KR101620046B1 - Electrospraying nozzle and a preparation method thereof, the nanoparticles synthesized apparatus and method using thereof - Google Patents

Abstract

The present invention relates to an electrostatic spray nozzle, a method of manufacturing the same, and an apparatus and method for synthesizing nanoparticles using the same. More particularly, the present invention relates to an electrostatic spray nozzle The present invention relates to an electrostatic spray nozzle for producing nanoparticles through the droplets, a method for producing the same, and an apparatus and a method for synthesizing nanoparticles using the same.
According to the present invention, various types of paper on which a flow path through which a fluid can flow are used. At this time, a plurality of hydrophobic papers can be stacked to constitute a housing of a nozzle. Capillary phenomenon can be generated by hydrophilic paper in a housing made of hydrophobic paper to enable solution flow, Price and manufacturing process are simple, mass production is great, design change is free, and practicality can be increased.

Description

TECHNICAL FIELD The present invention relates to an electrostatic spray nozzle, a manufacturing method thereof, an apparatus and a method for synthesizing nanoparticles using the same,

The present invention relates to an electrostatic spray nozzle, a method of manufacturing the same, and an apparatus and method for synthesizing nanoparticles using the same. More particularly, the present invention relates to an electrostatic spray nozzle The present invention relates to an electrostatic spray nozzle for producing nanoparticles through the droplets, a method for producing the same, and an apparatus and a method for synthesizing nanoparticles using the same.

Electrospray is a method of spraying a liquid with a surface droplet droplet using only electric force. Electrostatic spraying has many advantages compared to pressure sprayers using air pressure or droplet generators using ultrasonic waves. Although the atomizer using air pressure can spray droplets by spraying a large amount of liquid, the size of the droplets is several tens to several hundreds of micrometers, and it is difficult to obtain droplets of a smaller size due to the characteristics of the mechanical nozzles. On the other hand, a droplet generator using ultrasonic waves can generate liquid droplets at a high concentration by vibrating the liquid surface with ultrasonic waves. However, since the liquid droplets do not have a charge and the concentration is high, the liquid droplets flocculate between droplets and can not generate droplets of uniform size.

On the other hand, electrostatic spraying using electric force is simple to manufacture the system because the shape and structure of the nozzle are simple, and it is very simple to generate droplets of a size of several hundred nm to several tens of μm. In addition, since the droplets have a monodisperse distribution and the surface of the droplet is charged, the droplets do not cohere with each other and the droplet control using the external electric field is easy. Particularly, these advantages are mainly seen in the cone-jet mode, which is the most stable of the electrostatic spray modes.

However, there is a disadvantage in that when the droplet is generated through electrostatic spraying, the amount of spray is too small. Two methods are used to overcome this problem. One is the use of multi-jet mode, which means that several conjuncts are created from one nozzle.

The multi-jet mode electrostatic spraying apparatus and system of the nonconductive liquid using the coaxial groove nozzle for the electrostatic spraying apparatus, which is proposed by Korean Patent No. 10-1235865 for the multi-jet mode, We proposed a micro liquid preparation method using an electrostatic atomizer. The multi-jet method generally increases the amount of spraying due to the formation of multiple cones, but is not widely used due to its own instability and high voltage conditions.

The second method is to increase the number of nozzles, so that the fluid introduced into one hole is divided into several channels and sprayed at the end of each nozzle. As the number of nozzles increases, the amount of spray increases proportionally. Moreover, it is more stable and reproducible than multi-jet mode, and more research has been conducted (W. Deng, Journal of Aerosol Science, 2009). One of these methods is disclosed in Korean Patent No. 10-1260414. This is because the electrostatic spray is uniformly and stably performed by the spray tip formed at the outlet of the slit nozzle, so that large-area coating is possible, A slit nozzle having a spray tip, and a thin film coating method using the slit nozzle.

However, in the case of a multi-channel electrostatic atomizing system, there is a disadvantage in that not all the channels are supplied with an equal amount of fluid. This is a phenomenon caused by the minute energy difference of each of the channels, so that the fluid flows selectively to the lower energy side and flows only in that direction, and is not supplied to the remaining channels. This overloads certain channels, and if a substance is dissolved in the fluid, it will block the nozzles at the end of the channel, making multi-channel spraying impossible.

This phenomenon is particularly pronounced in water, a fluid with a high intermolecular attraction and a high surface tension. Therefore, electrostatic atomization studies on water are very inadequate compared to electrostatic atomization studies on other organic solvents, and there is little research on multi-channel atomization of water.

In order to solve these problems, the present invention proposes an electrostatic spray nozzle capable of producing a droplet of an aqueous solution at low cost, a method for manufacturing the same, and an apparatus and method for synthesizing nanoparticles using the same.

Korean Patent No. 10-1260414

SUMMARY OF THE INVENTION An object of the present invention is to provide an electrostatic atomization nozzle capable of producing paper, a method for manufacturing the same, and an apparatus and a method for synthesizing nanoparticles using the same.

Another object of the present invention is to provide an electrostatic spray nozzle capable of being manufactured in paper and capable of changing the design of the nozzle freely and capable of increasing the spray amount compared to a metal spray nozzle, a method for manufacturing the same, and an apparatus and a method for synthesizing nanoparticles using the same .

Another object of the present invention is to provide an electrostatic spray nozzle having a simple manufacturing process and a high mass productivity, a method for manufacturing the same, and an apparatus and a method for synthesizing nanoparticles using the same.

In order to achieve the above-mentioned object, there is provided a nozzle body, comprising: a supply passage for supplying a fluid; a nozzle having one end connected to the supply passage and the other end opened to the outside; Wherein the injection path includes a hydrophilic porous material for moving the fluid on at least one side of the nozzle.

Stacking a spray induction layer of a hydrophilic porous material on the lower nozzle body, the spray induction layer including a supply passage and a spray passage, the lower nozzle body being formed of a hydrophobic material, Depositing at least two intermediate nozzle bodies of a hydrophobic material on which the supply passage and the spray passage are formed, and stacking an upper nozzle body formed of a hydrophobic material on the laminated middle nozzle body, A method of manufacturing a spray nozzle is proposed.

A pump for storing the aqueous solution and supplying the aqueous solution to the nozzle, a power source for applying a positive (+) voltage to the aqueous solution stored in the pump, a lower part of the static spray nozzle And a collector for collecting liquid droplets ejected from the nozzle, the collector being positioned between the nozzle and the stage, wherein the collector and the collector are spaced apart from each other.

Comprising the steps of: preparing an aqueous solution containing a metal precursor and a reducing agent; spraying the aqueous solution through the nozzle with droplets; mixing the sprayed droplets with an oil and a surfactant mixed solution to produce a metal ion emulsion; And reducing the ionic emulsion to produce metal nanoparticles.

According to the present invention, various types of hydrophilic porous materials on which a flow path through which a fluid can flow are used. At this time, a plurality of hydrophobic materials may be stacked to constitute a nozzle housing, capillary phenomenon may be generated by a hydrophilic porous material inside a housing made of a hydrophobic material to enable solution flow, Accordingly, it is possible to increase the practicality because the manufacturing cost is low and the manufacturing process is simple, mass production is great, and design change is free.

1 is a view showing an electrostatic spray nozzle according to an embodiment of the present invention formed in a single channel;
FIG. 2 is a view showing an electrostatic spray nozzle formed in a dual channel according to an embodiment of the present invention; FIG.
FIG. 3 is a view showing an electrostatic atomizing nozzle according to an embodiment of the present invention formed in a quadruple channel; FIG.
FIG. 4 is a view showing the atomization of the electrostatic spray nozzle according to one embodiment of the present invention; FIG.
5 is a view illustrating a method of manufacturing an electrostatic spray nozzle according to an embodiment of the present invention;
6 is a view illustrating an apparatus for synthesizing nanoparticles using an electrostatic spray nozzle according to an embodiment of the present invention;
FIG. 7 is a flowchart illustrating a method of synthesizing nanoparticles using an electrostatic spray nozzle according to an embodiment of the present invention; FIG.
FIG. 8 is a view showing a spray experiment of a nanoparticle synthesizer using an electrostatic spray nozzle according to an embodiment of the present invention; FIG.
FIG. 9 is a micrograph of gold nanoparticles produced through a nanoparticle synthesis apparatus using an electrostatic spray nozzle according to an embodiment of the present invention. FIG.

An object of the present invention is to provide an electrostatic spray nozzle which can be made of paper and can be freely changed in design, capable of increasing the amount of spraying compared with a metal spray nozzle, And a method for synthesizing nanoparticles using the same.

In order to achieve the above object, the present invention provides a fluid ejecting apparatus including a nozzle body, a supply passage for supplying fluid, a nozzle having one end connected to the supply passage and the other end opened to the outside, Wherein the injection path includes a hydrophilic porous material for moving the fluid on at least one side of the spray path.

Hereinafter, an electrostatic spray nozzle according to an embodiment of the present invention will be described with reference to the drawings.

FIG. 1 (a) and FIG. 1 (b) are views showing that the electrostatic atomizing nozzle according to one embodiment of the present invention is formed as a single channel.

1 (a), an electrostatic spray nozzle 1 according to an embodiment of the present invention may include a nozzle body 10, a supply passage 30, and a spray passage 50.

The nozzle body 10 may be a housing of a nozzle and the nozzle body 10 may be formed of a material such as polyimide (PI), polyethylene terephthalate (PET), polyether naphthalate (PEN), polyethersulfone (PES) Nylon, polyetheretherketone (PEEK), polycarbonate (PC), and polyarylate (PAR).

The supply passage 30 can move the fluid supplied from the outside and can be formed to have a relatively larger width than the injection passage 50.

The injection path 50 is connected to the supply path 30 to form an injection port 55 for injecting the fluid supplied through the supply path 30 into the outside, The width of the flow path is narrowed in the direction of the injection port 55 from the connection end with the supply flow path 30. This may be a means for forming the liquid supplied to the jet passage 50 as a droplet.

1B is a vertical cross-sectional view of the electrostatic atomizing nozzle 1 shown in FIG. 1A. FIG. 1B illustrates a hydrophilic porous material formed on at least one surface of the injection path 50 .

The injection path 50 is formed in the nozzle body 10 to allow the fluid to flow therethrough. At least one surface of the injection path 50 may include a hydrophilic porous material 70. As a means for allowing an aqueous solution containing water to flow well, water basically has a high attraction force between molecules and a large surface tension. Due to such a phenomenon, the aqueous solution may not flow well into the jet passage 50. In order to solve this problem, a hydrophilic porous material 70 may be formed on at least one surface of the injection path 50. When the hydrophilic porous material 70 is formed on one side of the injection path 50, the aqueous solution supplied from the supply path 30 flows through the injection path 50 by the capillary phenomenon of the hydrophilic porous material 70 The flow of the fluid can be easily generated. The hydrophilic porous material 70 may be formed of a hydrophilic paper, and the hydrophilic porous material 70 may be a hydrophilic porous material such as a filter paper, a printing paper, a cardboard, a corrugated cardboard, But are not limited to, one or more of PTFE, silica, polyethylene, polyester, nitrocellulose, polyvinylidene difluoride (PVDF), polysulfone, and cellulose .

Hereinafter, referring to FIGS. 2 and 3, description will be given of a case where at least two jetting ports of the electrostatic atomizing nozzle according to the embodiment of the present invention are provided.

2 (a) is a horizontal sectional view of the electrostatic spray nozzle 2 according to an embodiment of the present invention.

2 (a), an electrostatic spray nozzle 2 according to an embodiment of the present invention includes a nozzle body 10, a supply passage 30, a supply passage 40, a spray passage 50, (60).

The nozzle body 10 may be a housing of a nozzle and the nozzle body 10 may be formed of a material such as polyimide (PI), polyethylene terephthalate (PET), polyether naphthalate (PEN), polyethersulfone (PES) Nylon, polyetheretherketone (PEEK), polycarbonate (PC), and polyarylate (PAR).

The supply passage 30 can move the fluid supplied from the outside and can be formed to have a relatively wider width than the injection passage 50.

The supply path 40 may be a flow path for distributing the fluid introduced from the supply path 30 to the injection path 50. At least one surface of the supply path 40 may be formed of a hydrophilic porous material 70, have.

The injection path 50 can flow a relatively uniform amount of fluid through the supply path 40 and the width of the injection path 55 can be narrowed from the connection end to the supply path 40 in the direction of the injection port 55 do. This may be means for forming the fluid supplied to the injection path 50 in a droplet state. The injection paths 50 are provided to extend two from one another and a droplet may be injected from the injection port 55 of each injection path 50.

The distribution passage 60 can control the amounts of the fluid flowing in the injection passage 50 similar to each other immediately before the fluid moving in the injection passage 50 is injected through the injection port 55 to the outside. This can redistribute the fluid supplied from the supply line 40 to the injection path 50 to produce similarly the amount of liquid droplets ejected through each injection port 55. At this time, the distribution channel 60 may be located at an upper portion of the ejection opening 55 at a distance of 2 mm to 10 mm. If the distribution channel 60 is located at a position less than 2 mm, the redistribution of the fluid may not take place well. If the distribution channel 60 is located at a position exceeding 10 mm, the redistribution of the fluid is performed too quickly, May be lowered.

At least one surface of the supply passage 30, the supply passage 40, the injection passage 50 and the distribution passage 60 may be formed of a hydrophilic porous material 70, (PTFE), silica, polyethylene, polyester, nitrocellulose, polyvinylidene difluoride (PVDF), polyvinylidene fluoride (PVDF) as well as hydrophilic papers, , Polysulfone, and cellulose. However, the present invention is not limited thereto.

2 (b) is a vertical cross-sectional view of the electrostatic atomizing nozzle 2 shown in FIG. 2 (a), and a hydrophilic paper formed on at least one surface of the injection path 50 through FIG. 2 (b) will be described.

The injection path 50 is formed in the nozzle body 10 to allow the fluid to flow therethrough. At least one surface of the injection path 50 may include a hydrophilic porous material 70. The hydrophilic porous material 70 is a means for allowing an aqueous solution to flow well. Basically, water has a high attractive force between molecules and has a large surface tension. Due to such a phenomenon, the aqueous solution may not flow well into the jet passage 50. In order to solve such a problem, a hydrophilic porous material 70 may be formed on at least one side of the injection path 50, and preferably both sides of the injection path 50 may be formed of a hydrophilic porous material 70 have. When the hydrophilic porous material 70 is formed on both sides of the injection path 50, the aqueous solution supplied from the supply path flows along the injection path 50 by the capillary phenomenon of the hydrophilic porous material 70, The flow can be made more smooth and the effect of capillary phenomenon can be further enhanced as compared with the case where the hydrophilic porous material 70 is formed on one side of the injection path 50. At this time, a channel 90 having an empty space must be formed between the hydrophilic porous materials 70 formed on both surfaces. In the case where the passage 90 having no empty space is not formed between the hydrophilic porous materials 70, the flow of the fluid may be further reduced, so that the passage 90 having the empty space through which the fluid flows is preferably formed . The hydrophilic porous material 70 may be selected from the group consisting of polytetrafluoroethylene (PTFE), silica, polyethylene, polyester, nitrocellulose, polyvinylpyrrolidone, But are not limited to, any one or more of polyphenyl dendrifluoride (PVDF), polysulfone, and cellulose.

3 (a) is a horizontal sectional view of the electrostatic spray nozzle 3 according to an embodiment of the present invention.

3 (a), an electrostatic spray nozzle 3 according to an embodiment of the present invention includes a nozzle body 10, a supply passage 30, a supply passage 40, a spray passage 50, (60). This may include four injection paths 50 in a similar manner to the electrostatic spray nozzle 2 of FIG. 2 described above.

The supply passage 30 can supply the fluid to the four injection passages 50 through at least one supply passage 40 in order to supply substantially the same amount of fluid to the four injection passages 50. [ The distribution passage 60 is formed so that the adjacent injection passages 50 are connected to each other so that the amount of the fluid flowing inside the injection passage 50 immediately before the fluid is injected to the outside through the injection port 55 is similar Can be controlled. This may be means for redistributing the fluid supplied from the supply line 40 to the injection path 50 and controlling the amount of droplets ejected through the respective injection ports 55 to be similar to each other. At this time, the distribution channel 60 may be located at an upper portion of the ejection opening 55 at a distance of 2 mm to 10 mm. If the distribution channel 60 is located at a position less than 2 mm, the redistribution of the fluid may not take place well. If the distribution channel 60 is located at a position exceeding 10 mm, the redistribution of the fluid is performed too quickly, May be lowered.

At least one surface of the supply passage 30, the supply passage 40, the injection passage 50 and the distribution passage 60 may be formed of a hydrophilic porous material 70, May be formed of a hydrophilic paper and a polymer material having both a hydrophilic characteristic and a porous characteristic simultaneously. The hydrophilic porous material 70 may be selected from the group consisting of polytetrafluoroethylene (PTFE), silica, polyethylene, polyester, nitrocellulose, polyvinylpyrrolidone, But are not limited to, any one or more of polyphenyl dendrifluoride (PVDF), polysulfone, and cellulose.

3 (b) is a vertical cross-sectional view of the electrostatic atomizing nozzle 3 shown in FIG. 3 (a), and hydrophilic paper formed on at least one surface of the injection path 50 through FIG. 3 (b).

The injection path 50 is formed in the nozzle body 10 so that the fluid can flow. Both surfaces of the injection path 50 may include a hydrophilic porous material 70. The hydrophilic porous material 70 is a means for performing the same function as the above-mentioned contents, and thus a detailed description thereof will be omitted.

The nozzle may be formed with a larger number of injection paths 50 as well as the quadruple nozzle shown in FIGS. 3 (a) and 3 (b). Depending on the number of the injection paths 50, The position of the supply passage 40, and the number of the distribution channels 60 may be changed.

4 is a front view of the electrostatic spray nozzle 3 according to one embodiment of the present invention.

Referring to FIG. 4, the hydrophilic porous material 70 formed on one side of the injection path 50 may include a group 75 extending from the injection path 50. This may be a means for preventing the fluid discharged from the injection port 55 from collecting at the discharge port 55 due to the surface tension of itself and preventing the droplet from being injected properly, It can play a role that can be ejected to the outside. In addition, the group 75 may be formed of a hydrophilic paper.

In order to manufacture the electrostatic spray nozzle,

Aligning the bottom nozzle body formed of a hydrophobic material;

Stacking a spray inducing layer formed of a hydrophilic porous material on the lower nozzle body and including a shape of a spray passage;

Stacking at least two intermediate nozzle bodies of a hydrophobic material having the supply passage and the injection passage formed on the lower nozzle body; And

And laminating an upper nozzle body formed of a hydrophobic material on the laminated intermediate nozzle body.

Hereinafter, a method of manufacturing an electrostatic spray nozzle according to an embodiment of the present invention will be described in detail with reference to FIG.

5 is a view illustrating a method of manufacturing the electrostatic spray nozzle according to the embodiment of FIG.

Referring to FIG. 5, first, the lower nozzle body 110 formed of a hydrophobic material is aligned (S100). The hydrophobic material may be manufactured by coating a hydrophilic material with a hydrophobic material, and the lower nozzle body 110 prevents a fluid inside the nozzle from flowing to a position other than a desired direction as a part of the nozzle housing.

Next, an injection inducing layer 120 formed of a hydrophilic material and including the shape of a flow path for fluid flow is stacked on the lower nozzle body (S110).

The injection inducing layer 120 may have a shape including a shape of the supply passage 30, the supply passage 40, the injection passage 50, the distribution passage 60 and the group 75, Thereby forming a capillary phenomenon. The injection inducing layer 120 may be formed of at least one of polytetrafluoroethylene (PTFE), silica, polyethylene, polyester, polyester, polyvinyl chloride, polyvinylidene fluoride, But is not limited to, any one or more of cellulose, nitrocellulose, polyphenyldendifluoride (PVDF), polysulfone, and cellulose. The injection inducing layer 120 may be formed of at least one of polytetrafluoroethylene (PTFE), silica, polyethylene, polyester, nitrocellulose, polyphenyldendifluoride (PVDF), polysulfone, and cellulose cellulose may be prepared by slicing a material to a certain thickness.

A middle nozzle body made of a hydrophobic material is stacked on the upper portion of the lower nozzle body 110 and the side surface of the injection inducing layer 120. Next, at least one intermediate nozzle body 130 and 140 made of a hydrophobic material is stacked on the injection inducing layer 120 (S120).

The intermediate nozzle bodies 130 and 140 may have the same shape and may be formed in a shape in which the shape of the injection inducing layer 120 is removed. The reason why two or more intermediate nozzle bodies 130 and 140 are stacked is that a flow path of an empty space is formed above the injection inducing layer 120 to allow the fluid to flow. However, when the intermediate nozzle body 130 is formed of a thicker paper than the spray inducing layer 120, it may be composed of only one intermediate nozzle body 130. The intermediate nozzle bodies 130 and 140 are formed in a shape corresponding to the shape of the injection inducing layer 120. The intermediate nozzle bodies 130 and 140 are formed in a shape corresponding to the shape of the injection inducing layer 120, And may include a flow path 60.

Next, a fluid induction layer 150 including a flow path formed in the intermediate nozzle bodies 130 and 140 is stacked on the intermediate nozzle bodies 130 and 140 (S130).

The fluid induction layer 150 may include a shape of the supply passage 30, the supply passage 40, the injection passage 50, and the distribution passage 60. Only the injection inducing layer 120 may be laminated without performing the step S130, so that the capillary phenomenon may occur. However, when the fluid induction layer 150 is provided through step S130, the effect of the capillary phenomenon can be further increased. The fluid guiding layer 150 may be formed of at least one of polytetrafluoroethylene (PTFE), silica, polyethylene, polyester, polyester, polyvinyl chloride, polyvinylidene fluoride, But is not limited to, any one or more of cellulose, nitrocellulose, polyphenyldendifluoride (PVDF), polysulfone, and cellulose. The fluid induction layer 150 may be formed of a material selected from the group consisting of polytetrafluoroethylene (PTFE), silica, polyethylene, polyester, nitrocellulose, polyphenyldendifluoride (PVDF), polysulfone, and cellulose cellulose may be prepared by slicing a material to a certain thickness.

Finally, an upper nozzle body 160 formed of a hydrophobic material is laminated on the laminated intermediate nozzle body 140 (S140).

The upper nozzle body 160 may have the same shape as the lower nozzle body 110 and prevent the fluid in the nozzle from flowing to a position other than the desired direction as a part of the nozzle housing.

After stacking in steps S110 to S140, the nozzles may be manufactured by fixing the stacked layers to each other through an adhesive. In this case, the adhesive is preferably used as a non-water-soluble component. When the adhesive is water-soluble, the adhesive may not be adhered due to the fluid flowing in the nozzle, Do.

According to the present invention, by using the electrostatic spray nozzle according to an embodiment of the present invention,

A nozzle for spraying the aqueous solution into the droplet;

A pump for storing the aqueous solution and supplying the aqueous solution to the nozzle;

A power supply for applying a positive (+) voltage to the aqueous solution stored in the pump;

A stage which is formed at a lower portion of the electrostatic spray nozzle and is grounded; And

And a collecting part located between the nozzle and the stage and collecting droplets ejected from the nozzle. The present invention also provides an apparatus for synthesizing nanoparticles using the electrostatic atomizing nozzle.

Hereinafter, an apparatus for synthesizing nanoparticles using an electrostatic spray nozzle according to an embodiment of the present invention will be described with reference to FIG.

Referring to FIG. 6, an apparatus for synthesizing nanoparticles using an electrostatic atomizing nozzle according to an exemplary embodiment of the present invention includes a nozzle 100, a pump 200, a power source 300, a stage 400, and a collecting unit 500 can do.

The nozzle 100 may be a means for ejecting droplets by electrostatic spraying, and the nozzle 100 is formed of an electrostatic spray nozzle according to an embodiment of the present invention. The injection port of the nozzle 100 is positioned toward the stage and can be located apart from the stage.

The pump 200 may store the aqueous solution in the nozzle 100 and may be a means for continuously supplying the stored aqueous solution to the nozzle 100 at a constant level.

The power supply unit 300 may apply a voltage of 1 V or more as a means for applying a voltage to the aqueous solution stored in the pump 200, but is not limited thereto. A voltage may be applied to the aqueous solution stored in the pump 200 by the power supply unit 300, and the voltage may be a positive voltage. The voltage applied to the aqueous solution by the power supply unit 300 is preferably 1 kV to 15 kV, but is not limited thereto. If the voltage applied to the aqueous solution is 1 kV, the electrostatic spray phenomenon may not occur. If the voltage applied to the aqueous solution exceeds 15 kV, safety may be a problem.

The stage 400 may be spaced apart from the lower portion of the ejection orifice of the nozzle 100 and may be grounded. The stage 400 is a means for causing an aqueous solution flowing from the pump 200 to the nozzle 100 to generate an electrostatic spray phenomenon and a positive voltage applied to the fluid inside the nozzle 100 and a ground voltage applied to the grounded stage 400 And the aqueous solution is formed into a droplet by the electric force, and the formed aqueous solution droplet is ejected in the direction of the stage 400 with a positive (+) voltage applied. At this time, since the aqueous solution droplets have a positive voltage, they can be uniformly sprayed without being clumped together.

The collecting unit 500 may be formed of a non-conductive material as a means for collecting the aqueous liquid droplets jetted from the nozzle 100 in the direction of the stage 400.

Using the nanoparticle synthesis apparatus using the electrostatic spray nozzle,

The present invention relates to a process for producing an aqueous solution comprising a metal precursor and a reducing agent (step 1);

The step of spraying the aqueous solution with droplets by the nozzle (step 2);

The sprayed aqueous solution droplet is mixed with an oil and a surfactant mixed solution to produce a metal ion emulsion (step 3); And

And reducing the metal ion emulsion to produce metal nanoparticles (step 4). The present invention also provides a method for synthesizing nanoparticles using an electrostatic spray nozzle.

Hereinafter, the nanoparticle synthesis method using the electrostatic spray nozzle according to the present invention will be described step by step with reference to the drawings.

In the method for synthesizing nanoparticles using the electrostatic spray nozzle according to the present invention, step 1 is performed to prepare an aqueous solution containing a metal precursor and a capping agent.

The metal precursor may be at least one selected from the group consisting of hydrogen tetrachloroaurate trihydrate [HAuCl ₄ .H ₂ O], silver nitrate [AgNO ₃ ], silver 2-ethylhexanoate [AgOOCCH (C ₂ H ₅ ) C ₄ H ₉ ] [Cu (CH ₃ COO) ₂ ], caprochloride [CuCl ₂ ], hexachloroplatinate hexahydrate [H ₂ PtCl ₆ .H ₂ O], zinc acetate and nickel 2-ethylhexanoate [ _{Ni (OOCCH (C 2 H 5} ) C 4 H 9) 2], Niklas nitrate _{[Ni (NO 3) 2]} , cobalt nitrate hexahydrate _{[Co (NO 3) 2 H} 2 O], ammonium molybdate tetrahydrate _{[(NH 4) 6Mo 7 O} 24 · H 2 O), manganese 2-ethylhexanoate carbonate _{[Mn (OOCCH (C 2 H} 5) C 4 H 9) 2], tungsten chloride hexa [WCl _6], (C ₄ H ₅ ), aluminum 2-ethylhexanonate [AlOH (OOCCH (C ₂ H _{5) 2} ], tetrachloromonium chloride [Cl ₄ Ge], seranium tetrachloride [SeCl ₄ ], iron 2-ethylhexanonate [C ₂₄ H ₄₅ FeO ₆ ] ) C ₄ H ₉ ) ₂ ], aluminum Titanium trichloride [AlCl _3], titanium 2-ethylhexanoate carbonate _{[Ti (OOCCH (C 2 H} 5) C 4 H 9) 2], titanium tetrachloride [TiCl _4], palladium dichloride [PdCl2], indium 2 -Ethyl hexanonate [In (OOCCH (C ₂ H ₅ ) C ₄ H ₉ ) ₂ ] and indium trichloride [InCl ₃ ].

The metal precursor may be at least one selected from the group consisting of ethyl hexanoate, dialkyl isocarbamate, carboxyl acid, carboxylate, pyridine, diamine, arachine, diaracine, phosphine, diphosphine, arenes, chloride, At least one selected from the group consisting of acetonates, metal oxides, carbonyls, carbonates, hydrates, hydroxides, nitrates, oxalates and mixtures thereof.

The reducing agent may comprise trisodium citrate.

The reducing agent may include any one of trisodium citrate, monosodium citrate, potassium citrate, and alcohol.

In the nanoparticle synthesis method using the electrostatic spray nozzle according to the present invention, in the step 2, the aqueous solution is sprayed into the droplet by the nozzle.

In the step 2, a droplet may be generated by the method of electrostatic spraying by the voltage of the power source unit, and a plurality of nozzles may be provided to generate droplets. At this time, the sprayed aqueous solution droplet may be sprayed toward the collecting part and reacted with another material located inside the collecting part.

In the method for synthesizing nanoparticles using the electrostatic spray nozzle according to the present invention, in the step 3, the sprayed aqueous solution droplets are mixed with an oil and a surfactant mixed solution to produce a metal ion emulsion.

The oil may be selected from the group consisting of mineral oil lubricating oil, vegetable lubricating oil, synthetic lubricating oil or a mixture thereof, and the surfactant may include AOT.

In the nanoparticle synthesis method using the electrostatic spray nozzle according to the present invention, the metal ion emulsion is reduced by the step 4 to produce metal nanoparticles.

In the step 4, the metal ion emulsion may be reduced by heating the metal ion emulsion, and the metal nanoparticles may be produced by the reduction method.

Hereinafter, the present invention will be described in more detail with reference to specific examples and experimental examples. The following examples and experimental examples are provided to illustrate the present invention, but the present invention is not limited by the following examples and experimental examples.

≪ Example 1 > Production of paper nozzle

Referring to FIG. 1, one injection path and one supply path are provided, and a hydrophilic porous material is formed on one side of the injection path and the supply path. In addition, the ends of the hydrophilic porous material formed a group. At this time, the nozzle body was made of hydrophobic paper with hydrophobic coating on the filter paper, and the hydrophilic porous material was made of filter paper and adhered using double - sided tape.

≪ Example 2 >

Referring to FIG. 2, one injection path is formed for connecting two injection paths, one injection path is connected to the two injection paths, and one supply path for supplying a fluid to the injection path is connected to the one supply path Wherein a hydrophilic porous material is formed on both sides of the injection path, the distribution path, the supply path, and the supply path, and the end of the hydrophilic porous material on one surface of the amphiphilic porous layer is formed as a bundle , The same procedure as in Example 1 was carried out.

≪ Example 3 >

Referring to FIG. 3, there are provided four injection paths, three distribution paths for connecting adjacent ones of the four injection paths, and one supply path for supplying the fluid to the injection paths Wherein the end of the hydrophilic porous material on one side of the porous porous layer as the injection flow path, the distribution path, the supply path, and the supply path is formed of the two supply paths connected to the one supply path Were prepared in the same manner as in Example 1.

≪ Comparative Example 1 &

Except that a hydrophilic porous material was not formed and a distribution channel was not provided.

≪ Comparative Example 2 &

The same procedure as in Example 2 was carried out except that no distribution channel was provided.

≪ Comparative Example 3 &

The same procedure as in Example 2 was carried out except that a hydrophilic porous material was not formed.

<Experimental Example> Analysis of Electrostatic Spray Nozzle

(1) Available flow rate measurement of electrostatic spray nozzle

In order to confirm the available flow rate of the nozzle of Example 1, spraying was carried out while varying the flow rate by 10 μl / h. When the supply amount is larger than the maximum spray amount, since the surplus amount is released without being sprayed, the time point at which such surplus amount discharge stops is measured. As a result, the available flow rate of a single channel was found to be up to 110 μl / h and a minimum of 70 μl / h depending on the sample.

Spray test was carried out in the same manner as in Experimental Example 1 to confirm the available flow rate of the nozzle of Example 2. As a result, the available flow rate of the dual channel was found to be a maximum of 190 μl / h and a minimum flow rate of 120 μl / h depending on the sample difference.

(2) Spray voltage measurement of nozzle

In order to confirm the driving voltage section of the nozzle of Example 1, the voltage was changed to confirm the change in spray pattern. As a result, it was confirmed that the spraying started at an average of 3.8 kV and the spraying was cut off at about 11 kV.

Spray test was carried out in the same manner as in Experimental Example 3 to confirm the drive voltage section of the nozzle of Example 2. As a result, on the left and right channels, on average 5.1 kV. It was confirmed that spraying started at 5.4 kV, and the section where the spraying stopped was not confirmed.

(3) Droplet size measurement of nozzle

In order to measure the spray droplet size of the nozzle of Example 1, the size of droplets generated during spraying was measured using a Phase Doppler Particle Analyzer equipment. As a result, it was confirmed that an average droplet of 3.37 μm was generated.

In order to measure the spray droplet size of the nozzle of Example 2, the size of droplets generated during spraying was measured in the same manner as in Experimental Example 5. As a result, it was confirmed that droplets of 3.35 μm and 3.55 μm were generated on the left and right channels, respectively.

In the case of the nozzles of Embodiments 1 to 3, droplet spraying proceeded to generate droplets. Especially in the case of Examples 2 and 3, droplets were uniformly sprayed at each jetting port. However, in the case of Comparative Examples 1 to 3, the droplet spraying proceeded, but severe uneven spraying proceeded. From this, the electrostatic spraying nozzle of the present invention including the hydrophilic porous material had an effect capable of supplying uniform droplets .

(4) Spray test of quadrupole electrostatic spray nozzle

A spray test of the nozzle of Example 3 was performed and is shown in FIG. Referring to FIG. 5, it can be seen that even in the case of a quadruple channel electrostatic atomizing nozzle having four jetting ports, jetting of droplets is uniformly and stably performed.

Example 4 Synthesis of Gold Nanoparticles

Step 1: An aqueous solution of 1.18 mg of hydrogen tetrachloroaurate trihydrate [HAuCl ₄ .H ₂ O] and 5 mg of trisodium citrate was prepared in 10 ml of water as a solution to be sprayed. Hydrogen tetrachloroaurate trihydrate [HAuCl ₄ .H ₂ O] is a metal precursor for supplying gold ions, and trisodium citrate serves as a reducing agent for reducing gold ions to form nanoparticles . As an oil to receive the sprayed aqueous solution, 60 mg of the surfactant AOT is dissolved in the industrial olive oil.

Step 2: A voltage of 7 kV was applied to the nozzle manufactured by the method of Example 1 through the power source portion, and the aqueous solution droplet was generated and sprayed by the electrostatic spraying method. At this time, the droplet was injected into the industrial olive oil located in the collecting part with the AOT mixed solution as a surfactant.

Step 3: The aqueous solution droplet is injected into the industrial olive oil located in the collecting part with the AOT mixed solution as the surfactant, and the edge of the droplet is surrounded by the surfactant to form a stable metal ion emulsion.

Step 4: The metal ion emulsion is heated to 90 degrees. Trisodium citrate, which was dissolved in the emulsion, has a property of reducing gold ions to gold nanoparticles when the temperature is elevated. When heated, a reduction reaction occurs in the metal ion emulsion to form gold nanoparticles do.

At this time, the gold nanoparticles produced were observed with a scanning electron microscope, and the results are shown in FIG. As can be seen from the photograph of FIG. 6, it can be confirmed that gold nanoparticles were produced by spraying through a nozzle in Example 4.

10: Nozzle body
30: Supply flow
40: Supply chain
50:
55:
60: Distribution channel
70: hydrophilic porous material
90: Euro in empty space
110: lower nozzle body
120: injection inducing layer
130, 140: Middle nozzle body
150: fluid induction layer
160: upper nozzle body
100: nozzle
200: pump
300:
400: stage
500: collecting section

Claims (17)

A lower nozzle body 110 formed of a hydrophobic material;
An injection inducing layer 120 formed of a hydrophilic porous material and including a supply passage 30 and an injection passage 50;
A middle nozzle body 130 formed of a hydrophobic material and including at least one layer including a supply passage and an injection passage, the one layer existing in the same layer as the injection inducing layer and the at least one layer provided above the injection inducing layer, , 140); And
An upper nozzle body 160 formed of a hydrophobic material; Are sequentially stacked,
A supply passage formed inside the nozzle body for supplying fluid; And an injection port 55, one end of which is connected to the supply passage 30 in the injection-inducing layer and the intermediate nozzle body, and the other end of which is opened to the outside,
And a jet flow path for jetting the fluid supplied from the supply flow path 30 in the jetting inductive layer and the intermediate nozzle body to the outside, wherein the jet flow path 50 in the jetting induction layer and the intermediate nozzle body includes And a hydrophilic porous material (70) for transferring the fluid.
The method according to claim 1,
The nozzle body includes:
(PI), polyethylene terephthalate (PET), polyether naphthalate (PEN), polyether sulfone (PES), nylon, polyetheretherketone (PEEK), polycarbonate (PAR). &Lt; RTI ID = 0.0 &gt; 1 &lt; / RTI &gt;
The method according to claim 1,
The injection path
And the width of the electrostatic atomizing nozzle is reduced in the direction of the jetting port at a connection end connected to the supply passage.
The method according to claim 1,
The injection path
Wherein the capillary phenomenon generated by the hydrophilic porous material moves the fluid in a direction from the connection end connected to the supply passage to the injection port.
The method according to claim 1,
The jetting port
Wherein the width of the electrostatic atomizing nozzle is 1 nm to 1 mm.
The method according to claim 1,
The hydrophilic porous material may be,
And a needle extending out from an injection port of the injection path.
Claim 7 has been abandoned due to the setting registration fee. The method according to claim 1,
The hydrophilic porous material may be,
A polymer selected from the group consisting of polytetrafluoroethylene (PTFE), silica, polyethylene, polyester, nitrocellulose, polyphenyldendifluoride (PVDF), polysulfone, and cellulose Wherein the electrostatic atomizing nozzle comprises:
The method according to claim 1,
The hydrophilic porous material may be,
Wherein the electrostatic spray nozzle is formed of paper.
The method according to claim 1,
At least two injection paths are provided,
Wherein the at least two injection paths
Further comprising at least one distribution channel for redistributing the amount of fluid flowing through each injection path.
10. The method of claim 9,
The distribution channel includes:
Wherein the nozzle is formed at an upper end of 2 mm to 10 mm of the nozzle.
Aligning the bottom nozzle body formed of a hydrophobic material;
Stacking a spray induction layer of hydrophilic porous material on the lower nozzle body and including a supply passage and an injection passage;
Layering a middle nozzle body of a hydrophobic material on the upper portion of the lower nozzle body and the side of the injection inducing layer;
Stacking at least one intermediate nozzle body of a hydrophobic material having the supply passage and the injection passage formed on the injection inducing layer; And
The method of claim 1, further comprising laminating an upper nozzle body formed of a hydrophobic material on the laminated intermediate nozzle body.
12. The method of claim 11,
The step of laminating at least two intermediate nozzle bodies comprises:
And laminating two to five electrostatic atomizing nozzles.
12. The method of claim 11,
The injection induction layer
And a group of elongated forms in the injection flow path.
12. The method of claim 11,
After the step of laminating at least one intermediate nozzle body,
Further comprising laminating a fluid induction layer formed of a hydrophilic porous material and including a shape of the supply passage and an injection path.
15. The method of claim 14,
Between the fluid induction layer and the jetting induction layer,
Wherein a flow path of an empty space is formed to allow the fluid to flow.
An electrostatic spray nozzle according to claim 1 for spraying an aqueous solution into droplets;
A pump for storing the aqueous solution and supplying the aqueous solution to the electrostatic spray nozzle;
A power supply for applying a positive (+) voltage to the aqueous solution stored in the pump;
A stage which is formed at a lower portion of the electrostatic spray nozzle and is grounded; And
And a collecting part located between the electrostatic atomizing nozzle and the stage for collecting droplets ejected from the electrostatic atomizing nozzle.
A method for synthesizing nanoparticles using the apparatus for synthesizing nanoparticles according to claim 16,
Preparing an aqueous solution comprising a metal precursor and a reducing agent;
Spraying the aqueous solution into the droplet through the electrostatic spray nozzle of the nanoparticle synthesizer of claim 16;
Mixing the sprayed droplets with an oil and a surfactant mixed solution to produce a metal ion emulsion; And
And reducing the metal ion emulsion to produce metal nanoparticles.

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