KR101531855B1 - Apparatus for manufacturing nano colloid solution and method thereof - Google Patents

Abstract

The present invention relates to an explosion chamber which receives a metal wire from the outside as a dispersion medium therein and produces a nano-colloid; A storage chamber for transferring the nanocolloid from the explosion chamber through a transfer tube, collecting and storing the nanoparticles dispersed in the nanocolloid; A dispersion inducing unit connected to the conveying tube and forming an electric field around the conveying tube; And a cooling chamber for transferring the nanocolloid having a reduced concentration from the storage chamber and lowering the temperature of the nanocolloid.

Description

[0001] APPARATUS FOR MANUFACTURING NANO COLLOID SOLUTION AND METHOD THEREOF [0002]

More particularly, the present invention relates to a nano-colloid manufacturing apparatus which induces dispersion of nanoparticles upon high-voltage electrical explosion for manufacturing nanocolloids and circulates the nanocolloids produced thereby to produce high-concentration nanoparticles. ≪ / RTI >

In recent years, research on colloidal nanoparticles has been actively conducted with interest in nanotechnology, and methods for preparing nanoparticle dispersion media for utilizing colloidal nanoparticles include electrolysis, sol-gel method, microemulsion method, and chemical reduction method have.

The electrolysis method and the sol-gel method have a disadvantage in that the production cost is high and it is difficult to prepare a large amount of metal colloid, and since the microemulsion method has a complicated manufacturing method, it is difficult to control the size and shape of the particles, have.

The chemical reduction method is widely used in the production of nano metal particle dispersion media because of its simple manufacturing method and its mass production capability by producing nanoparticles by reduction of a metal salt using a dispersion medium having a reducing power in the presence of a polymer dispersion stabilizer, The use of stabilizers and the production of by-products are inevitable, which leads to a disadvantage that the environment-friendliness and purity are inferior.

The electric explosion method uses a pulse power to generate an electrical explosion in a dispersion medium in which a metal wire is blown in the form of fine particles or metal vapor when a high voltage high current passes through a metal wire to manufacture a nano metal particle dispersion medium This process is advantageous in that it can produce nanoparticles of high purity and uniform size, can control the agglomeration of the particles and can control the formation of a coating film, The utilization of the dispersion medium is increasing.

Nanoparticles produced through such an electric explosion method are attracting attention as a core technology that is utilized for medicine, flavor scholarship, and advanced information and communication technology. Particularly, nano-colloids are prepared by dispersing and suspending nano-sized metal particles in a dispersion medium. They are used in various fields such as pharmaceuticals and cosmetics as well as in the production of conductive pastes and inks. Currently, these products are highly functional, It is in the trend of developing toward the pursuit of value.

In addition, with the development of these products, it is required to produce nanoparticles of better quality. However, conventional techniques have a limitation in obtaining high-concentration nano-colloids because of problems such as voltage, agglomeration of particles, and dispersing power.

Therefore, in order to produce a high-quality nano-colloid, an effective method for concentrating finer nanoparticles at a high concentration is needed.

An object of the present invention is to provide a nanocolloid containing fine nanoparticles by inducing dispersion of nanoparticles at the moment of electric explosion for nanocolloid production while applying electric voltage by applying a high voltage, To thereby obtain a nanocolloid having a high concentration. The present invention also provides an apparatus and a method for manufacturing a nanocolloid.

The technical objects to be achieved by the present invention are not limited to the above-mentioned technical problems.

In order to achieve the above object, the present invention provides a nanocolloid manufacturing apparatus comprising: an explosion chamber which receives a metal wire from the outside as a dispersion medium in the inside thereof, manufactures nanocolloids by electric explosion, and guides the nanocolloids to a transfer tube; A dispersion induction unit connected to the transfer tube and forming an electric field around the transfer tube to densify nanoparticles of nanocolloids in the transfer tube; A storage chamber for collecting and storing nanocolloids containing nanoparticles densely packed in the transfer tube; And a cooling chamber for receiving the nanocolloid including nanoparticles not densified through the circulation tube connected to the storage chamber and lowering the temperature of the nanocolloid, wherein the nanocolloid transferred to the cooling chamber is stored in a storage chamber Concentrations may be lower than nano-colloids.

Specifically, the explosion chamber may be made of a metal material.

The explosion chamber may be made of aluminum.

The dispersion induction unit may be an induction electrode in which an anode and a cathode are stacked alternately with an insulator interposed therebetween.

The dispersion induction unit may be installed to operate the nanocolloidal manufacturing apparatus at all times.

According to another aspect of the present invention, there is provided a method of manufacturing a nanocolloid, comprising: (S10) feeding a metal wire into an explosion chamber filled with a dispersion medium; (S20) of generating nanocolloid by electric explosion in the explosion chamber and transferring colloid by electric field; Collecting the nanoparticles dispersed in the colloid (S30); And cooling the colloid including the nanoparticles not collected in the above to re-enter the explosion chamber (S40).

Specifically, the electric explosion in the step S20 may be performed by applying a voltage of 500 to 1500V.

The nanoparticles in step S20 may be particles formed by converting at least 65% of the metal wires in step S10.

In the step S20, the electric field may be constantly formed during the production of the nanocolloid.

Ultrasonic waves may further be irradiated to disperse the nanoparticles in the nanocolloid generated by the electric explosion of step S20.

According to the apparatus and method for producing a nanocolloid according to the present invention, it is possible to produce high-quality nanocolloids containing high-concentration fine nanoparticles and to ensure uniform dispersion of the prepared nanocolloids for a long time can do. In addition, the quality of the secondary processed product made using the nanocolloid produced by the present invention can be improved.

1 is a conceptual diagram of a nanocolloid manufacturing apparatus according to an embodiment of the present invention.
FIG. 2 is a graph of a current waveform curve at a conventional charge voltage of 340 V, and FIG. 3 is a graph of a current waveform curve at a charge voltage of 1223 V of the present invention.
4 is a flowchart of a method of manufacturing a nanocolloid according to an embodiment of the present invention.
Meanwhile, FIG. 5 is a TEM photograph for identifying nanoparticles in a nanocolloid produced using a conventional nanocolloid production apparatus, and FIG. 6 is a TEM photograph showing a nanocolloid produced in the nanocolloid using the apparatus and method of the present invention. It is a TEM photograph for identifying particles.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. In the drawings, the same components are denoted by the same reference symbols whenever possible. In the following description, well-known functions or constructions are not described in detail since they would obscure the invention in unnecessary detail.

1 is a conceptual diagram of a nanocolloid manufacturing apparatus according to an embodiment of the present invention. 1, an apparatus 100 for manufacturing a nanocolloid of the present invention includes an explosion chamber 110, a dispersion induction unit 113, a storage chamber 120, a cooling chamber 130, and a cooling unit 150 do.

The liquid electrical explosion method according to the present invention is to form the metal wire 300 supplied into the explosion chamber 110 into nanoparticles by electric explosion. The metal wire 300 is supplied from the outside by a feeding device 200 separately provided at an upper part of the explosion chamber 110 to be immersed in the liquid dispersion medium 111 received in the explosion chamber 110. That is, the metal wire 300 is supplied from the outside into the explosion chamber 110, is immersed in the dispersion medium 111, and is then formed into nanoparticles by electrical explosion due to the pulse power generated by application of a high voltage current. The feeding and electrical explosion of the metal wire 300 can be repeated several times depending on the concentration of the nanocolloid to be obtained.

Here, the dispersion medium 111 may vary depending on the kind of the nanoparticles, that is, the dispersion medium. Concretely, it is possible to select a dispersion medium (111) as a solvent which can mix well with the dispersion medium in a liquid solvent such as distilled water, water, alcohol, benzene, or acetone.

In this case, the magnitude of the applied high voltage current directly affects the particle size of the metal powder formed in the electric explosion. This is because, as shown in FIG. 2 and FIG. 3, there is a difference in electric explosion conversion efficiency depending on the magnitude of the applied voltage. This conversion efficiency means a quantitative ratio in which the metal wire 300 supplied into the explosion chamber 110 is converted into nanoparticles by electrical explosion.

2 is a current waveform curve when a voltage of 340 V related to the related art is applied. Specifically, the current waveform curve is 2200 kPa, the charging voltage is 340 V, the charging energy is 127 J, the peak current value is 675 A, The width was measured as 71 占 퐏 ec. When the electric explosion was performed under such conditions, the nanoparticles were prepared by the submerged electric explosion method by charging at 340V, and the energy was supplemented by increasing the charging capacity of the capacitor bank. 3 is a current waveform curve when a high voltage is applied according to the present invention. Specifically, the charging curve is a charge curve of 170 ㎌, a charging voltage of 1223 V, a charging energy of 127 J, a peak current value of 825 A, and a pulse width of 59 ec ec Respectively. When the electric explosion was performed under such conditions, the voltage was increased at 127 J, which is the same value as the conventional charge energy, and the charge capacity was reduced to reduce the discharge time.

2 and FIG. 3, the current waveform associated with the prior art of FIG. 2 has a gradual slope, whereas the current waveform associated with the present invention of FIG. 3 has a rising slope It can be confirmed that it is abrupt. This further shortens the heating time in FIG. 3 as compared with FIG. 2, and shortens the instantaneous sublimation time (metal solid: metal gas) caused by cooling by the dispersion medium 111 after nanoparticle formation due to electric explosion . Because of this difference, energy loss is reduced in the present invention and a larger electric explosion energy is secured than in the conventional technique, so that the yield of nanoparticles having finer particle size can be increased. That is, the greater the magnitude of the voltage applied when forming the metal powder by the electric explosion method, the more fine metal powder can be obtained at a high concentration.

However, when an excessive voltage of 3 kV or more is applied when the electric explosion order in the explosion chamber 110 is repeated and the high concentration state is reached, the applied high voltage is not discharged through the metal wire 300 but is dispersed around the metal nanoparticles It may be difficult to generate nanoparticles by electric explosion. Therefore, it is preferable that the voltage is less than 3 kV when electric explosion occurs.

element Content (mg / l) 2 (Prior Art) 3 (present invention) Ni 22.42 321.90

<Table 1> shows the results of the ICP mass spectrometry of the amount of nanoparticles produced by the submerged electric explosion of nickel metal wires under the condition of FIG. 2 and the conditions of FIG. 3, It can be seen that the yield of nanoparticles was improved about 14 times as compared with the conventional method under the high voltage (1223 V) condition of the present invention.

In addition, in the apparatus 100 for manufacturing a nanocolloid of the present invention, the explosion chamber 110 is a portion to which a high voltage of 1000 V or more is applied directly to the explosion chamber 110 to withstand an explosion force of an electric explosion generated when a voltage is applied . The explosion chamber 110 is formed of aluminum or an aluminum alloy, and is useful for realizing the explosion chamber 110 which is light and durable.

A kind of transfer tube 160 is connected to one side of the explosion chamber 110. The transfer tube 160 is connected between the explosion chamber 110 and the storage chamber 120 so that the nanocolloid generated by the electric explosion in the explosion chamber 110 is discharged through the transfer tube 160 into the explosion chamber 110 110 to the storage chamber 120.

When the nanocolloid is transferred from the explosion chamber 110 to the storage chamber 120, the nanoparticles generated by the electric explosion and suspended in the nanocolloid are collected into the storage chamber 120. At the same time, the concentration of nanocolloid in the explosion chamber 110 is reduced.

Thus, when the concentration of nanocolloids in the explosion chamber 110 is reduced, the nanoparticles produced by the present invention can be prevented from instantaneously coagulating and increasing in size again. This is because, if the fine nanoparticles are usually collected at a high concentration, the nanoparticles aggregate with the surrounding nanoparticles due to the electrostatic attraction between the nanoparticles, so that the nanoparticle concentration in the explosion chamber 110 of the present invention is reduced The coagulation between the nanoparticles produced by the electric explosion is suppressed.

The delivery tube 160 connecting the explosion chamber 110 and the storage chamber 120 includes a dispersion induction unit 113 for guiding the nanoparticles generated in the explosion chamber 110 to flow toward the storage chamber 120, Respectively. The dispersion induction unit 113 is a kind of induction electrode in which an anode and a cathode are stacked alternately with an insulator interposed therebetween. The induction unit 113 is connected to the outside of the transfer tube 160 to form an electric field, Colloids and nanoparticles.

Specifically, the electric field generated around the transfer tube 160 by the dispersion induction unit 113 is transferred from the explosion chamber 110 to the transfer tube (not shown) having the dispersion induction unit 113 160 so that the nanoparticles are dispersed in the explosion chamber 110. As a result, the concentration of nanoparticles in the explosion chamber 110 is further lowered, effectively suppressing the aggregation between the nanoparticles described above. At the same time, the nanoparticles collected in the transfer tube 160 are charged with the same polarity, and the probability of occurrence of coagulation between the nanoparticles is lowered. In addition, the polarity of the nanoparticles flowing into the electric field of the transfer tube 160 is neutralized by the influence of the electric field, and the aggregation of the nanoparticles collected in the subsequent storage container is prevented.

The dispersion inducing unit 113 continuously operates the nanocolloidal manufacturing apparatus 100 of the present invention to continuously induce the flow of nanocolloids and nanoparticles from the explosion chamber 110 toward the transfer tube 160. The nanoparticle concentration in the explosion chamber 110 is reduced while inducing a large amount of nanoparticles generated in the explosion chamber 110 in the direction of the transfer tube 160 instantaneously in the electric explosion, Is not agglomerated and maintains fine nanoparticle size.

At least one ultrasonic wave generation unit 115 is further installed in the explosion chamber 110 or the transfer tube 160. The ultrasonic wave generating unit 115 irradiates ultrasonic waves to the explosion chamber 110 or the transfer tube 160 to apply vibration to the nanoparticles to prevent adjacent nanoparticles from aggregating with each other and to increase the degree of dispersion of the nanoparticles . The ultrasonic wave generating unit 115 may be of a horn-type, a bath-type, or the like.

In the storage chamber 120, a circulation tube is separately formed in addition to the transfer tube 160. In the circulating tube, a dispersion medium 111 containing a small amount of nanoparticles remaining in the storage chamber 120 is recovered. This circulating tube is installed to flow the nanocolloidal solution in the entire nanocolloidal manufacturing apparatus 100 in the cooling chamber 130 and a first circulation tube 171 for guiding the nanocolloidal solution from the storage chamber 120 to the cooling chamber 130 A second circulation tube 172 for guiding the circulation pump 140 to the circulation pump 140 and a third circulation tube 172 for guiding the dispersion medium 111 flowing out from the circulation pump 140 to the cooling chamber 130 through another cooling unit 150, A circulation tube 173 and a fourth circulation tube 174 for guiding the dispersion medium 111 flowing out from the circulation pump 140 to the explosion chamber 110.

Here, the cooling chamber 130 stores and cools the dispersion medium 111 flowing through the first circulation tube 171. The cooling of the dispersion medium 111 in this way is intended to lower the temperature of the nanocolloid raised by electric explosion. If the temperature of the nano-colloid is maintained at a high temperature for a long time, the nano-colloid manufacturing apparatus 100 may be exposed to high temperature for a long time, It is very important to cool the nano-colloid again.

It is preferable that the cooling chamber 130 is formed such that the inner space of the cooling chamber 130 is at least one time larger than the volume of the stored dispersion medium 111 so that the dispersion medium 111 is effectively cooled in a natural state. The cooling water is circulated from the cooling chamber 130 through the circulation pump 140 to the cooling unit 150 through the second and third circulation tubes 173 and then flows into the cooling chamber 130 again. The dispersion medium 111 can be cooled more effectively.

At this time, it is preferable that the cooling unit 150 uses a common cooler module, and is configured to operate the cooling unit 150 according to need by a separately provided power source device.

The dispersion medium 111 in the cooling chamber 130 passes through the circulation pump 140 and part of the dispersion medium 111 is cooled through the cooling unit 150 and then flows into the cooling chamber 130, And the remaining dispersion medium 111 is guided to the explosion chamber 110 through the fourth circulation tube 174. [

The dispersion medium 111 flowing into the explosion chamber 110 through the fourth circulation tube 174 is a very low concentration of nanoparticles in the nanocolloid and flows into the explosion chamber 110, But also to reduce the concentration of nano-colloids.

Hereinafter, the method for producing a nanocolloid of the present invention will be described below.

The method of manufacturing nanocolloids of the present invention comprises the steps of feeding a metal wire 300 into an explosion chamber 110, generating nanoparticles by electric explosion and transferring nanoparticles by an electric field S20, Collecting the generated nanoparticles separately (S30), and cooling the dispersion medium 111 to the explosion chamber 110 (S40).

In this nano-colloid manufacturing method, first, the metal wire 300 is fed into the explosion chamber 110 and dipped in the dispersion medium 111 accommodated in the explosion chamber 110. At this time, the metal wire 300 is immersed in the dispersion medium 111 and is mounted between the two electrodes of the anode 117 and the cathode 119 provided in the explosion chamber 110. At this time, the metal wire 300 is repeatedly supplied at a predetermined length and time interval by the feeding device 200 separately provided outside the explosion chamber 110, so that the explosion of the electric wire can be repeatedly performed.

When the metal wire 300 is mounted between the two electrodes, an instantaneous high voltage is applied to the two electrodes to perform electrical explosion on the metal wire 300. At this time, the nanoparticles are instantaneously formed and simultaneously the nanoparticles are transferred to the outside of the explosion chamber 110 through the transfer tube 160 by the electric field (S20).

Here, a high voltage of 500 to 1500 V is applied between the two electrodes to perform electric explosion. If the applied voltage is less than 500 V, the voltage intensity is insufficient for obtaining the high concentration fine nanoparticles to be obtained in the present invention. If the applied voltage is higher than 1500 V, cracks may be generated in the nanocolloid manufacturing apparatus, The generated current may be discharged to the nanoparticles dispersed in the nanocolloid rather than to the metal wire, and this may act as a factor that hinders the generation of the nanoparticles.

For example, in the case of the embodiment shown in FIG. 3 and Table 1 described above, a voltage of 1223 V was applied to perform electrical explosion to obtain 321.90 mg / L of nanoparticles. The nanoparticles thus obtained are particles produced by converting at least 65% or more of the metal wires of the step (10), and the conversion efficiency is much improved as compared with the conventional technology in the production of nanoparticles by the submerged electric explosion device .

The nanoparticles thus obtained are simultaneously transferred to the outside of the explosion chamber 110 along the transfer tube 160 by the electric field. This instantaneous transfer is possible by the electric field formed in the transfer tube 160 at the same time as the electric explosion. At this time, the electric field may be formed by the dispersion inducing unit 113 installed at the portion connected to the transfer tube 160. When the nanoparticles are transferred to the outside from the explosion chamber 110, the concentration of nanocolloids in the explosion chamber 110 is relatively reduced, and thus the aggregation of the generated nanoparticles is prevented. In the subsequent explosion of the nanoparticles, The yield is further increased.

Next, the nanoparticles and nanocolloids transferred to the transfer tube 160 are guided to the storage tube through the transfer tube 160. In the storage tube, nanoparticles dispersed in the nanocolloid are collected and stored, and the remaining dispersion medium 111 is discharged through a separately installed circulation tube. (S30) At this time, the dispersion medium 111 is filled with a small amount of nanoparticles The concentration of the nanocolloid is remarkably reduced to 50 ppm or less compared to that before the storage chamber 120. However,

Finally, the dispersion medium 111 flowing out from the storage tube is cooled along the circulation tube and re-introduced into the explosion chamber 110. (S40) Here, in order to cool the dispersion medium 111, The temperature of the dispersion medium 111 may be lowered by cooling the substrate 111, or the temperature of the dispersion medium 111 may be rapidly lowered by driving the separately installed cooling unit 150 as necessary.

FIG. 5 is a TEM photograph for identifying nanoparticles in a nanocolloid produced by using a conventional nanocolloid manufacturing apparatus. FIG. 6 is a TEM photograph of a nanocolloid produced by the apparatus 100 for producing a nanocolloid of the present invention, This is a TEM photograph for identifying the nanoparticles in the colloid.

Referring to FIG. 5, conventional nanocolloid manufacturing apparatuses have difficulty in obtaining fine nanoparticles at a high concentration due to problems such as voltage, agglomeration of particles, and dispersing power. Particularly, when a high voltage is applied in an electric explosion, cracks are generated in the inside and outside of the nanocolloid manufacturing apparatus due to explosive force due to a high voltage, so that durability is very low. Therefore, electric explosion has to be performed by applying a voltage of about 300 to 400V.

In the conventional nanocolloid production apparatus, when a voltage of about 340 V was applied to perform electrical explosion, as shown in the TEM image of FIG. 5, the generated nanoparticles aggregated, Can be identified.

FIG. 6 is a photograph of an embodiment of the nanoparticles produced by the apparatus 100 for producing a nanocolloid of the present invention and the method of the present invention. In this embodiment, the ultrasonic irradiation and the electric field for improving the dispersion degree of the nanoparticles An electrical explosion by a voltage of 1223 V was carried out together. Here, in this photograph, not only the state in which the nanoparticles are uniformly dispersed can be confirmed, but also the nanoparticles grown as nanoparticles larger in size than the conventional ones can be confirmed to be remarkably reduced.

According to the apparatus and method for producing a nanocolloid according to the present invention, it is possible to produce high-quality nanocolloids containing high-concentration fine nanoparticles and to ensure uniform dispersion of the prepared nanocolloids for a long time can do. In addition, the quality of the secondary processed product made using the nanocolloid produced by the present invention can be improved.

The apparatus and method for manufacturing a nanocolloid as described above are not limited to the construction and the operation of the embodiments described above. The embodiments may be configured so that all or some of the embodiments may be selectively combined so that various modifications may be made.

100: Nano colloid manufacturing apparatus 110: Explosion chamber
111: dispersion medium 113: dispersion induction unit
115: Ultrasonic generating unit 117: Explosion chamber anode electrode
119: explosion chamber cathode electrode 120: storage chamber
130: cooling chamber 140: circulation pump
150: Cooling unit 160: Feed tube
171: first circulation tube 172: second circulation tube
173: third circulation tube 174: fourth circulation tube
200: feeding device 300: metal wire

Claims (10)

An explosion chamber which receives a metal wire from the outside as a dispersion medium therein, manufactures nanocolloids by electric explosion and guides the metal nanowires to a transfer tube;
A dispersion induction unit connected to the transfer tube and forming an electric field around the transfer tube to densify nanoparticles of nanocolloids in the transfer tube;
A storage chamber for collecting and storing nanocolloids containing nanoparticles densely packed in the transfer tube; And
And a cooling chamber for receiving the nano-colloid including the uncleaved nanoparticles through the circulation tube connected to the storage chamber and lowering the temperature of the nano-colloid,
Wherein the nanocolloid transferred to the cooling chamber has a lower concentration than the nanocolloid stored in the storage chamber.
The method according to claim 1,
Wherein the explosion chamber is made of a metal.
The method according to claim 1,
Wherein the explosion chamber is made of aluminum.
The method according to claim 1,
Wherein the dispersion induction unit is an induction electrode in which an anode and a cathode are stacked alternately with an insulator interposed therebetween.
The method according to claim 1,
Wherein the dispersion induction unit is installed to operate at all times in the nanocolloid manufacturing apparatus.
(S10) feeding a metal wire into the explosion chamber filled with the dispersion medium;
(S20) of generating nanocolloid by electric explosion in the explosion chamber and transferring colloid by electric field;
Collecting the nanoparticles dispersed in the colloid (S30); And
(S40) cooling the colloid including the nanoparticles not collected in the above to re-enter the explosion chamber (S40).
The method of claim 6,
Wherein the electric explosion in the step (S20) is performed by applying a voltage of 500 to 1500V.
The method of claim 6,
Wherein the nanoparticles of step (S20) are particles produced by converting at least 65% or more of the metal wires of step (S10).
The method of claim 6,
Wherein the electric field is constantly formed during the production of the nanocolloid in the step (S20).
The method of claim 6,
Wherein the ultrasonic wave is further irradiated to disperse the nanoparticles in the nanocolloid generated by the electric explosion in the step (S20).

Images