JP5908623B1 - Nanoparticle production system - Google Patents

Abstract

The present invention provides a nanoparticle manufacturing system capable of preventing optical effects such as reflection and refraction from being affected by a cooling liquid in a cavity. A cooling liquid is introduced into the ablation cavity 11 and laser light provided from a laser source 14 is guided directly to the surface of the target material 2 located in the ablation cavity 11 using an optical conduit 15. A nanoparticle manufacturing system that controls the distance between the light outlet end 152 of the optical conduit 15 and the target material 2 to a specific distance (<5 mm). [Selection] Figure 2

Description

  The present invention relates to the technical field of nanoparticles, and more particularly to a nanoparticle production system.

  A nanoparticle is a solid fine granule composed of dozens to hundreds of atoms, generally means an ultrafine granule having a particle size of between 1 nm and 100 nm, and has very special physical properties. And has chemical properties. In the chemical field, an extremely high catalytic efficiency appears for a catalyst prepared using nanotechnology. In the electronic field, nano-level metal conductors are created in a metal mesh and applied in a touch panel. Also, special metals such as aluminum and lead are made into superconductors by nanotechnology. As can be seen from this, nanotechnology and nanomaterials have already been widely applied in fields such as chemistry, materials, photoelectrics, biology and medicine.

  In view of the widespread application of nanomaterials, scientists actively try to research and develop methods for producing various nanogranules or nanounits. The preparation of metal nanoparticles can be divided into a laser ablation method, a metal vapor synthesis method, and a chemical reduction method. Among them, the laser ablation method is commonly used as a method for producing nanogranules or nanounits.

  Referring to the block diagram of the conventional laser ablation facility shown in FIG. As shown in FIG. 1, a conventional laser ablation equipment 1 ′ includes a laser source 10 ′, a substrate 11 ′, a focusing lens 12 ′, an ablation cavity 13 ′, a first mixing cavity 14 ′, and a first mixing cavity 14 ′. A pump 15 ′, a second mixing cavity 14a ′, and a second pump 15a ′ are provided. Among them, the substrate 11 'is installed at the bottom of the ablation cavity 13', and a target material 2 'such as metal black is placed thereon.

  Following the above, the laser light emitted from the laser source 10 'is focused through the focusing lens 12', and the laser light is transparent window 130 'installed at the top of the ablation cavity 13'. And is injected toward the target material 2 'placed at the bottom of the ablation cavity 13'. When a metal ablation phenomenon occurs on the target material 2 ′ by irradiation with laser light whose power is controlled to 90 mJ / pulse, a high-density metal atomic cloud is generated on the target material 2 ′. Further, a plurality of metal nanoparticles are generated in the ablation cavity 13 ′ by the action of the surfactant 3 ′ injected into the ablation cavity 13 ′ (for example, abbreviated as sodium dodecyl sulfate, SDS).

As shown in FIG. 1, the generated metal nanoparticles are transferred to the first mixing cavity 14 ′ and the second mixing cavity 14 a ′ via the first collection conduit 131 ′ and the second collection conduit 131 a ′, respectively. Is done. Among them, the first pump 15 'feeds the first polymer solution through the first solution feed pipe 151' into the first mixing cavity 14 ', and the second pump 15a'. The second polymer solution (or the first polymer solution) is fed into the second mixing cavity 14a ′ through the second solution feeding pipe 151a ′. Thus, the plurality of metal nanoparticles and the first polymer solution are mixed in the first mixing cavity 14 ′ so as to be the first nanopolymer solution, and the plurality of metal nanoparticles and the second polymer solution are mixed. Are mixed in the second mixing cavity 14a ′ so as to be the second nanopolymer solution.
Finally, the first nano polymer solution and the second nano polymer solution are passed through the first discharge pipe 141 ′ and the first discharge pipe 141a ′, respectively, in the first stage product processing section ( By being transported to the first product process stage and the second product process stage, the first composite nano unit and the second composite nano unit are obtained through the next process.

  Although the laser ablation equipment 1 'illustrated in FIG. 1 has already been widely applied to the production of various composite nano products, the laser ablation equipment 1' still has the following main drawbacks.

  (1) In the laser ablation equipment 1 ', it is necessary to precisely control the power of the laser beam to 90 mJ / pulse, and this causes a metal ablation phenomenon on the target material 2'. As can be seen from this, the laser source 10 ′ applied in the laser ablation equipment 1 ′ must be a high-power, high-accuracy laser generator, and the purchase cost is inevitably considerably high. I have to be.

  (2) In addition, the laser ablation equipment 1 ′ focuses the laser beam on the target material 2 ′ using the focusing lens 12 ′, whereby the target material 2 ′ is obtained by the high energy of the laser beam. Causes a metal ablation phenomenon on the top. However, since the surface of the target material 2 ′ (that is, the metal block material) may be uneven, there is a possibility that the plurality of metal nanoparticles generated by the metal ablation phenomenon lack the uniformity of the particle size. is there.

  (3) Subsequent to the first point (1), the surfactant 3 ′ is injected into the ablation cavity 13 ′. Therefore, when laser light is incident on the ablation cavity 13 ′, the Part of the laser light is affected by the surfactant 3 ′ and causes optical effects such as reflection and refraction, leading to a decrease in the incidence rate of the laser light and an increase in the cost of using the equipment.

  Therefore, many disadvantages appear in practical application of the conventional laser ablation equipment 1 '. In view of this, the inventors of the present application have researched and completed the nanoparticle production system of the present invention as a result of research and invention as much as possible.

  The main object of the present invention is to provide a nanoparticle production system different from conventional nanoparticle production facilities. This nanoparticle manufacturing system uses an optical conduit to guide laser light provided from a laser source directly to the surface of a target material located in the ablation cavity, which allows the laser light to be cooled in the ablation cavity. For example, it is possible to prevent an optical effect such as reflection or refraction from occurring. In addition, in the nanoparticle production system provided by the present invention, the distance between the light outlet end of the optical conduit and the target material is controlled to a specific distance (<5 mm). With this design, even if the laser beam provided from the laser source is a low-power (<30 mJ / pulse) laser beam, the laser beam is laser ablated to convert the target material into a plurality of nanoparticles. Can be created.

  Therefore, in order to achieve the main object of the present invention, the inventors of the present application submit a nanoparticle production system.

  Such a nanoparticle manufacturing system is connected to the ablation cavity via an ablation cavity provided with a transparent window on the top thereof, a substrate provided in the ablation cavity for placing a target material, and a cooling liquid transport pipe. A cooling liquid input device for allowing cooling liquid to flow into the ablation cavity, a laser source for providing laser light, and at least one light conduit having a light introducing end and a light leading end. A first distance is separated between the liquid level height of the liquid and the installation height of the transparent window, and a second distance is separated between the liquid level height and the surface of the target material. Is coupled to the laser source, and the light exit end extends into the ablation cavity, thereby A third distance is provided between the end and the surface of the target material, and the laser light is introduced into the ablation cavity via the at least one optical conduit and emitted toward the target material. Thereafter, the target material is ablated by the laser beam so as to become a plurality of nanoparticles.

It is a block diagram of the conventional laser ablation equipment. It is a typical block diagram of the nanoparticle manufacturing system of this invention. It is a typical connection block diagram of an ablation cavity, an optical conduit, and a low-pressure homogenizer. It is a 1st typical block diagram of a nano unit manufacturing system. It is a 2nd schematic block diagram of a nano unit manufacturing system.

  In order to more clearly describe the nanoparticle production system submitted by the present invention, a preferred embodiment of the present invention will be described in detail below with reference to the accompanying drawings.

  FIG. 2 is a schematic configuration diagram of the nanoparticle production system of the present invention. As shown in FIG. 2, the nanoparticle production system 1 includes an ablation cavity 11, a substrate 12, a cooling liquid input device 13, a laser source 14, at least one optical conduit 15, and a target material feed. A supply device 1A, a liquid level control device 1B, a low-pressure homogenizer 1C, and a constant temperature system (not shown) are provided. Among them, the ablation cavity 11 is made of polyfluoroethene (PTFE) and a transparent window 111 is provided on the top thereof.

Subsequently, referring to FIG. 2, the schematic connection configuration diagram of the ablation cavity, the optical conduit and the low-pressure homogenizer shown in FIG. 3 will be referred to at the same time. As shown in the figure, the substrate 12 is provided in the ablation cavity 11 for placing the target material 2 thereon. In operation, the operator can feed the target material 2 into the ablation cavity 11 by operating the target material feeding device 1 </ b> A connected to the ablation cavity 11.
In the present invention, the target material 2 is an inert metal target material, and the material of the substrate 12 is the same as the material of the target material 2. The cooling liquid charging device 13 is connected to the ablation cavity 11 via a cooling liquid transport pipe 131 and is used for charging the cooling liquid into the ablation cavity 11. Among them, the cooling liquid may be any one of an organic phase cold condensate and an aqueous phase cold condensate. It should be particularly noted that the first distance d1 is separated between the liquid level height of the cooling liquid and the installation height of the transparent window 111, and the first distance d1 is between the liquid level height and the surface of the target material 2. Two distances d2 are separated. Among them, the liquid level control device 1B connected to the ablation cavity 11 injects / extracts the cooling liquid, and sets the distance between the liquid level and the installation height to the first distance d1. Control.

The laser source 14 provides laser light to the surface of the target material 2 via at least one light conduit 15. As shown in FIGS. 2 and 3, the optical conduit 15 may be either one of an optical fiber or a quartz glass column, and has a light introduction end 151 and a light extraction end 152. The light introduction end 151 is connected to the laser source 14, and the light extraction end 152 extends into the ablation cavity 11, so that the light introduction end 152 is interposed between the light extraction end 152 and the surface of the target material 2. Is separated by a third distance d3.
Further, the laser light is introduced into the ablation cavity 11 through the at least one optical conduit 15, and after being emitted toward the target material 2, a plurality of the target materials 2 are formed by the laser light. Ablated to become individual nanoparticles. Here, since the material of the board | substrate 12 is the same as the material of the target material 2, the point which should be replenished, even if a laser beam injects and passes through the target material 2, the laser beam which injects and passed through the target material 2 is the same. Further, it is emitted toward the substrate 12. By designing in this way, it is possible to prevent the generation of unnecessary contaminants by directly emitting the laser light that has passed through the target material 2 toward the inner wall surface of the ablation cavity 11.

  The nanoparticle production system 1 of the present invention further includes a low-pressure homogenizer 1C and a constant temperature system (not shown), in which the low-pressure homogenizer 1C is connected to the ablation cavity 11 and is contained in the ablation cavity 11. The cooling liquid is circulated to accelerate the plurality of nanoparticles to be generated in the cooling liquid. The constant temperature system is connected to the ablation cavity 11 and maintains the temperature of the cooling liquid.

As can be seen from the above description, the nanoparticle production system 1 as shown in FIGS. 2 and 3 is an ablation laser facility for creating an inert metal target material into a plurality of nanoparticles. Furthermore, the nanoparticle production system 1 as shown in FIG. 2 can be combined with other processing equipment to become a nanounit production system.
A first schematic configuration diagram of the nanounit manufacturing system shown in FIG. 4 will be referred to. As shown in FIG. 4, the nano unit manufacturing system includes a nano particle manufacturing system 1 as shown in FIG. 2, a primary mixing device 16, a polymer material charging device 17, and a secondary mixing device 18. The nano-unit molding device 19, the first high-pressure homogenizer 1D, and the second high-pressure homogenizer 1E are further provided.

  Subsequently to the above, the primary mixing device 16 is connected to the ablation cavity 11 via a nanoparticle transport tube 112, and the polymer material charging device 17 is connected to the primary mixing device via a polymer material transport tube 171. Connected to device 16. With this arrangement, the plurality of nanoparticles pass through the nanoparticle transport pipe 112 and are transported from the ablation cavity 11 to the primary mixing device 16, and at the same time, the polymer material feeding device 17 is Then, the polymer solution is passed through the polymer material transport pipe 171 and the polymer solution is fed into the primary mixing device 16, and the plurality of nanoparticles and the polymer solution are fed into the primary mixing device 16. Mix to make a primary mixed solution. Here, the point to be replenished is that the polymer solution may be either one of an organic phase polymer solution or an aqueous phase polymer solution.

The secondary mixing device 18 is connected to the primary mixing device 16 through a first mixed solution transport pipe 161, and the nano unit forming device 19 is connected to the secondary mixing device 18 through a second mixed solution transport pipe 181. Connected to device 18. With this arrangement, the primary mixed solution is fed from the primary mixing device 16 to the secondary mixing device 18, and the primary mixed solution is nano / high by a remixing process performed by the secondary mixing device 18. Mix to a molecular mixture solution.
Further, the nano / polymer mixed solution is delivered from the secondary mixing device 18 to the nano unit forming device 19 and is formed into a composite nano unit in the nano unit forming device 19. The replenishment point is that in the present invention, the ablation cavity 11, the primary mixing device 16, the secondary mixing device 18 and the nano unit molding device 19 are all installed in a vacuum environment. .

  Further, in order to control the flow rate of the cooling liquid and the polymer solution, the nano unit manufacturing system includes a first flow rate control valve 132 on the cooling liquid transport pipe 131 and the polymer material transport pipe 171, respectively. A second flow rate control valve 172 is additionally attached. In order to accelerate the operations of the primary mixing process and the secondary mixing process, the first high-pressure homogenizer 1D is connected to the primary mixer 16 to mix the plurality of nanoparticles and the polymer solution. At the same time, the second high pressure homogenizer 1E is connected to the secondary mixing device 18 to accelerate the completion of the remixing step.

The nano-unit manufacturing system disclosed in FIG. 4 includes a nano-particle manufacturing system 1, a primary mixing device 16, a polymer material charging device 17, a secondary mixing device 18, a nano-unit molding device 19, as shown in FIG. The high-pressure homogenizer 1D and the second high-pressure homogenizer 1E are, however, not limited to the embodiment of the nano unit manufacturing system.
Reference is made to the second schematic configuration diagram of the nanounit manufacturing system shown in FIG. As shown in FIG. 5, the nano unit manufacturing system includes a nano particle manufacturing system 1 as shown in FIG. 1, and further includes a milling device 1 </ b> R and the polymer material charging device 17. Among them, the milling device 1R is connected to the ablation cavity 11 via the nanoparticle transport pipe 112, and transports the plurality of nanoparticles from the ablation cavity 11 into the milling device 1R. it can. In addition, the polymer material feeding device 17 is connected to the milling device 1R via the polymer material transport pipe 171 and feeds the polymer solution into the milling device 1R. In this way, the plurality of nanoparticles and the polymer solution can be prepared in the powder mill 1R so as to become powder nano units.

  As described above, the components and technical features of the nanoparticle production system of the present invention have been disclosed sufficiently and clearly. Furthermore, according to the above, it can be seen that the nanoparticle production system of the present invention has the following three advantages.

  (1) Unlike the conventional nanoparticle production facility, the nanoparticle production system of the present invention uses the optical conduit 15 to transmit the laser light provided from the laser source 14 into the ablation cavity 11. By guiding directly on the surface, it is possible to prevent the laser light from being affected by the cooling liquid in the ablation cavity 11 and causing optical effects such as reflection and refraction.

  (2) In addition, in the present invention, the distance between the light outlet end 152 of the optical conduit 15 and the target material 2 is controlled to a specific distance (<5 mm). With this design, even if the laser beam provided from the laser source 14 is a low-power (<30 mJ / pulse) laser beam, the laser beam is laser ablated to form the target material 2 with a plurality of nanometers. Can be made into particles.

  (3) Following the above point (2), the present invention controls the distance between the light outlet end 152 of the optical conduit 15 and the target material 2 to a specific distance (<5 mm). The laser beam provided from the laser source 14 can be a plurality of metal nanoparticles having a uniform particle size for the target material 2 even if it has an uneven surface.

  It should be emphasized that the above detailed description specifically describes possible embodiments of the present invention, and the patent scope of the present invention is not limited to these embodiments. As long as the technical spirit of the invention is not departed from, the implementation or modification of the effect is still within the scope of the claims of the present application.

DESCRIPTION OF SYMBOLS 1 Nanoparticle manufacturing system 11 Ablation cavity 12 Board | substrate 13 Cooling liquid injection | throwing-in apparatus 14 Laser source 15 Optical conduit 1A Target material feeding apparatus 1B Liquid level control apparatus 1C Low pressure homogenization apparatus 111 Transparent window 2 Target material 131 Cooling liquid transport pipe d1 1st Distance d2 Second distance d3 Third distance 151 Light introduction end 152 Light extraction end 16 Primary mixing device 17 Polymer material charging device 18 Secondary mixing device 19 Nano unit molding device 1D First high pressure homogenizer 1E Second high pressure homogenizer 112 Nanoparticle transport pipe 171 Polymer material transport pipe 161 First mixed solution transport pipe 181 Second mixed solution transport pipe 132 First flow rate control valve 172 Second flow rate control valve 1R Milling apparatus 1 ′ Laser ablation equipment 10 ′ Laser source 11 ′ Substrate 12 ′ focusing lens 13 ′ ablation cavity 14 ′ first mixing cavity 15 ′ 1st pump 14a ′ 2nd mixing cavity 15a ′ 2nd pump 2 ′ target material 130 ′ transparent window 3 ′ surfactant 131 ′ 1st collection line 131a ′ 2nd collection line 151 ′ 1st solution feed Inlet line 151a ′ Second solution inlet line 141 ′ First outlet line 141a ′ Second outlet line

Claims (15)

A nanoparticle manufacturing system,
An ablation cavity provided with a transparent window on its top,
A substrate provided in the ablation cavity for placing a target material;
A cooling liquid charging device connected to the ablation cavity via a cooling liquid transport pipe and for charging the cooling liquid into the ablation cavity;
A laser source providing laser light;
Comprising at least one light conduit having a light inlet end and a light outlet end;
A first distance is separated between the liquid level height of the cooling liquid and the installation height of the transparent window, and a second distance is separated between the liquid level height and the surface of the target material,
The light introduction end is connected to the laser source, and the light extraction end extends into the ablation cavity, thereby providing a third distance between the light extraction end and the surface of the target material. Separated,
The laser light is introduced into the ablation cavity through the at least one optical conduit, and after being emitted toward the target material, the target material becomes a plurality of nanoparticles by the laser light. Characterized by being ablated,
Nanoparticle production system.   The nanoparticle production system according to claim 1, wherein the cooling liquid is one of an organic phase cold condensate and an aqueous phase condensate.   The nanoparticle production system according to claim 1, wherein the ablation cavity is made of polyfluoroethene (Polytetrafluorene, PTFE).   The nanoparticle manufacturing system according to claim 1, wherein the target material is an inert metal target material.   The nanoparticle manufacturing system according to claim 1, wherein the optical conduit is any one of an optical fiber and a quartz glass column.   2. The nanoparticle manufacturing system according to claim 1, wherein the first distance is smaller than 5 mm, the second distance is smaller than 5 cm, and the third distance is smaller than 5 mm.   A target material feeding device connected to the ablation cavity for feeding the target material into the ablation cavity, and connected to the ablation cavity for detecting the liquid level height of the cooling liquid and the cooling liquid And a liquid level control device for controlling the distance between the liquid level and the installation height to the first distance, and the ablation cavity, and the ablation cavity includes the liquid level controller. A low pressure homogenizer for circulating a cooling liquid to accelerate the plurality of nanoparticles to be generated in the cooling liquid, and connected to the ablation cavity for maintaining the temperature of the cooling liquid The nanoparticle production system according to claim 1, further comprising a thermostat system. Temu.   The nanoparticle manufacturing system according to claim 4, wherein a material of the substrate is the same as a material of the target material.   The nanoparticle manufacturing system according to claim 7, further comprising a milling device connected to the ablation cavity via a nanoparticle transport tube.   A primary mixing device connected to the ablation cavity via a nanoparticle transport tube, and a primary mixing device connected to the primary mixing device via a polymer material transport tube, and feeding a polymer solution into the primary mixing device. A polymer material charging device for mixing the plurality of nanoparticles and the polymer solution into the primary mixing device so as to be a primary mixed solution; and the primary solution via a first mixed solution transport pipe. A secondary mixing device connected to the mixing device; and a nano-unit molding device connected to the secondary mixing device via a second mixed solution transport pipe, wherein the primary mixed solution is extracted from the primary mixing device. The primary mixed solution is fed into the secondary mixing device and mixed into a nano / polymer mixed solution by a remixing step performed by the secondary mixing device, and the nano / polymer mixed solution is Secondary mixing While being sent to put al the nano unit forming device, characterized in that it is molded to the composite nano units in the nano units forming apparatus, nanoparticles manufacturing system according to claim 7.   A plurality of nanoparticles and the polymer are further connected to a milling device via the polymer material transport pipe, and further comprising a polymer material charging device for feeding the polymer solution into the milling device. 11. The nanoparticle production system according to claim 10, further comprising a polymer material charging device for making the solution into a powdery nanounit in the milling device.   The nanoparticle production system according to claim 10, wherein the polymer solution is one of an organic phase polymer solution and an aqueous phase polymer solution. A first high pressure homogenizer coupled to the primary mixing device for accelerating the mixing of the plurality of nanoparticles and the polymer solution;
The system according to claim 10, further comprising a second high-pressure homogenizer connected to the secondary mixing device and accelerating completion of the remixing step.   11. The nanoparticle manufacturing system according to claim 10, wherein the ablation cavity, the primary mixing device, the secondary mixing device, and the inside of the nano unit molding device are all installed in a vacuum environment.   11. The nanoparticle production system according to claim 10, wherein a first flow rate control valve and a second flow rate control valve are mounted on the cooling liquid transport tube and the polymer material transport tube, respectively.

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