-54.

The present invention relates to a high-efficiency gas phase synthesis nanoparticle automatic control collection method,

A first step of vaporizing the precursor material in a vaporizer, a second step in which a pyrolysis reaction occurs in a reaction furnace in which a vaporized vaporized material in the vaporizer is transferred to a carrier gas and includes a reaction tube composed of a plurality of tubes, A third step of condensing high-temperature nanoparticles formed in the reactor in a condenser, and a fourth step of recovering the nanoparticles condensed in the third step using a filter of a particle collecting device. Synthetic nanoparticle automatic control capture method.

In addition, the third step may include: a condensed outer appearance in which the cooling fluid is circulated; a cooling fluid inflow portion into which the cooling fluid formed in the outer pipe flows; a cooling fluid discharge portion in which the cooling fluid is discharged from the outer pipe; A condenser tube having a polygonal or ball shape for increasing the cooling efficiency and a condenser tube for cooling the condenser tube.

The fourth step may include a collecting pipe, and a bag filter tube formed at an end of the collecting pipe. A collecting filter formed between the bag filter tube and the collecting tube, a compression gas inlet connected to one end of the collecting tube, the other end being connected to one end of the bag filter tube, A first exhaust pipe through which a carrier gas including nanoparticles is introduced, a nanoparticle introduced into the nanoparticle inflow section after the nanoparticles are collected by the bag filter, and a second exhaust pipe through which the carrier gas is discharged, And a second exhaust pipe for exhausting the compressed gas to be collected by a collecting filter, wherein the compressed gas inlet, the nanoparticle inlet, the first exhaust pipe, and the second exhaust pipe can be carried out in a particle collecting device in which a valve is formed have.

In addition, in the fourth step, the injection condition of the compressed gas is determined by the injection nozzle to remove the nanoparticles collected in the bag filter when the pressure value of the bag filter pressure gauge installed in the bag filter tube rises above a predetermined pressure And a pressure control unit for controlling the valve to be sprayed.

In the gas phase synthesis reaction of the present invention, by using a multi-tube for efficient heat transfer, it is possible to increase the synthesis amount of nanoparticles having constant physical / chemical characteristics.

The cooling efficiency can be greatly improved by increasing the contact area between the high temperature particles synthesized and the cooling surface according to the cooling apparatus used in the present method.

By using an automatically controlled filter device, the nanoparticle recovery rate can be greatly increased by trapping the particles.

Above the predetermined pressure, the nanoparticle collection direction is automatically controlled to prevent the internal pressure in the process from excessively increasing.

The overall process is simplified by reducing the number of additional processes such as vacuum pumps.

In addition, it is easy to uniformly maintain the internal pressure of the reaction tube by uniformly inducing a constant flow of the vaporized material entering the multi-tube by using the dispersing plate and the amount of gas in each reactor.

FIG. 1 is a block diagram of a large-scale synthesis of nanoparticles and a particle collecting device according to an embodiment of the present invention.
2 is a view of a multi-tube reaction tube according to one embodiment of the present invention.
FIG. 3 is a diagram of a precursor dispersing apparatus, which is an embodiment of the present invention.
FIG. 4 is a diagram of a condenser having an inner pipe as a ball, which is one embodiment of the present invention.
FIG. 5 is an operational flow chart in which nanoparticles of a particle collecting apparatus according to an embodiment of the present invention are collected in a bag filter.
Fig. 6 is an operational flow chart in which nanoparticles of a particle collecting apparatus according to an embodiment of the present invention are collected by a collecting filter.
7 is a graph of the amount of particles collected per hour according to a method of collecting the produced particles according to an embodiment of the present invention.
FIG. 8 is a graph of particle generation of nanoparticles synthesized from precursor materials having different volatilization temperatures, which is an embodiment of the present invention.
9 is a SEM photograph of nanoparticles synthesized through an embodiment of the present invention.

The terms and words used in the present specification and claims should not be construed as limited to ordinary or dictionary terms and the inventor may appropriately define the concept of the term in order to best describe its invention It should be construed as meaning and concept consistent with the technical idea of the present invention. Therefore, the embodiments described herein are merely the most preferred embodiments of the present invention and are not intended to represent all of the technical ideas of the present invention, so that there are various equivalents and modifications that can be substituted at the time of the present application It should be understood.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, a metal complex-type insect-control net having antibacterial properties according to the present invention and a method for producing the same will be described in detail with reference to the accompanying drawings.

FIG. 1 is a block diagram of a large-scale synthesis of nanoparticles and a particle collecting device according to an embodiment of the present invention.

The method and apparatus for mass synthesis of nanoparticles by the gas phase synthesis method according to the present invention and the high efficiency collection and collection apparatus of the synthesized particles are classified into a multitubular gas phase synthesis apparatus for increasing the amount of nanoparticles to be synthesized, And a collecting device for collecting the collected objects efficiently and automatically. First, a gas phase synthesis apparatus for producing a large amount of nanoparticles will be described as follows. As shown in FIG. 1, single nanoparticle to multi-component nanoparticle precursor materials are located in different particle generators. And then maintained at a constant temperature using a temperature controller in consideration of the volatilization temperature of each precursor material. The volatilized precursor material is fed to the multitubular electric furnace reactor via argon (Ar) or air, and high temperature particles are synthesized by the particle synthesis mechanism.

Such a high efficiency gas phase synthesis nanoparticle automatic control and collecting apparatus includes a vaporizer 100 for vaporizing a precursor material; A reaction tube (200) including a reaction tube (210) composed of a plurality of tubes in which vaporized vaporized substances in the vaporizer are transferred to a carrier gas to cause a thermal decomposition reaction; A condenser 300 for condensing high-temperature nanoparticles formed in the reaction furnace; And a particle collecting device 400 for collecting the nanoparticles condensed in the condenser using a filter.

The carrier gas may be any one or a mixture of two or more of argon, nitrogen, helium, oxygen, and air. It is clear that there is no limit to the composition of the carrier gas if there is no physicochemical effect on the formation of the nanoparticles of the precursor. The carrier gas may be a mixed gas of argon and air in a ratio of 1:10.

The material of the reaction tube may be SUS 316, alumina, quartz, or mullite. Further, it is obvious that the material of the reaction tube is not particularly limited as long as it is a metal or a ceramic material that can accommodate the reaction conditions such as the temperature required for the reaction tube. In addition, in the embodiment of the present invention, the multitubular reaction tube is made of alumina material, and the other connecting portion and the gas line are made of SUS316.

2 is a view of a multi-tube reaction tube according to one embodiment of the present invention. A fluidized dispersion plate is placed on the upstream side of the multi-tubular reactor to induce a uniform flow of volatilized precursor material, and a certain amount of precursor material flows into the multi-tubular reactor. In order to improve heat transfer and thermal efficiency, it is possible to arrange the gap without any space so that there is no space between the reaction tubes, and the flow of the reaction tube is arranged in one direction.

The material of the multi-tube may be SUS 316, alumina, stone, or mullite. Also, the shape of the multi-tube may be polygonal or cylindrical. The plurality of multi-tubes may have a constant diameter or a cross-sectional area of the tube or may have a difference. The arrangement of the multi-tubes may be arranged at a uniform interval in the cross section of the reaction tube, or may be arranged with a gap in the radial direction from the center of the cross section. A metal bar 211 having a high thermal conductivity may be additionally provided at the center of the cross section of the reaction tube in order to increase the heating effect and prevent the breakage of the reaction tube. The material and the shape of the metal bar are not limited as long as the objects and effects of the metal bar can be achieved. The material of the metal bar may be aluminum, copper, silver, stainless steel, or the like. The shape of the metal bar may be polygonal, cylindrical, or a combined bundle of a plurality of metal bars. In addition, when a round multi-tube is inserted into the reaction tube and the SiC heating element (silicon carbide, non-metallic heating body) is placed inside the reaction tube, the effect of simultaneously heating the inside and the outside of the reaction tube can be obtained and thermal conductivity and thermal efficiency It can be a strength in terms of.

FIG. 3 is a diagram of a precursor dispersing apparatus, which is an embodiment of the present invention. A dispersion plate 220 for guiding a constant flow of the vapor is installed at a predetermined position of the reaction tube. The dispersion plate may be installed at one or more of the front end, the rear end of the reaction tube, and the reaction tube surrounded by the heating medium. The material of the dispersion plate may be SUS 316, alumina, stone, or mullite. The shape of the dispersion plate may be polygonal or cylindrical. The shape of the hole formed in the dispersing plate may be polygonal or cylindrical, and the polygonal or the diameter may be variously designed according to the linear velocity condition of the carrier gas including the vaporized precursor of the set reaction condition.

The dispersion plate may be installed at one or more of the front end, the rear end of the reaction tube, and the reaction tube surrounded by the heating medium. The heating medium is not limited as long as it is a medium capable of heating the temperature of the reaction tube to a temperature necessary for the reaction. The heating medium may be any one or a combination of two or more of SiC, super cantal, resistance heating element and electric furnace. In an embodiment of the present invention, each of the dispersing plates has holes, and each lid is covered with an upper part. When the gas is injected into the upper part of the lid, The heating medium is in contact with the electric furnace and the heating band can be wound and maintained at 95 ° C.

FIG. 4 is a diagram of a condenser having an inner pipe as a ball, which is one embodiment of the present invention. The synthesized high-temperature particles will be described in the condenser and automatic collection and recovery steps as follows. The particles produced by the above process are located at a high temperature between the synthesizing device and the collecting device in order to prolong the life of the filter placed behind the cooling device and to increase the collection efficiency. The high-temperature synthesis gas produced through the gas phase synthesis apparatus is introduced into a ball-shaped cooling apparatus according to the gas flow. After the introduction, the gas flow is slowed by the expansion of the space, and vortices of the particles are generated inside the cooling device. After that, the cooling water of the high temperature particles is efficiently cooled by the low temperature cooling water on the inner wall of the double pipe and moved to the particle collecting device. Therefore, the condenser includes a condensing outer pipe 310 through which a cooling fluid is circulated, a cooling fluid inlet 320 through which the cooling fluid is introduced into the outer tube, a cooling fluid outlet 330 through which the cooling fluid formed in the outer tube is discharged, It may be in the form of a double tube for increasing the cooling efficiency, including a condensing inner tube 340 having a polygonal or ball shape for increasing the contact cross-sectional area of the cooling fluid, and a temperature control device 350. The surface of the inner tube of condensation may be selectively formed with pins or wrinkles to enhance heat transfer. The shape of the fin is not particularly limited as long as heat transfer can be increased, and the shape of the inner tube can be variously designed. It can be selectively formed on the inner or outer surface of the condensed inner tube.

In the previous step, the cooled nanoparticles are effectively trapped in a ceramic filter bag that can withstand high temperatures and pressures. The bag filter has a pore size (0.3 μm) capable of collecting particles of 2 nm or more to 90%. The nanoparticles introduced from the cooling device are collected by the gas flow from the outside of the circular bag filter to the inside of the bag filter . Due to the continuous synthesis and collection of nanoparticles, the filter pore is clogged and the internal pressure is increased accordingly. When the internal pressure reaches 0.5 atm, the solenoid valve is activated to pulsing the particles. That is, as the compressed air flows downward for a short time (about 0.5 second), the nanoparticles accumulated in the bag filter are moved to the trapping filter in the form of a lower plate, and then collected in the second filter . When the internal pressure returns to the normal state, the particles are collected again in the upper bag filter. When a large amount of nanoparticles are synthesized and continuously collected through this device, the cooling efficiency of the hot gas due to the use of the thermophoretic linear collecting tube, which is a conventional collecting method, is lowered and the collection efficiency is lowered. There is an advantage that can be made.

FIG. 5 is an operational flow chart in which nanoparticles of a particle collecting apparatus according to an embodiment of the present invention are collected in a bag filter.

The particle collecting device includes a collecting pipe (410), and a bag filter pipe (420) formed at the end of the collecting pipe. A collecting filter 430 formed between the bag filter tube and the collecting tube, a compression gas inlet 440 connected to one end of the collecting tube and the other end connected to the bag filter tube, A first exhaust pipe 460 through which the nanoparticles introduced into the nanoparticle inflow portion are collected after the bag filter is collected, and the carrier gas is discharged from the first exhaust pipe 460; And a second exhaust pipe (470) for discharging the compressed gas injected through the injection nozzle to collect the nanoparticles collected in the bag filter by the collecting filter, wherein the compression gas inlet, the nanoparticle inlet, A valve may be formed in the first exhaust pipe and the second exhaust pipe. The shape and material of the bag filter, which is one embodiment of the present invention, is a ceramic filter (pore size-0.3 탆) having an outer diameter of 60 mm and an inner diameter of about 45 mm. The number of the bag filter is 1, It is self-evident.

Fig. 6 is an operational flow chart in which nanoparticles of a particle collecting apparatus according to an embodiment of the present invention are collected by a collecting filter. The compressed gas inlet may further include an injection nozzle 441 for injecting the compressed gas into the bag filter.

When the pressure of the bag filter pressure gauge 422 provided inside the bag filter tube rises above a predetermined pressure, the injection condition of the compressed gas in the particle collecting device is set so that injection And a pressure control unit 480 for controlling the valve. In one embodiment of the present invention, the reaction can proceed at 0.25 bar and flush at 0.5 bar.

Also, the vaporizer may include a bubbler 110 in which a precursor is accommodated and vaporized, and a thermostat 120 for heating the bubbler. The bubbler may be formed in a cylindrical shape or a polygonal shape, and may have one or two or more plates. An oil bath, a thermal insulation, a hot wire or a band heater can be applied to the thermostatic chamber.

7 is a graph of the amount of particles collected per hour according to a method of collecting the produced particles according to an embodiment of the present invention.

[Example 1]

TiO ₂ precursor TTIP (TTIP, Ti [OCH (CH ₃ ) ₂ ] ₄ , Kanto Chemical Co. Inc.) is maintained at 95 ° C in the form of external warming using the apparatus of FIG. At this time, argon (Ar) gas of 4.3 L / min is introduced into the TTIP supply unit, and the precursor is volatilized and introduced into the reactor in which air of 41 L / min flows. The injected precursor forms TiO ₂ nanoparticles in a reactor maintained at 900 ° C. The formed nanoparticles are passed through a ball type cooling tube to collect particles generated by an automatically controlled particle collection device. FIG. 7 shows the collection (collected / recovered amount) of a single collection method of the thermogravimetric method, the electric dust collection method and the impinger method in order to compare the collection efficiency according to the collection device.

The specific recovered amount is shown in Table 1.

Collection type Ball type Water-cooled collection tube Electric collector Collector Recovery (%) 0.8 to 1.5 g / h
10.5 to 13 g (10%) / TTIP 500 ml 1.7 to 1.8 g / h
18 ~ 20g (15%) / TTIP 500ml Collection type Impinger Collection tube Ceramic filter Collector Recovery (%) 2.0 to 2.7 g / h
25 ~ 32g (25%) / TTIP 500ml 6 to 7 g / h
110 ~ 120g (86%) / TTIP 500ml

FIG. 8 is a graph of particle generation of nanoparticles synthesized from precursor materials having different volatilization temperatures, which is an embodiment of the present invention.

[Example 2]

The amount of particles generated (amount of synthesis, amount collected / recovered) of the nanoparticles synthesized from the precursor materials having different volatilization temperatures is shown in Fig. In order to compare the amount of nanoparticles synthesized and collected by the present invention as a comparative example, nanoparticles are collected through a conventional thermophoresis method. In the graph, the amount of nanoparticles produced by the conventional method and the present invention showed a tendency that the amount of generated particles did not increase significantly when the precursor volatilization temperature was above 90 ° C. On the other hand, it can be confirmed that the amount of nanoparticles generated by 20 times or more is increased when a large amount of synthesis and automatic collection control apparatus using the multi-tube mentioned in the present invention is used as compared with the conventional method.

Although the present invention has been described with reference to the accompanying drawings and embodiments, it is to be understood that the present invention is not limited to the above-described embodiments, but may be modified and changed without departing from the scope and spirit of the invention. It is clear that the present invention is not limited to the above-described embodiments. Accordingly, the scope of protection of the present invention should be construed according to the following claims, and all technical ideas which fall within the scope of equivalence by alteration, substitution, substitution, and the like within the scope of the present invention, Range. In addition, it should be clarified that some configurations of the drawings are intended to explain the configuration more clearly and are provided in an exaggerated or reduced size than the actual configuration.

100: vaporizer
110: Bubbler
120: thermostat
200: Reaction furnace
210: Reaction tube
211: metal bar
220: Dispersion plate
230: heating medium
300: condenser
310: condensation appearance
320: cooling fluid inlet
330: Cooling fluid outlet
340: Internal condensation pipe
350: Temperature control device
400: Particle collecting device
410: collection tube
420: bag filter tube
421: Bag filter
422: Back filter pressure gauge
430: collection filter
440: Compressed gas inlet
441: injection nozzle
450: nanoparticle inflow part
460: First exhaust pipe
470: Second exhaust pipe
480:

Claims (16)

In a high efficiency gas phase synthesis nanoparticle automatic control collecting apparatus,
A vaporizer to vaporize the precursor material;
A reaction furnace comprising a reaction tube composed of two or more multi-tubes in which vaporized vaporized substances in the vaporizer are transferred to a carrier gas to cause a thermal decomposition reaction;
A condenser for condensing high-temperature nanoparticles formed in the reaction furnace; And
And a particle collecting device for collecting the nanoparticles condensed in the condenser by using a filter,
The reactor is provided with a dispersing plate for inducing a constant flow of the vaporized material at a predetermined position of the reaction tube,
The two or more multi-tubes may be arranged at a uniform interval on the cross section of the reaction tube, or may be disposed radially spaced apart from the center of the cross section,
A metal bar having a high thermal conductivity is additionally provided at the center of the cross section of the reaction tube in order to increase the heating effect and prevent the breakage of the reaction tube,
The condenser includes a condensation outer tube through which a cooling fluid is circulated, a cooling fluid inlet through which a cooling fluid formed in the condensation outer tube flows, a cooling fluid outlet through which the cooling fluid is discharged from the condensation outer tube, A condensation inner tube having a polygonal shape or a ball shape, and a temperature control device,
Wherein the surface of the inner tube of condensation is selectively formed with fins or wrinkles to enhance heat transfer.
delete The method according to claim 1,
Wherein the reactor further comprises a heating medium in the center of the cross section of the reaction tube for surrounding the reaction tube to warm the reaction tube.
delete The method of claim 3,
Wherein the dispersion plate is installed at one or more of a front end of the reaction tube, a rear end thereof, and a reaction tube surrounded by the heating medium.
delete delete delete The method according to claim 1,
The particle collecting apparatus includes a collecting pipe, a bag filter tube formed at the end of the collecting tube, a collecting filter formed between the bag filter tube and the collecting tube, a collecting filter connected to one end of the collecting tube, A nanoparticle inlet connected to one end of the bag filter tube and through which a carrier gas including nanoparticles cooled from the condenser flows, nanoparticles introduced into the nanoparticle inlet are collected in a bag filter, A first exhaust pipe through which the carrier gas is discharged and a second exhaust pipe through which the compressed gas is discharged for collecting the nanoparticles collected in the bag filter by the collecting filter, wherein the pressurized gas inlet, the nanoparticle inlet, Wherein a valve is formed in the first exhaust pipe and the second exhaust pipe.
10. The method of claim 9,
Wherein the compressed gas inlet further comprises an injection nozzle for injecting a compressed gas into the interior of the bag filter.
11. The method of claim 10,
The injection condition of the compressed gas of the particle collecting apparatus is controlled such that when the pressure value of the bag filter pressure gauge installed in the bag filter tube rises above a predetermined pressure, the valve is injected to remove the nanoparticles collected in the bag filter Wherein the pressure control unit further comprises a pressure control unit for controlling the flow rate of the gas.
The method according to claim 1,
Wherein the vaporizer comprises a bubbler containing a precursor and being vaporized, and a thermostat for warming the bubbler.
A method for automatically collecting high-efficiency gaseous synthetic nano-particles using the high-efficiency gas-phase synthetic nano-particle automatic control apparatus according to any one of claims 1, 3, 5, and 12,
A first step of vaporizing the precursor material in a vaporizer;
A second step in which a pyrolysis reaction occurs in a reaction furnace including a reaction tube composed of a plurality of tubes, wherein the vaporized vaporized material is transferred to a carrier gas;
A third step of condensing high-temperature nanoparticles formed in the reactor in the second step in a condenser; And
And a fourth step of recovering the nanoparticles condensed in the third step using a filter of a particle collecting device. delete delete delete

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