WO2009092207A1

WO2009092207A1 - A stirring device, a device with said stirring device for producing nanometer powder and its method

Info

Publication number: WO2009092207A1
Application number: PCT/CN2008/070675
Authority: WO
Inventors: Cheolsu Lee; Seokkeun Koh; Jaeho Joo; Unjung Yeo
Original assignee: Inano Limited
Priority date: 2008-01-22
Filing date: 2008-04-03
Publication date: 2009-07-30
Also published as: CN101925402A

Abstract

A stirring device, a device with said stirring device for producing nanometer powder and its method are provided. The device for producing nanometer powder includes a stirring tank (530) for containing supporters (520) of nanometer material, a vertical transportation part (531) located in the stirring tank (530) for transporting said supporters (520) from lower portion to upper portion of the stirring tank (530) by helical rotation, a support plate (534) located in the stirring tank (530) and at upper portion of the vertical transportation part (531) for supporting supporters (520) from said vertical transportation part (531), said support plate (534) is cone-shaped or frustum of a cone in shape of which central section is higher and circumference section is lower, and a depositing device including a depositing source located in the stirring tank (530) and above the support plate (531) for depositing nanometer powder on the supporters in manner of physics disposition. The device for producing nanometer powder can mix the supporters or supporter chips uniformly and reduce the friction between supporters or supporter chips.

Description

Agitating device, nano powder manufacturing device with agitating device, and manufacturing method. The present application claims priority to Chinese Patent Application No. 200810004352, filed on Jan. 22, 2008, the entire contents of the Chinese Patent Application No. 200810004352. Incorporated here by reference.

Technical field

The present invention relates to the field of nanotechnology, and in particular to a stirring device, a nanopowder manufacturing device having the stirring device, and a manufacturing method. Background technique

Nanotechnology has become the most fundamental foundation in important technical fields such as information and communication technology (IT), life science technology (BT), and environmental technology (ET), which are called high-tech, and has great potential in the field of technology development. Influence. Nanometers (the Nano) refers to a unit equivalent to ^10-9 meters, so-called nano-technology is constructed or isolated atoms and molecules and to control the operation of the constituent elements of technology. Nanotechnology is characterized by high-tech intensification, high economic spread, maximum energy efficiency, and environmental affinity.

Nano industry segments can be categorized as Nano Processes, Nano Structures, Nano Functions, Nano Components & Systems, Nano Infrastructures, and Nanomaterials. (Nano Materials) and so on. Nanotechnology can be applied to nano materials, nano devices, nano bios, medical, environmental, energy, nanosystems, security, etc., and has a wide range of applications. The most basic nanomaterials in the field of nanotechnology can be divided into Nano Particles, Nano Wire, Nano Tube, Nano Wall, and Nano Capsule. , Nano Rod, etc.

The nanopowder refers to ultrafine particles which are not in the size and shape of the particles and have an average particle diameter of 100 nm or less. The manufacturing method of the nano powder can be classified into a gas phase method, a liquid phase method, and a solid phase method. Representative manufacturing methods using the gas phase method include a gas evaporation/condensation method and a gas phase synthesis method, and a liquid phase method includes a precipitation method and a spray drying method. The method has a mechanized pulverization method in the solid phase method. The manufactured nanopowder exhibits specific electrical, magnetic, mechanical, and catalytic properties that cannot be observed in the original material due to the miniaturization of the material structure (below 100 nm) and the accompanying increase in surface area. Therefore, it can be applied to a new generation of functional materials such as magnetic components, sensors, filters, and catalysts.

There are various methods for fabricating nanoparticles in the prior art, which can be broadly classified into physical methods and chemical methods. Since the chemical method utilizes a chemical reaction, it is necessary to use an oxidizer and a reducing agent (red _UC tant). Therefore, nanoparticles produced by chemical reactions may have residual ions in many reaction processes, so aggregation between particles is likely to occur. In order to prevent aggregation between particles, an additive such as a surfactant or a dispersant is usually used, so that the purity of the nanoparticles is relatively low. When the application product is manufactured, it is also easy to react with the additive, and after the completion of the nanoparticle production process, a toxic derivative is produced. In addition, the method of chemically manufacturing nanoparticles is difficult to produce quantitative nanoparticles when mixing inert metals or metal salts of different properties, so there are limitations in the material selection of the nanoparticles. Due to such problems, the method of chemically manufacturing nanoparticles reduces the original function of the nanoparticles, requiring additional costs for the treatment of oxidants, reducing agents, residual acids and the like.

The method of physically manufacturing nanoparticles can be divided into a Top Down method and a Bottom Up method. The down-direct method is, for example, mechanically pulverizing the mass to produce nanoparticles; the upward-oriented method, for example, refers to the application of an energy source to the material to produce nanoparticles by evaporation/condensation. A representative example of a low-level physical manufacturing method of nanoparticles is a high-energy pulverization method (High Energy Mi lling), and an example of an upward-oriented method is an inert gas condensation (IGC). In addition to gas phase condensation, the upward-oriented nanoparticle production method includes thermal evaporation, E-beam evaporation, DC sputtering, DC sputtering, and RF sputtering. RFS), Ion Beam Sputtering (IBS), Molecular Beam Epitaxy (MBE), Flame Aerosol Process (FAP), Chemical Vapor Deposition (CVD), Chemical Vapor Synthesis (CVS), Arc Discharge (Arc Discharge) Process) and laser ablation (Laser Ablation) and other methods. The existing physical methods for manufacturing nanopowders generally have the following problems: uneven particle size, difficulty in controlling particle size, inefficient manufacturing processes, contamination, and limitations in mass production. Among the existing methods for physically manufacturing nanoparticles, the most representative methods can be classified into mechanical pulverization, electric blasting, and Inert Gas Condensation (IGC).

Although the mechanical pulverization method is suitable for mass production, it is difficult to control the size of the nanoparticles below 100 nm, and there is a problem of contamination during the pulverization process.

The method of fabricating nanoparticles by electric blasting is to use a pulse power in a vacuum to produce a nanoparticle by instantaneously releasing a charged high voltage and a high current to evaporate/condense on a metal wire of a capacitor. . Since this method utilizes instantaneous blasting, there are disadvantages in that it is difficult to control the size of the nanoparticles and it is necessary to recollect the nanoparticles. Although some attempts have been made to produce nanoparticles by the same method in solution, such methods also require separation of the solution and the nanopowder, so that it is difficult to singulate the process and obtain pure nanoparticles.

Although the inert gas condensation method can produce a nanopowder of higher purity, the materials that can be used for manufacturing have limitations. The inert gas condensation process requires the nanoparticles to be condensed after the cooling rods, and the condensed nanoparticles need to be recollected. If it is to be applied to the final product, it needs to be processed through additional processes, so it is not suitable for mass production. The nanopowder produced by the inert gas condensation method is rapidly oxidized in the atmosphere, so it can be applied to the product immediately after being recovered in a vacuum chamber, or a small amount of oxygen is injected into the vacuum chamber to slowly oxidize the nanopowder. The surface facilitates the removal of nanopowder in air. Most of these methods do not use supports that are directly used in the application when manufacturing nanopowders. The nanopowder ^[ ^1-11] manufactured by the support is easy to take, and when the constituent material of the final product is used as the support, the manufacturing process can be simplified. However, the nano-powder manufacturing devices suggested in the existing patents or papers have low deposition efficiency, wide nano-particle size distribution, uneven support agitation, excessive load on the support, and durability of the device. Low question. In particular, when manufacturing a nanoparticle production apparatus for mass production, there is inefficient continuous deposition, and the support is unevenly stirred. The durability of the equipment is low, the overload of the agitating structure, and the pulverization of the support due to the load between the supports.

In the case of continuous deposition, particles will form nuclei and the nuclei will grow. When the nuclei grow to overlap with adjacent nuclei, nanosized particles will rapidly grow into thin films. The use of a support to produce a uniform and stable nanopowder is important for discontinuous deposition, i.e., controlling the time and non-deposition time of nanomaterial deposition on the support. By appropriately controlling the deposition time to prevent excessive growth of the nanoparticles, the nanoparticles tend to be stable during the non-deposition time, and even if exposed to the deposition area, the nanoparticles do not continue to grow, forming other nuclei on the support. In addition, to produce pure and uniform size nanoparticles, the support must be uniformly agitated.

Now, various deposition sources have been used in the industrial field (for example, using resistance heating, induced heating, plasma jet, electron beam, laser beam deposition source, and ion beam sputtering, DC (Direct Current) sputtering. A deposition source such as RF (Radio Frequency) sputtering or Electron Cyclotron Resonance (ECR) is applied to a nanoparticle production apparatus to produce a variety of materials such as metals, ceramics, oxides, and organic materials into nanoparticles.

Most of the original physical nanoparticle manufacturing devices were made for research purposes, and their design is only suitable for small-scale production. Such devices are not suitable for industrial mass production. A prior art example of manufacturing nanoparticles by support agitation is shown in Figures 1 - 4.

Most of the nanoparticle manufacturing apparatuses that previously used the support to manufacture nanopowders or chips have been stirred by a horizontal stirring shaft. It is divided into a case where a single agitating shaft is used and a plurality of agitating shafts are used. Fig. 1 and Fig. 2 show an example of a stirring device of a horizontal axis stirring method. Due to the rotation of the agitation tanks 130, 230, the support materials are brought together in one direction, so that the support material cannot be uniformly stirred. The agitating device shown in Fig. 1 has a structure in which the agitating tank 130 rotates in the main body, and adopts a drum-type horizontal axis rotating type stirring structure, and the deposition source 111 is located inside the rotating tub. In Fig. 1, the drum is rotated in one direction 131. The support body 120 cannot be completely stirred during the stirring process, and the rotating drum and the support material slide with each other, and some powders may not be stirred. In particular, the slippage between the cohesive support and the agitation tank is more serious. In order to solve these problems, it is necessary to construct the rotating drum. There is also a problem in that the deposition source is located inside the rotating drum, so if a small or low density support material is used, the deposition source is highly likely to be contaminated. Fig. 2 shows a stirring structure of a horizontal shaft rotating mode in the stirring device, the stirring tank 230 is fixed, and the deposition source 211 is located outside the stirring tank. Fig. 2 is also the same as the apparatus of Fig. 1. Since the rotation of the support body 220 is tilted sideways due to the rotation, and the occurrence of excessive accumulation of the support material in a specific field is caused, it is difficult to achieve uniform agitation of the support material. In addition, when the support material is stirred, the rotating wing (or agitating wing) 231 is exposed to the upper portion, and thus the nanoparticles are deposited on the rotating wing, so that the deposition of the nanoparticles in unnecessary places reduces the deposition efficiency of the nanoparticles. , thus becoming an inefficient process. The use of a single rotating shaft configuration to manufacture a mass production device has certain limitations. To expand the capacity, a plurality of single horizontal axes can be used in series in FIG. When the rotating shafts of the plurality of shafts are provided as described above, the respective rotating shafts are rotated in a certain direction, and the support material is moved in the same direction, so that the effect of being unable to uniformly stir can not be achieved. In order to prevent this, it is necessary to convert the rotation direction of the rotary shaft into a random rotation. The random rotation of the agitator shaft causes friction between the support materials, which is caused by the instantaneous rotation of the rotating shaft direction, resulting in irregular movement of the support material, uneven support agitation, loss of the support material, and durability of the device. Reduce and many other issues. In the manner in which the nanoparticles are fabricated using the support material, continuous movement and uniform agitation of the support material are important. The rapidly changing direction of rotation causes the agitating structure to force the support material, causing severe comminution of the support particles or the support material being instantaneously blown to the outside. In addition, the disadvantage of these devices is that heat is generated by random agitation, so that a heat-resistant support material cannot be used. The pulverization of the support material forms fine particles, thereby generating dust. When the support body flows out of the agitation tank and flows into the vacuum exhaust pipe, the support material will contaminate the vacuum pump, shorten the repair/maintenance period, generate additional repair/maintenance costs, and reduce the production efficiency of the product. In addition, the rapid change of the direction of rotation switches a strong external force on the rotating part, reducing the durability of the device. From the viewpoint of the control layer such as the size, content, and distribution of the nanoparticles, if the support material cannot be stably and uniformly stirred, it is difficult to produce nanoparticles of a certain size. On the whole, most of the nanoparticles formed are more likely to be of different sizes.

Figures 3 and 4 show an example of a stirring device that detaches the horizontal rotating shaft structure to produce nanoparticles. The apparatus shown in Fig. 3 can be regarded as a stirring mode similar to that of Fig. 1, except that the rotating shaft of the stirring tank 330 has an angle from the horizontal, and the deposition source 311 is moved from the inside of the stirring tank to the outer position. A device such as that of FIG. 3 has difficulty in securing a deposition area, so there is a problem in the efficiency of deposition and the fabrication of a large-capacity device. In Fig. 1, the problem indicated in the apparatus is the same, and the phenomenon that the support material slides off from the wall surface occurs, and particularly when the fine powder having cohesive force between the support bodies is stirred, it is difficult to achieve uniform stirring of the fine powder. Therefore, such a device is difficult to solve the uniform agitation of the support powder and to ensure the deposition area problem, thereby reducing the efficiency of the nanofabrication process, and at the same time having limitations in manufacturing a mass production device. Fig. 4 is an example of a stirring device in which a stirring shaft adopts a vertical stirring configuration. Such a device is a very effective method for agitating a solution phase material, but when stirring a solid powder or chip or the like in a solid form, in order to mix the support materials at the upper and lower positions, it is necessary to increase the stirring blade. The speed of rotation or change its construction. When the speed of the stirring wing is increased, not only the mixing efficiency of the upper and lower materials cannot be achieved, but the material surrounding the rotating wing may be crushed by external force. Therefore, such a configuration can be regarded as a pulverizing device which is more suitable as a stirring device than a support material. Summary of the invention

In view of the respective drawbacks of existing nanoparticle manufacturing apparatuses, it is an object of the present invention to provide a stirring apparatus for uniformly mixing a support or a support chip and reducing friction between a support or a support chip. .

Another object of the present invention is to provide a nanopowder manufacturing apparatus for producing a nano powder having a uniform size.

Accordingly, the present invention also provides a method of producing a nanopowder to produce a nano powder of uniform size.

In order to achieve the above object, an embodiment of the present invention provides a stirring device, the stirring device comprising: a stirring tank for supporting a nano material;

a vertical conveying member located in the agitation tank for vertically conveying the support body from a lower portion of the agitation tank to an upper portion of the agitation tank by a spiral rotation;

a support plate located in the agitation tank and at the upper portion of the vertical conveying member for supporting the vertical conveying A support body that is conveyed by the component, wherein the support plate has a tapered shape or a truncated cone shape with a middle height and a low outer circumference.

In order to achieve the above object, an embodiment of the present invention further provides a nano powder manufacturing apparatus, the apparatus comprising:

a stirring tank for supporting the nano material;

a support plate, located in the agitation tank and in an upper portion of the vertical conveying member, for supporting the support conveyed by the vertical conveying member, the support plate being a middle-high, low-cone-shaped cone or frustum shape; and a deposition device, deposition The apparatus includes a deposition source located in the agitation tank and above the support plate for depositing the nanopowder to the support by physical deposition.

In order to achieve the above object, an embodiment of the present invention further provides a method for manufacturing a nano powder, the method comprising:

a loading step for loading the support into the agitation tank and performing deposition source material installation, wherein the agitation tank and the deposition source are disposed in a vacuum chamber in an atmospheric state;

a vacuuming step of venting the vacuum chamber with a vacuum pump to bring the vacuum chamber to a predetermined vacuum;

a stirring and deposition step, stirring the support body by means of stirring of a spiral vertical conveying support, and depositing a nano powder by a physical deposition method to a support in a deposition area while stirring;

The nanopowder acquisition step breaks the vacuum in the vacuum chamber, and the nanopowder attached to the support is obtained from the agitation tank. The nanopowder attached to the support can be processed later or applied directly to the application product.

The nanoparticle manufacturing device of the embodiment of the invention adopts a spiral vertical conveying type support body stirring device to minimize the mechanized load and transport the support body with a certain speed and direction, thereby achieving uniform stirring and improvement of the support body. The deposition efficiency, thereby producing a certain size of nanoparticles, while realizing the mechanical load and the load of the device are minimized, and the nanoparticle manufacturing device for improving the durability of the device is realized. DRAWINGS

The drawings described herein are provided to provide a further understanding of the invention, and are not intended to limit the invention. In the drawing:

1 is a schematic view of a stirring device using a horizontal axis rotation method in the prior art;

2 is a second schematic view of a stirring device using a horizontal axis rotation method in the prior art;

3 is a schematic view of a stirring device using a tilting shaft rotation mode in the prior art;

4 is a schematic view of a stirring device using a vertical rotation mode in the prior art;

5 is a schematic structural view of a nanopowder manufacturing apparatus adopting a vertical conveying method according to an embodiment of the present invention;

6 is a schematic view of an upper support support plate and a spreader according to an embodiment of the present invention;

7 is a simplified example of the structure of a nanopowder manufacturing apparatus in an embodiment of the present invention;

8 is an example of a transmission electron microscope (TEM) image of a silver nanoparticle manufactured by using an existing nano powder manufacturing apparatus;

Fig. 9 is a TEM image example of silver nanoparticles prepared by the nanopowder manufacturing apparatus of the present invention; Figs. 10a and 10b are schematic diagrams showing the distribution of silver nanoparticles prepared by the nanopowder manufacturing apparatus according to the present invention. detailed description

In order to make the objects, technical solutions and advantages of the present invention more comprehensible, the specific embodiments of the present invention will be described in detail below. The illustrative embodiments of the present invention and the description thereof are intended to be illustrative of the invention, but are not intended to limit the invention.

Embodiment 1

Embodiments of the present invention provide a support stirring device and a nano powder manufacturing device for nano powder manufacturing. Fig. 5 is a schematic view showing the structure of a nanopowder manufacturing apparatus adopting a vertical conveying method in the embodiment of the present invention, and Fig. 7 is a more specific example. Referring to FIG. 5 and FIG. 7, the nano powder manufacturing apparatus of this embodiment includes:

a support agitating device comprising: a stirring tank, a vertical conveying member, a support plate 534, And one or more upper rotors (or spreaders) 532;

a deposition device comprising a deposition source located above a support plate of the agitation device for depositing a nanopowder to the support by physical deposition;

a vacuum chamber for accommodating the deposition source and the stirring device, wherein the vacuum chamber is maintained in a vacuum state so that the deposition source and the stirring device are in a vacuum;

A vacuum pump is connected to the vacuum chamber for vacuuming the vacuum chamber to maintain a vacuum in the vacuum chamber. In the embodiment of the present invention, the vacuum degree in the vacuum chamber can be controlled at 5 X 10 ^-1 Torr to 1 X 10 ^-6 Torr as needed, but is not limited thereto. In order to remove moisture, gas or volatile substances from the support, a heating device 536 may be provided outside the agitation tank to heat the support in the agitation tank. When a volatile support is used in the vacuum chamber, a cooling device 536 may be provided outside the agitation tank to cool the support in the agitation tank. It is also possible to provide heating and cooling means at the same time to decide whether to open the heating or cooling device as needed.

In the above stirring device:

The vertical conveying member is located in the agitation tank 530 for vertically conveying the support body 520 from the lower portion of the agitation tank to the upper portion of the agitation tank. In this embodiment, the vertical conveying member further includes: a rotating shaft and a fixed A spiral rotor on the rotating shaft. For convenience of description, the vertical conveying member may also be referred to as a spiral main rotating shaft 531 or a spiral bolt.

The support plate 534 is located at an upper portion of the vertical conveying member for supporting the support body conveyed by the vertical conveying member, and the support plate is preferably disposed in the middle (close to rotation) in order to facilitate the sliding of the support body on the support plate. Axis) High, peripheral (away from the axis of rotation) Low cone or frustum shape. Optionally, an outer circumference of the spiral main rotating shaft 531 may be provided with a separating cylinder, and an upper portion of the cylinder may be integrally or fixedly connected with the supporting plate, and a gap between the lower portion of the cylinder and the bottom of the stirring tank may be The support is moved to the main rotation shaft through the gap, and the support is moved to the upper portion of the agitation tank by the rotation of the spiral rotor. Of course, the length of the spacer cylinder can also be set shorter, such as only enclosing the upper portion of the spiral main rotating shaft to expose the lower portion. The support plate and the isolation tube can be fixed in the agitation tank by various existing methods (such as by a bracket or the like), and will not be described in detail herein. The one or more upper rotors (or spreaders) 532 are located on the support plate for agitating the support on the support plate.

The support on the support plate is moved to the edge of the support plate and dropped into the agitation tank when it is dropped.

Since the rotation of the main rotating shaft 531 is rotated in a certain direction, not only the external force to the support material is minimized, but also the phenomenon that the support powder is pulverized is minimized, and the support material is moved to the rotation of the spiral bolt 531 to In the upper portion, the support material that moves to the upper portion passes through the deposition region while moving along the inclined surface of the support support plate 534. The deposition material to be deposited on the deposition source may use noble metals or oxides such as gold, silver, platinum, rhodium, ruthenium, palladium, iridium, osmium, etc., organic compounds, alloys, common metals (such as aluminum A1), bismuth (Se), silicon ( Materials such as Si) and germanium (Ge) are used as deposition materials for deposition sources. In the case where the deposition material is electrically conductive, methods such as DC sputtering and ion beam sputtering may be used. In the case where the deposition material does not have conductivity, RF sputtering, ion beam sputtering, or the like may be employed, but In this connection, intermediate frequency sputtering, microwave deposition, double magnetic sputtering, thermal deposition, electron beam deposition, laser deposition, electron cyclotron resonance or ion plating may also be employed. In the deposition area, due to the rotation of the upper agitating wing ( spreader) 532, the support material moves with the inclined surface of the support plate 534, thereby achieving uniform agitation. The support moved to the edge of the support plate is dropped into the support agitation tank to obtain a stabilized non-deposition time for the nanoparticles deposited on the support. In order to control the time during which the nanoparticles are deposited onto the support, holes 612 are drilled in the support plate (as shown in Figure 6) to allow the support to fall quickly from the support plate, thereby controlling the support exposure time and thereby controlling the deposition. The time the material is deposited onto the support. Both the number of holes and the size of the aperture can be varied. Controlling the support exposure time in the deposition zone essentially means adjusting the ratio of non-deposition time to deposition time to achieve control of the nanoparticle size of the support surface. In the present invention, in order to smoothly move the support body downward, when the stirring tank 530 is designed, the lower portion is made smaller than the upper portion (i.e., the upper portion is thicker and thinner). At least one lower rotating wing 533 is also installed in order to uniformly agitate the lower support (each layer may be different in angle from the main rotating shaft, and two or more rotating wings may be provided in each layer). The upper rotary wing and the lower rotary wing may be fixed to the spiral main rotation shaft 531 (but are not limited thereto). The support material moved to the agitation tank 530 is slowly moved to the lower part of the agitation tank as the lower rotary wing 533 is continuously stirred, and moved The support moved to the main rotating shaft 531 is moved to the upper portion of the stirring tank again by the rotation of the bolt. Repeatedly doing such a process, the nanoparticles supplied by the deposition source adhere to the surface of the support in the form of a powder or chip. The agitator structure of the present invention is constituted by a main-rotation shaft for conveying a support of a spiral type, an auxiliary agitating blade for upper agitation, an auxiliary agitating blade for agitating a lower support body, and the like, and a helical rotary shaft 531 adopting a vertical transfer method. To minimize the external force applied to the support. Further, in the structure of the agitator of the present embodiment, in order to improve the deposition efficiency in the deposition region, a structure in which the upper support agitating portion 532 is not exposed to the deposition source is formed, that is, the upper rotary wing is buried on the support plate. In the support body. The nanoparticle manufacturing apparatus having the above-described agitator structure according to the embodiment of the present invention has a uniform stirring property of the support material and a deposition efficiency in the deposition region, compared with the conventional support stirring method. The advantage of preventing the pulverization of the support or the like since the external force applied to the support is minimized during the stirring process. The nanoparticle manufacturing device of the embodiment of the invention minimizes the pollution of the vacuum pump and the load of the stirring shaft, reduces the maintenance cost of the equipment, and improves the durability of the equipment. The nanoparticle manufacturing apparatus according to the present invention can easily manipulate the surface area of the support volume when compared with the deposition area in the control of the nanoparticle, and can easily adjust the ratio of the deposition time to the non-deposition time, and is generally easy to adjust the nanoparticle. size. The nanopowders produced by the nanopowder manufacturing apparatus of the present invention may have an average size ranging from 1 nm to 500 nm, and the nanopowder deposited on the support may be in the range of 1 ppm to 10, OOO ppm.

The process flow of the nanoparticle manufacturing apparatus of the embodiment of the invention is divided into selecting a nano material and a support material, loading a nano material and a support material in a loading stage, a vacuum exhaust stage, a nano powder manufacturing (stirring/depositing) stage, and breaking The vacuum stage, the stage of taking out the nanopowder and the support material. To make nano-powders, first select the appropriate nano-target materials and support materials in the application field. As a pretreatment of the nanopowder manufacturing process, in order to enhance the adhesion between the support and the nanoparticles, the surface of the support may be pretreated in advance using physical or chemical methods commonly used in the prior art. As a process preparation, after the nano material and the support material are selected in the loading stage, the nano material ingot is mounted on the deposition source, and the support material is charged into the stirring tank. In the vacuum exhaust stage, the first vacuum is started by the low vacuum pump under atmospheric pressure, and after the appropriate vacuum is reached, the high vacuum pump is used. The second vacuum is exhausted. In order to effectively remove the air present between the air or the support contained in the support material during vacuum evacuation, the support material contained in the agitation tank may be stirred by a stirrer. At this time, in order to more effectively remove the air in the vacuum chamber, a heating device (536) as shown in Fig. 5 may be provided outside the stirring tank. In the case where a volatile support is used in the vacuum chamber, the temperature in the vacuum chamber can be lowered by installing a cooling device (536), thereby reducing the degree of support. After the vacuum evacuation process is completed, a process of growing nanoparticles on the support by the deposition source is entered. In this step, the stirring method of the spiral type vertical conveying support body is adopted, and the bottom and upper support bodies can also be assistedly stirred. The nanomaterial supplied from the deposition source grows on the support material into nanometer-sized particles. During the deposition/stirring stage, when the particles deposited on the support are exposed to the deposition source, the particles will grow, and the nanoparticles of a certain size will move from the exposed field to the inside of the stirred tank with the stirring of the support. The nanoparticles moving into the inside of the agitation tank are stabilized again before the support is exposed to the deposition field, and a certain size of nanoparticles is formed. If the nanoparticles are exposed to the deposition area before stabilization, the nanoparticles will grow more and are likely to grow into very large nanoparticles. The size of the nanoparticles formed on the support can be adjusted by adjustment of deposition time and non-deposition time. In the stirring/deposition process, the ratio of the deposition rate (Deposition Rate), the deposition time, the deposition time to the non-deposition time (related to the inclination of the support plate, the number and size of the holes on the support plate), and the stirring speed can be adjusted. The size and content of the nanoparticles are controlled by conditions such as the temperature of the evaporation source, the temperature of the support, the degree of vacuum, the ratio of the total surface area of the support exposed to the deposition area to the volume of the total support, and the like. Compared with the existing nanopowder manufacturing method, the main improvement lies in the manner of stirring of the support. For other details, such as how to charge the evaporation source, how to evaporate, how to evacuate, etc., it can be done by those skilled in the art. Therefore, the detailed description thereof is omitted in the present invention. After the completion of the nanoparticle production process, as a final stage, the vacuum in the vacuum chamber is broken, and the support to which the nanopowder is attached is taken out from the stirring tank. A further advantage of the nanopowder manufacturing process according to the present invention is that if the material of the final application product structural material is selected for use as a support material, the process can be simplified, and since it is not added with other additives, it is environmentally friendly. , and can maximize the inherent properties of nanopowders. 8 and 9 are transmission electron microscopes (TEM) of silver nanopowders produced by a nanopowder manufacturing apparatus using a conventional horizontal rotating shaft and a nanopowder manufacturing apparatus having a vertical transfer rotating shaft of the present invention, respectively. Image example. As is apparent from Figs. 8 and 9, the distribution of the nanoparticles produced by the nanoparticle production apparatus of the present invention is more uniform.

Fig. 10a and Fig. 10b show examples of the size distribution of the nanopowders produced by the conventional nanopowder manufacturing apparatus and the apparatus for producing nanopowder of the present invention, respectively. Figure 10a compares the size distribution of nanopowders at 2-30 nm, and Figure 10b compares the size distribution of nanopowders above 10 nm. Wherein A represents silver nanoparticles produced by a conventional stirring method, and B represents silver nanoparticles produced by the stirring method of the present invention. Figures 10a and 10b show the results of the relative transformations based on the largest number of particle sizes (i.e., the peaks of the two curves are normalized). As shown in Figs. 10a and 10b, many of the large particles produced by the uneven stirring can be observed in the nanopowder produced by the conventional stirring method. The nanopowder produced by the stirring method of the present invention can observe that the number of large particles is relatively small. Therefore, the mixer using the vertical conveying method can achieve uniform agitation and suppress the formation of large nanoparticles.

8 to 10a and 10b illustrate the nanopowder prepared by the present invention by taking silver nanopowder as an example, but the present invention is not limited thereto. With the nanopowder manufacturing apparatus of the present invention, nano powders of other materials can also be prepared, and other metals (such as gold, platinum, rhodium, ruthenium, palladium, iridium, ruthenium, etc.) and oxides can be prepared as well. Nano-powders of materials such as organic compounds, alloys, and semiconductors (such as Se, Si, and Ge).

For the nano-powders produced by the existing agitation method, the nanoparticles below 10 nm can account for 89.9% of all the nanoparticles, and the nanoparticles above 10 nm account for 10.1% of all the nanoparticles. For the nano-powder produced by the vertical transport method according to the present invention, the nano-powder of metal or other materials (such as oxide, organic, alloy, Se, Si, Ge, etc.) can be adjusted by adjusting the appropriate experimental conditions. The following indicators can be achieved: Nanoparticles below 10 nm account for 90% to 96.1% of all nanoparticles, and nanoparticles above 10 nm account for 3.9% to 10% of all nanoparticles. And, by adjusting the aforementioned deposition time, the ratio of deposition time to non-deposition time, and the stirring speed Conditions such as degree, can control the production of nano-powder to meet the predetermined indicators, for example, can control the production of nano-powder, so that nanoparticles below 10 nm account for 91%, 93%, or 96%, etc., and / or more than 10 nm The nanoparticles account for 5%, 6%, or 8% of all the nanoparticles, but are not limited thereto.

The nanoparticle production apparatus of the present invention is formed by a process of depositing nanoparticles on a powder or a chip as a supporter by a physical deposition method as exemplified above. The invention adopts a continuous deposition method to control the growth of nanoparticles, and has an effective device for controlling the size and content of mass production of nano powder.

The present invention is an excellent nano-powder manufacturing apparatus which enhances deposition efficiency and durability by a highly efficient support body stirring method compared with the existing support body stirring method. The nanoparticle production method used in the present invention belongs to an upward physical physical method nanoparticle production method for forming nanoparticles in a vacuum. The nanoparticle manufacturing device of the invention adopts a spiral vertical conveying mode support body stirring mode to minimize the mechanized load and transport the support body with a certain speed and direction, thereby achieving uniform stirring of the support body and improving deposition efficiency. In order to manufacture a certain size of nanoparticles, a nanoparticle manufacturing apparatus that achieves mechanical load and equipment load minimization and improves equipment durability is realized.

In the nanoparticle manufacturing apparatus of the present invention, the stirring method adopts a method of conveying the support powder or the chip in a vertical manner to minimize the friction between the support or the support chip, and uniformly mix the nano particles. Efficiency and durability of nanoparticle manufacturing equipment are related inventions suitable for mass production equipment. The present invention is a process of agitating a support powder or a chip in a vacuum while further including depositing a nanomaterial on a powder or a chip by a deposition device.

The above described specific embodiments of the present invention are further described in detail, and are intended to be illustrative of the embodiments of the present invention. The scope of the protection, any modifications, equivalents, improvements, etc., made within the spirit and scope of the invention are intended to be included within the scope of the invention. [I] British Patent Application Publication No. GB1537839.

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[3] High-dispersion d.c. sputtered platinum-titania powder catalyst active in ethane hydrogenolysis, J. Phys. Chem. 93 (1989), p. 1510.

[4] Nanoparticles of gold on γ-Α1203 produced by dc magnetron sputtering, J. Catal. 231 (2005), p.151.

[5] Gold catalysts prepared by coprecipitation for low-temperature oxidation of hydrogen and of carbon monoxide, J. Catal. 115 (1989), p. 301.

[6] A technique for sputter coating of ceramic reinforcement particles, Surf. Coat. Technol. 91 (1997), p. 64.

[7] Catalysis by Gold, Catal. Rev.-Sci. Eng. 41 (1999), p. 319.

[8] Gold: a relatively new catalyst, Catal. Today 72 (2002), p. 5.

[9] Surface treatment of aluminum oxide and tungsten carbide powders by ion beam sputter deposition, Surf. Coat. Technol. 163-164 (2003), p. 281.

[10] Gold as a Novel Catalyst in the 21st Century: Preparation, Working Mechanisms and Applications, Gold Bull. 37 (2004), p. 27

[I I] Oxidation of CO on Gold Supported Catalysts Prepared by Laser Vaporization: Direct Evidence of Support Contribution, J. Am. Chem. Soc. 126 (2004), p. 1199.

[12] Korean Patent Application No. KR1005862700000.

Claims

A nano powder manufacturing apparatus, characterized in that the apparatus comprises:

a stirring tank for supporting the nano material;

a support plate located in the agitation tank and at the upper portion of the vertical conveying member for supporting the vertical conveying right

a support body to which the component is conveyed, the support plate is a cone-shaped or frustum-shaped shape having a middle height and a low circumference; and a deposition device including a deposition source located in the agitation tank and above the support plate for utilizing The physical deposition method deposits a nanopowder onto the support.

2. The manufacturing apparatus according to claim 1, wherein the manufacturing apparatus further comprises: one or more upper rotary blades on the support plate for agitating the support on the support plate .

The manufacturing apparatus according to claim 1, further comprising: one or more lower rotary blades located in the agitation tank for agitating the support in the agitation tank.

The manufacturing apparatus according to claim 2 or 3, wherein the vertical conveying member comprises: a rotating shaft and a spiral rotating wing fixed to the rotating shaft.

The manufacturing apparatus according to claim 4, wherein the upper rotating wing and the lower rotating blade are fixed to the rotating shaft.

6. The manufacturing apparatus according to claim 1, wherein:

The upper rotating wing is embedded in a support on the support plate.

7. The manufacturing apparatus according to claim 1, wherein:

One or more holes are provided on the support plate.

8. The manufacturing apparatus according to claim 1, wherein:

The stirring tank is thick and thin.

9. The manufacturing apparatus according to claim 1, further comprising: a heating device provided outside the stirring tank for heating the support in the stirring tank.

10. The manufacturing apparatus according to claim 1, further comprising: a cooling device disposed outside the agitation tank for cooling the support in the agitation tank.

11. The manufacturing apparatus according to claim 1, further comprising: a vacuum chamber disposed outside the deposition source and the agitation tank;

A vacuum pump is used to extract the gas in the vacuum chamber to keep the inside of the vacuum chamber in a vacuum state.

12. The nanopowder manufacturing apparatus according to claim 1, wherein:

The material of the deposition source includes at least one of a metal, an oxide, an organic compound, an alloy, and a semiconductor.

13. The nanopowder manufacturing apparatus according to claim 12, wherein:

The metals are gold, silver, platinum, rhodium, ruthenium, palladium, iridium and osmium.

14. The nanopowder manufacturing apparatus according to claim 1, wherein:

The physical deposition methods include: direct current sputtering, radio frequency sputtering, medium frequency sputtering, ion beam sputtering, microwave deposition, double magnetic sputtering, thermal deposition, electron beam deposition, laser deposition, or ion plating.

15. A nano powder manufacturing method, characterized in that the method comprises the following steps:

The nanopowder acquisition step destroys the vacuum in the vacuum chamber, and the nanopowder attached to the support is obtained from the agitation tank.

16. The method of claim 15 wherein:

The evacuating step further includes agitating the branch by a stirring method of a spiral vertical conveying support Hold the body.

17. The method of claim 15 wherein:

The agitation and deposition step further includes cooling the support in the agitation tank.

18. The method of claim 15 wherein:

The loading step also includes pre-treating the support prior to the loading step.

19. The method of claim 15 wherein:

20. The method of claim 15 wherein:

The deposition source material includes: a metal, an oxide, an organic, an alloy, or a semiconductor.

21. A stirring device for nano powder manufacturing, characterized in that the device comprises: a stirring tank for supporting a nano material;

The support plate is located in the agitation tank and in the upper portion of the vertical conveying member for supporting the support conveyed by the vertical conveying member, and the support plate has a tapered shape or a truncated cone shape which is high in the middle and low in the outer circumference.

22. The agitation device of claim 21, further comprising: one or more upper rotors on the support plate for agitating the support on the support plate.

The agitation device according to claim 21, further comprising: one or more lower rotary blades located in the agitation tank for agitating the support in the agitation tank.

24. A stirring apparatus according to claim 22 or 23, wherein:

The vertical conveying member includes: a rotating shaft and a spiral rotating wing fixed to the rotating shaft.

25. The agitation device of claim 24, wherein:

The upper rotary wing and the lower rotary wing are fixed to the rotating shaft.

26. The agitation device of claim 21, wherein:

The upper rotating wing is embedded in a support on the support plate.

27. The stirring apparatus according to claim 21, wherein:

One or more holes are provided on the support plate.

28. The stirring apparatus according to claim 21, wherein:

The stirring tank is thick and thin.

The agitation device according to claim 21, further comprising: a heating device disposed outside the agitation tank for heating the support in the agitation tank.

30. The agitation device according to claim 21, further comprising: a cooling device disposed outside the agitation tank for cooling the support in the agitation tank.