KR101002018B1 - Method for shape controlling of gold nano material - Google Patents

Abstract

A method for controlling the shape of gold nanomaterials is provided.

Method for controlling the shape of the gold nanomaterial according to the present invention comprises the steps of preparing an aqueous solution of gold salt, cetyltrimethylammonium bromide and sodium hydroxide; And irradiating the mixed aqueous solution for 5 to 100 minutes with a proton beam having an irradiation rate of 1.5 to 15 Gy / s, wherein the concentration of cetyltrimethylammonium bromide in the mixed aqueous solution is below a critical micelle concentration, By controlling the irradiation rate and irradiation time of the proton beam, the shape of the gold nanomaterials can be adjusted from nanoparticles to nanowires as needed, and it is environmentally friendly by minimizing the amount of surfactants and does not require the addition of silver ions. Process efficiency is high because no separate purification process is required.

Description

Method for shape controlling of gold nano material

The present invention relates to a shape control method of gold nanomaterials, and more particularly, to a shape control method of gold nanomaterials capable of adjusting the shape of gold nanomaterials by controlling reaction conditions.

Nanoparticles of metals or semiconductors have been extensively studied due to their improved electrical, magnetic, optical, and catalytic properties compared to bulk states. Among various metal nanoparticles, considerable research is being conducted on gold nanoparticles recently. Recently, researches and practical applications of gold nanoparticles in various applications such as catalysts, biotransmitters, electronic materials, and optical materials have been conducted. It is done.

Conventional methods for producing gold nanoparticles include the following method.

One of the traditional methods, Turkevitch-Frens synthesis method is a method for producing gold nanoparticles by reducing the gold chloride (HAuCl ₄ ) in water using citric acid. Following this traditional method, a two-step process is used to stabilize gold nanoparticles using alkanethiolates and various functional thilate ligands and the Brust-Schiffrin method. Synthetic methods have been introduced. In addition, there is a method of producing gold nanoparticles by reducing gold complex ions present in a gold salt solution including sodium borohydride (NaBH ₄ ) in the presence of a dendrimer.

In addition, as a physical method, a method of producing gold nanoparticles using ultraviolet (UV), near infrared (Near-IR), ultrasonic waves, microwaves, proton beams, or the like is known.

Meanwhile, various methods for preparing gold nanorods or gold nanowires in addition to gold nanoparticles have been studied. Gold nanomaterials such as gold nanoparticles, gold nanorods, and gold nanowires have not only the size but shape of the nanomaterials. It is known that the physical and chemical properties change greatly. That is, it was necessary to adjust the particle diameter of the gold nanoparticles or the length of the gold nanorods (or gold nanowires) according to the use.

Korean Patent No. 795480 discloses a technique for controlling the size of gold nanoparticles according to temperature, but the shape of the gold nanoparticles cannot be controlled and the concentration of the surfactant used is 1 to 10% by weight in the total aqueous solution. Due to the excessive process, the process of finally removing the surfactant was essential and not environmentally friendly.

In addition, although the method of controlling the shape of the gold nanomaterial using the electron beam is known in the academic world, since the concentration of the surfactant must be added to exceed the critical micellar concentration (CMC), as mentioned above, There was a problem that could adversely affect the environment.

In addition, according to the previous researches of the present invention, it is also possible to control the shape of the gold nanomaterial by using a proton beam. In this case, silver ions must be added in order to manufacture one-dimensionally formed gold nanorods or gold nanowires. As a result, manufacturing cost increases, process efficiency decreases, and the process efficiency decreases because the process must be performed to remove the silver ions.

Therefore, the problem to be solved by the present invention is to control the shape of the gold nanomaterials from nanoparticles to nanowires as necessary by controlling the reaction conditions, environmentally friendly by minimizing the amount of the surfactant, adding silver ions There is no need to provide a method for controlling the shape of gold nanomaterials having excellent purity.

In order to achieve the above object,

Preparing an aqueous solution in which gold salt, cetyltrimethylammonium bromide and sodium hydroxide are mixed; And

Irradiating the mixed aqueous solution for 5 to 100 minutes with a proton beam having an irradiation rate of 1.5 to 15 Gy / s, wherein the concentration of cetyltrimethylammonium bromide in the mixed aqueous solution is below a critical micelle concentration. It provides a method for controlling the shape of a material.

According to one embodiment of the invention, the geumyeom is Keumsan potassium chloride (KAuCl _4), sodium (NaAuCl ₄₎ chloroauric acid, chloroauric acid (HAuCl _4), brominated Keumsan sodium (NaAuBr _4), yeomhwageum (AuCl), chloride J. It may be any one selected from the group consisting of gold (AuCl ₃ ) and gold bromide (AuBr ₃ ).

According to another embodiment of the present invention, the gold salt is geum chloride, and the molar ratio of the geum chloride, cetyltrimethylammonium bromide and sodium hydroxide in the mixed aqueous solution may be 1: 3: 15 to 1: 5: 25.

The concentration of cetyltrimethylammonium bromide in the mixed aqueous solution is preferably 0.9 to 1 mM.

According to another embodiment of the present invention, the shape control method of the gold nanomaterial according to the present invention is fixed to 2.77 Gy / s irradiation rate of the proton beam and the irradiation time of 25 to 40 minutes of the particle diameter of 3 ~ 45nm It may be to prepare gold nanoparticles.

In addition, in the shape control method of the gold nanomaterial according to the present invention, the irradiation rate of the proton beam is fixed at 2.77 Gy / s and the irradiation time is 50-85 minutes, and the gold nanoparticles having a particle diameter of 10-25 nm and a diameter of 10-20 nm It may be to prepare the gold nanorods and gold nanowires.

In addition, the shape control method of the gold nanomaterial according to the present invention is to produce gold nanoparticles having a particle diameter of 15 to 25nm by fixing the irradiation rate of the proton beam to less than 2.77 Gy / s and irradiation time 50 to 100 minutes. Can be.

According to the present invention, by controlling the irradiation rate and irradiation time of the proton beam, the shape of the gold nanomaterials can be adjusted from nanoparticles to nanowires as needed. There is no need for a separate purification process, so the process efficiency is high. In particular, when controlling the shape of the gold nanomaterial by fixing the irradiation rate of the proton beam and increasing or decreasing the irradiation time, there is an advantage that the process efficiency is excellent when applied to the actual process.

Hereinafter, the present invention will be described in more detail.

It is known that the physical and chemical properties of gold nanomaterials differ from those of bulk gold or gold elements, and these differences depend not only on the size but also on the shape of the gold nanomaterial. Therefore, techniques for controlling the shape of gold nanomaterials are very important when considering their applicability in electronic or optical fields.

In the present invention, by adjusting the reaction conditions by changing the irradiation rate or the irradiation time of the proton beam, gold nanoparticles as well as nanowires to provide a method that can adjust the shape of the gold nanomaterials as needed. . In particular, when fixing the average dose rate of the proton beam to a predetermined value or more and changing the irradiation time, the shape of the gold nanomaterial may be selectively changed to gold nanoparticles, gold nanorods, and gold nanowires. It is possible to control the shape of the gold nanomaterial by simply changing the irradiation time without changing the irradiation rate, and has the advantage of improving the process efficiency when applied to the actual process.

In the present invention, spherical gold nanoparticles, gold nanorods with controlled aspect ratios, as well as gold nanowires can be prepared by irradiating a proton beam having an irradiation rate of a predetermined value or more in the presence of cetyltrimethylammonium bromide below a critical micelle concentration. Provides a method of controlling the shape of the gold nanomaterial possible, the method of controlling the shape of the gold nanomaterial comprises the steps of preparing an aqueous solution of gold salt, cetyltrimethylammonium bromide and sodium hydroxide; And irradiating the mixed aqueous solution for 5 to 100 minutes with a proton beam having an irradiation rate of 1.5 to 15 Gy / s, wherein the concentration of cetyltrimethylammonium bromide in the mixed aqueous solution is below a critical micelle concentration.

The gold salt used above is not particularly limited as long as it is commonly used in the art, and for example, potassium chloride (KAuCl ₄ ), sodium chloride (NaAuCl ₄ ), gold chloride (HAuCl ₄ ), sodium bromide (NaAuBr ₄ ), gold chloride (AuCl), ferric chloride (AuCl ₃ ), and gold bromide (AuBr ₃ ).

The cetyltrimethylammonium bromide acts as a surfactant and is known to have a critical micelle concentration of at least 0.001 M at temperatures below 301K. This is because micelles are formed only when the critical micelle concentration is exceeded, which may cause nanoparticles to form and stabilize the nanoparticles. Therefore, in a conventional method using an electron beam or a method using a proton beam, the surfactant is added at about 10 times or more of the critical micelle concentration. Accordingly, the surfactant acts as an impurity on the produced nanomaterial, as well as the environment. Even had the disadvantage of adversely affecting. However, according to the present invention, even when using a surfactant below the critical micelle concentration, gold nanomaterials can be generated and thus, there is an advantage of being environmentally friendly. Generally, the reason for synthesizing nanomaterials above the critical micelle concentration is to control their size and shape. The present invention can control the size and shape of nanomaterials by appropriately controlling the irradiation rate and irradiation time of the proton beam. Therefore, gold nanomaterials can be formed using surfactants below the critical micelle concentration. On the other hand, the surfactant below the critical micelle concentration used in the present invention is considered to play a role in stabilizing the resulting gold nano-compound.

In addition, the present invention is characterized in that one-dimensional growth of gold nanomaterials is possible without the addition of separate silver ions, and at a specific irradiation rate and irradiation time used in the present invention, aggregation of the nanoparticles already generated is activated. Aggregation is likely to be toward the more reactive end surface than the side of the nanorods, and consequently, it is likely that they have grown into nanowires.

On the other hand, the present invention includes the step of irradiating the mixed aqueous solution for 5 to 100 minutes with a proton beam having an irradiation rate of 1.5 to 15 Gy / s, when the irradiation rate exceeds 15 Gy / s the energy to be irradiated It is not preferable because only excessively large and irregularly shaped gold nanoparticles are obtained and the shape of the gold nanomaterial cannot be controlled. In addition, as described below, one-dimensional growth of gold nanomaterials is possible only at a predetermined irradiation rate or more, thereby forming nanorods or nanowires.

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As already mentioned, the gold salt used in the present invention is not particularly limited as long as it is commonly used in the art, and when using gold chloride as the gold salt, the gold chloride, cetyltrimethylammonium bromide in the mixed aqueous solution And the molar ratio of sodium hydroxide may be 1: 3: 15 to 1: 5: 25. The molar ratio is an optimal range for controlling the shape of the gold nanomaterial by irradiation of a proton beam. In addition, it is preferable that the concentration of cetyltrimethylammonium bromide in the mixed aqueous solution is 0.9 to 1 mM. However, when the concentration of cetyltrimethylammonium bromide is less than 0.9 mM, it is difficult to form gold nanoparticles and when the concentration exceeds 1 mM, the critical micelle concentration is exceeded.

The shape control method of the gold nanomaterial according to the present invention may be to prepare gold nanoparticles having a particle diameter of 3 to 45nm by fixing the irradiation rate of the proton beam to 2.77 Gy / s and the irradiation time of 25 to 40 minutes, Under the same irradiation rate of the proton beam as above, the irradiation time may be 50 to 85 minutes to prepare gold nanoparticles having a particle diameter of 10 to 25 nm, gold nanorods having a diameter of 10 to 20 nm, and gold nanowires. In other words, the shape of the gold nanomaterial can be controlled by fixing the irradiation rate of the proton beam to a predetermined value (a value capable of one-dimensional growth of nanomaterials) and changing the irradiation time. Rods and gold nanowires can be manufactured as needed, and there is an advantage in that the process efficiency is excellent simply by adjusting the irradiation time.

In addition, according to the present invention, gold nanoparticles having a particle size of 15 to 25 nm may be prepared by fixing the irradiation rate of the proton beam to less than 2.77 Gy / s and having an irradiation time of 50 to 100 minutes. In the present invention, 2.77 Gy / The irradiation rate of the proton beam, s, corresponds to the threshold for one-dimensional growth of nanomaterials. Therefore, pure gold nanoparticles can be produced only when the value is less than the above value, and the distribution of the particle diameters is uniform compared with the case where the irradiation rate of the proton beam is fixed at 2.77 Gy / s and the irradiation time is 25 minutes.

When the proton beam is irradiated in the present invention, gold nanoparticles are first generated, and they act as nuclei to grow, and it is determined that one-dimensional growth is promoted as the irradiation time of the proton beam increases. If the amount of irradiation of the proton beam is too large, the gold nanorods and the gold nanowires that have already been formed are segmented to form small gold nanoparticles, which aggregate together to form irregular gold nanoparticles.

In the above, the irradiation rate of the proton beam is fixed at 2.77 Gy / s, and when the irradiation time of the proton beam is less than 25 minutes, the formation of gold nanoparticles may not be performed properly. When it exceeds 85 minutes, it is not preferable because the nanorods or nanowires are segmented and aggregated to produce nanoparticles of irregular shape.

Pure HAuCl ₄ solution is pale yellow, but the solution containing HAuCl ₄ and CTAB is dark yellow in color. When NaOH is added to the solution, the color of the solution becomes almost transparent. As the proton beam is irradiated, its color changes from pink to purple or brown.

Hereinafter, the present invention will be described in more detail with reference to preferred examples, but the present invention is not limited thereto.

Example 1

5 ml of 0.5 mM HAuCl ₄ aqueous solution, 5 ml of 2 mM cetyltrimethylammonium bromide (CTAB) and 100 μl of 0.5 M NaOH were mixed into the vial and stirred slowly for 10 seconds. Next, 0.5 ml of the mixed solution was transferred to a PCR tube and irradiated with a proton beam. Irradiation of a proton beam has been carried out by installing a 45MeV proton beam line to the MC-50 cyclotron at the Institute of Korea Atomic the beam line is designed to have a proton density of ^{1x10 7 ~1x10 10 protons / cm 2} . On the other hand, the energy of the proton beam was fixed at 20 MeV, and the irradiation amount of the proton beam was 2.77 Gy / s and the irradiation time was 25 minutes.

Example 2

5 ml of 0.5 mM HAuCl ₄ aqueous solution, 5 ml of 2 mM cetyltrimethylammonium bromide (CTAB) and 100 μl of 0.5 M NaOH were mixed into the vial and stirred slowly for 10 seconds. Next, 0.5 ml of the mixed solution was transferred to a PCR tube and irradiated with a proton beam. Proton beam irradiation was carried out by installing a 45MeV proton beam line in MC-50 cyclotron at the Korea Atomic Energy Research Institute. The beam line was designed to have a proton density of 1x10 ⁷ ~ 1x10 ¹⁰ protons / cm ² . On the other hand, the energy of the proton beam was fixed at 20 MeV, and the dose of the proton beam was 2.77 Gy / s and the irradiation time was 50 minutes.

Example 3

5 ml of 0.5 mM HAuCl ₄ aqueous solution, 5 ml of 2 mM cetyltrimethylammonium bromide (CTAB) and 100 μl of 0.5 M NaOH were mixed into the vial and stirred slowly for 10 seconds. Next, 0.5 ml of the mixed solution was transferred to a PCR tube and irradiated with a proton beam. Proton beam irradiation was carried out by installing a 45MeV proton beam line in MC-50 cyclotron at the Korea Atomic Energy Research Institute. The beam line was designed to have a proton density of 1x10 ⁷ ~ 1x10 ¹⁰ protons / cm ² . On the other hand, the energy of the proton beam was fixed at 20 MeV, and the irradiation amount of the proton beam was 2.77 Gy / s and the irradiation time was 75 minutes.

Example 4

5 ml of 0.5 mM HAuCl ₄ aqueous solution, 5 ml of 2 mM cetyltrimethylammonium bromide (CTAB) and 100 μl of 0.5 M NaOH were mixed into the vial and stirred slowly for 10 seconds. Next, 0.5 ml of the mixed solution was transferred to a PCR tube and irradiated with a proton beam. Irradiation of a proton beam has been carried out by installing a 45MeV proton beam line to the MC-50 cyclotron at the Institute of Korea Atomic the beam line is designed to have a proton density of ^{1x10 7 ~1x10 10 protons / cm 2} . On the other hand, the energy of the proton beam was fixed at 20 MeV, and the irradiation amount of the proton beam was 2.77 Gy / s and the irradiation time was 100 minutes.

Example 5

5 ml of 0.5 mM HAuCl ₄ aqueous solution, 5 ml of 2 mM cetyltrimethylammonium bromide (CTAB) and 100 μl of 0.5 M NaOH were mixed into the vial and stirred slowly for 10 seconds. Next, 0.5 ml of the mixed solution was transferred to a PCR tube and irradiated with a proton beam. Irradiation of a proton beam has been carried out by installing a 45MeV proton beam line to the MC-50 cyclotron at the Institute of Korea Atomic the beam line is designed to have a proton density of ^{1x10 7 ~1x10 10 protons / cm 2} . On the other hand, the energy of the proton beam was fixed at 20 MeV, and the irradiation amount of the proton beam was 5.54 Gy / s and the irradiation time was 12.5 minutes.

Example 6

5 ml of 0.5 mM HAuCl ₄ aqueous solution, 5 ml of 2 mM cetyltrimethylammonium bromide (CTAB) and 100 μl of 0.5 M NaOH were mixed into the vial and stirred slowly for 10 seconds. Next, 0.5 ml of the mixed solution was transferred to a PCR tube and irradiated with a proton beam. Irradiation of a proton beam has been carried out by installing a 45MeV proton beam line to the MC-50 cyclotron at the Institute of Korea Atomic the beam line is designed to have a proton density of ^{1x10 7 ~1x10 10 protons / cm 2} . On the other hand, the energy of the proton beam was fixed at 20 MeV, and the irradiation amount of the proton beam was 8.31 Gy / s and the irradiation time was 8.33 minutes.

Example 7

5 ml of 0.5 mM HAuCl ₄ aqueous solution, 5 ml of 2 mM cetyltrimethylammonium bromide (CTAB) and 100 μl of 0.5 M NaOH were mixed into the vial and stirred slowly for 10 seconds. Next, 0.5 ml of the mixed solution was transferred to a PCR tube and irradiated with a proton beam. Irradiation of a proton beam has been carried out by installing a 45MeV proton beam line to the MC-50 cyclotron at the Institute of Korea Atomic the beam line is designed to have a proton density of ^{1x10 7 ~1x10 10 protons / cm 2} . On the other hand, the energy of the proton beam was fixed at 20 MeV, and the dose of the proton beam was 13.85 Gy / s and the irradiation time was 5 minutes.

Comparative Example 1

5 ml of 0.5 mM HAuCl ₄ aqueous solution, 5 ml of 2 mM cetyltrimethylammonium bromide (CTAB) and 100 μl of 0.5 M NaOH were mixed into the vial and stirred slowly for 10 seconds. Next, 0.5 ml of the mixed solution was transferred to a PCR tube and irradiated with a proton beam. Proton beam irradiation was carried out by installing a 45MeV proton beam line in MC-50 cyclotron at the Korea Atomic Energy Research Institute. The beam line was designed to have a proton density of 1x10 ⁷ ~ 1x10 ¹⁰ protons / cm ² . On the other hand, the energy of the proton beam was fixed at 20 MeV, and the irradiation amount of the proton beam was 1.385 Gy / s and the irradiation time was 50 minutes.

Test Example 1

UV - vis  Measurement of Absorption Spectrum

For the gold nanomaterial dispersion solution prepared in Examples 1 to 7 and Comparative Example 1, the absorption spectrum was measured using a UV-2550 spectrophotometer, and the results are shown in FIGS. 1 and 2.

1 shows UV-vis absorption spectra for Examples 1 to 4, and FIG. 2 shows UV-vis absorption spectra for Examples 5 to 7 and Comparative Example 1. FIG.

Referring to FIG. 1, in Example 1, an absorption band appears near 543 nm, which corresponds to the surface plasmon absorption band of gold nanocrystals. On the other hand, in the case of Example 2, as the irradiation time is doubled as 50 minutes, the maximum absorption band is shifted to short wavelength of 527nm, it can be seen that the broad shoulder (shoulder) is generated. This short wavelength shift means that the size of the gold nanoparticles produced is smaller. In addition, the shoulder is spread over the visible light region and the infrared region, which indicates that the gold nanorods and the gold nanowires are formed by the surface plasmons of the nanorods and the nanowires. In the case of Example 3, the maximum absorption band is shifted further toward shorter wavelengths at 524 nm and is widely distributed over the infrared region at about 640 nm, so that the broad shoulder is slightly smaller than Example 2, but the difference is very small. Therefore, in this case, it can be confirmed that gold nanorods and gold nanowires are formed. Finally, in the case of Example 4, the maximum absorption band again shifts to a wavelength of 541 nm, which means that the generated gold nanorods or nanowires are fragmented and then aggregated together to generate large nanoparticles. On the other hand, it can be seen that the broad shoulders widely distributed in the visible and infrared regions did not change, which means that the size of the nanoparticles or nanorods produced is irregular.

Meanwhile, referring to FIG. 2, in Comparative Example 1, the surface plasmon absorption band of the gold nanocrystals appears at 527 nm, but no broad shoulder is widely distributed in the visible and infrared regions. On the other hand, in Example 5, the maximum absorption band appears at 526 nm and a broad shoulder in the region of about 630 nm. In the case of Example 6, the maximum absorption band appears at 527 nm and there is a broad shoulder, and in Example 7, the maximum absorption band appears at 529 nm and the broad shoulder is slightly increased. In Comparative Example 1 and Examples 5 to 7, the irradiation rate and irradiation time were different, but the total irradiation amount was the same as 4155 Gy.

Test Example 2

TEM  Photo measurement

The TEM photographs were measured using JEM-2100F with respect to the gold nanomaterial dispersion solutions prepared in Examples 1 to 7 and Comparative Example 1, and the results are shown in FIGS. 3 and 4. FIG. 3 is a TEM photograph of Examples 1 to 4, and FIG. 4 is a TEM photograph of Examples 5 to 7 and Comparative Example 1. FIG.

Referring to FIG. 3, (a) shows a TEM photograph of Example 1, showing that spherical gold nanoparticles having an average particle diameter of 3 to 45 nm were generated. Next, referring to the photograph (b) for Example 2, it can be seen that gold nanorods and nanowires having a tadpole shape are formed by one-dimensional growth with gold nanoparticles having an average particle diameter of about 20 nm. The diameter of the nanowires is about 13 nm and the gold nanorods and gold nanowires affect the formation of broad shoulders in the region of about 640 nm in the UV-vis spectrum of FIG. 1. Next, in the case of (c), the TEM photograph of Example 3 shows a similar tendency to that of (b), but it can be seen that the aspect ratio of the nanowires is slightly reduced. Finally, referring to (d), gold nanoparticles having an average particle diameter of 2 to 50 nm occupy most of them, a small number of gold nanorods are observed, and gold nanowires are hardly observed. As mentioned above, if the fixation rate of the proton beam is fixed to more than the dose that allows one-dimensional growth and the irradiation time is increased, the gold nanoparticles are generated after the gold nanoparticles are generated, and then the gold nanorods and the gold nanowires are used as the mother nucleus. When is formed and the irradiation time is longer, the gold nanorods and gold nanowires are segmented and aggregated to form irregular gold nanoparticles. In the present invention, the minimum value of the irradiation rate for allowing gold nanoparticles to grow in one dimension is 2.77 Gy / s.

On the other hand, referring to Figure 4, (a) is a TEM photograph of Comparative Example 1, only the gold nanoparticles having an average particle diameter of 22nm when the irradiation rate of the proton beam is 1.358Gy / s and the irradiation time is 50 minutes It can be confirmed that this was formed. The irradiation rate and the irradiation time is 4155Gy in terms of the irradiation dose, and the remaining irradiation rate and irradiation time of the proton beams in the other Examples 5-7, but the total irradiation dose is the same as 4155Gy. Meanwhile, referring to (c) to (d) of FIG. 4, gold nanoparticles, as well as gold nanorods having a diameter of about 11 nm and an aspect ratio of about 2, and gold nanowires having a diameter of about 11 nm and an aspect ratio of about 17 are formed. It can be confirmed.

Therefore, according to the present invention, in order to manufacture only gold nanoparticles, the irradiation time of the proton beam may be adjusted to less than 2.77 G / s, or the irradiation time may be shortened even if it is 2.77 G / s or more. In order to manufacture, the irradiation rate of the proton beam is set to 2.77 G / s or more and the irradiation time is adjusted so that gold nanoparticles, gold nanorods, as well as gold nanowires can be easily manufactured as necessary. The use of a surfactant is sufficient, and since there is no need to add a separate silver ion, there is an advantage that an environmentally friendly and high purity gold nanomaterial can be obtained.

1 is a UV-vis absorption spectrum for Examples 1-4.

2 shows UV-vis absorption spectra for Examples 5 to 7 and Comparative Example 1. FIG.

3 is a TEM photograph of Examples 1 to 4.

4 is a TEM photograph of Examples 5 to 7 and Comparative Example 1. FIG.

Claims (7)

Preparing an aqueous solution of gold salt, cetyltrimethylammonium bromide and sodium hydroxide; And Irradiating the mixed aqueous solution for 5 to 100 minutes with a proton beam having an irradiation rate of 1.5 to 15 Gy / s, wherein the concentration of cetyltrimethylammonium bromide in the mixed aqueous solution is below a critical micelle concentration. Shape control method of material. The method of claim 1, The gold salt is potassium chloride (KAuCl ₄ ), sodium chlorate (NaAuCl ₄ ), gold chlorate (HAuCl ₄ ), sodium bromide (NaAuBr ₄ ), gold chloride (AuCl), gold chloride (AuCl ₃ ) and gold bromide ( AuBr ₃ ) shape control method of the gold nanomaterial, characterized in that any one selected from the group consisting of. The method of claim 1, The gold salt is geum chloride, the molar ratio of the geum chloride, cetyltrimethylammonium bromide and sodium hydroxide in the mixed aqueous solution is 1: 3: 15 to 1: 5: 25 shape control method. The method of claim 1, The concentration of cetyltrimethylammonium bromide in the mixed aqueous solution is 0.9 ~ 1mM shape control method of the gold nanomaterial. The method of claim 1, The method of controlling the shape of a gold nanomaterial, characterized in that the proton beam is fixed at 2.77 Gy / s and the irradiation time is 25-40 minutes to produce gold nanoparticles having an average particle diameter of 3 to 45 nm. The method of claim 1, The proton beam was irradiated at 2.77 Gy / s and the irradiation time was 50 to 85 minutes to produce gold nanoparticles having an average particle diameter of 10 to 25 nm, gold nanorods having a diameter of 10 to 20 nm, and gold nanowires. Shape control method of the gold nanomaterial. The method of claim 1, The shape control method of the gold nanomaterial, characterized in that to produce a gold nanoparticles having an average particle diameter of 15 to 25nm by fixing the irradiation rate of the proton beam to less than 2.77 Gy / s and irradiation time 50 to 100 minutes.

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