KR101842751B1 - method for preparing zinc oxide nanoparticle, and zinc oxide nanoparticle prepared by the same - Google Patents
method for preparing zinc oxide nanoparticle, and zinc oxide nanoparticle prepared by the same Download PDFInfo
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- KR101842751B1 KR101842751B1 KR1020150173282A KR20150173282A KR101842751B1 KR 101842751 B1 KR101842751 B1 KR 101842751B1 KR 1020150173282 A KR1020150173282 A KR 1020150173282A KR 20150173282 A KR20150173282 A KR 20150173282A KR 101842751 B1 KR101842751 B1 KR 101842751B1
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- C—CHEMISTRY; METALLURGY
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- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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Abstract
The present invention relates to a process for preparing zinc oxide nanoparticles, which comprises reacting a zinc precursor with an alkylamine in an aqueous solution, and a zinc oxide nanoparticle produced thereby. According to the present invention, zinc oxide nanoparticles having excellent optical properties, catalytic activity, and magnetic properties can be produced simply and safely with high production efficiency.
Description
The present invention relates to a process for preparing zinc oxide nanoparticles and zinc oxide nanoparticles prepared therefrom, and more particularly to a process for producing zinc oxide nanoparticles, which comprises reacting a zinc precursor with an alkylamine in an aqueous solution, Zinc oxide nanoparticles.
Zinc oxide (ZnO), a piezoelectric and semiconductor material, attracts many researchers in nanoscience and engineering because of its unique physical properties and potential applications. In particular, ZnO nanoparticles have a wide range of biological applications such as extensive biological sensing, labeling, gene delivery, drug delivery, and nanomedicine, which is more biocompatible than other semiconductor materials including CdSe, InP, and TiO 2 .
In addition, ZnO nanoparticles also have a relatively large direct band gap of ~3.3 eV with a high exciton binding energy of 60 meV at room temperature, so that research on ZnO nanoparticles has been conducted on semiconductors, displays, information Telecommunication industry, and optical devices.
In order to enable practical use of ZnO nanoparticles in these applications, it is essential to develop economical methods for large-scale production. Three important properties - inexpensive reagents, simple synthetic routes, and significant yields - are required to maximize the economic efficiency of nanoparticle synthesis.
Various methods for synthesizing ZnO nanoparticles including a thermal method, a sol-gel method, a physical chemical vapor deposition method, a chemical solution deposition method, and an electrochemical deposition method have been reported. However, these methods require high reaction temperatures and pressures, additional heat treatment and reaction conditions of toxic organic solvents. Particularly, the production method of zinc oxide nanoparticles using an organic solvent causes environmental problems, is not suitable for mass production, and the yield is as low as 80%.
Recently, several research groups reported that ZnO nanoparticles were synthesized at low temperature in the aqueous phase, but the concentration of the synthesized nanoparticles was low and morphological control was difficult.
In addition, although a method of preparing ZnO nanoparticles using an aqueous solution of Zn (OH) 2 has been disclosed, a high reaction temperature of 500 ° C is required and it is not suitable for mass production since it requires two steps.
In addition, when polyethyleneimine is used as a reducing agent and a stabilizer in the conventional solution, the polyethyleneimine has a disadvantage that its molecular weight is too large to be applied.
Therefore, for industrial applications, simple synthesis methods that produce high yields of ZnO nanoparticles under mild ambient reaction conditions are essential.
Accordingly, the inventor of the present invention has made extensive efforts to solve the problems of the prior art. As a result, the inventors of the present invention have found that when an alkylamine is used, it is not necessary to use a stabilizer or the like because an alkylamine acts as an oxidizer and a stabilizer. It is possible to remarkably simplify the manufacturing process and to improve the working environment because it is possible to manufacture metal nanoparticles having excellent properties even when using a solvent which is easy to handle as well as a high temperature treatment of 100 DEG C or more, .
It is an object of the present invention to provide a method for manufacturing zinc oxide nanoparticles having a simple, safe and high production efficiency.
It is another object of the present invention to provide zinc oxide nanoparticles having excellent optical properties, catalytic activity and magnetic properties.
The first aspect of the present invention provides a method for producing zinc oxide nanoparticles, which comprises reacting a zinc precursor with an alkylamine in an aqueous solution.
The second aspect of the present invention also provides zinc oxide nanoparticles in which the two hexagonal nanorods have a hierarchical structure.
The method for producing the zinc oxide nanoparticles of the present invention can be carried out in an aqueous solution. That is, water can be used as the main solvent. In the conventional manufacturing method, a solvent which is harmful to a human body such as an organic solvent or accompanies an environmental pollution problem is used in most cases, but the present invention can drastically improve such a problem. In addition, there is also the advantage that there is no need for separate wastewater treatment facilities and atmospheric purification facilities. This is not only a great advantage in industry, but also very beneficial to the environment.
In a preferred embodiment, the zinc precursor is zinc chloride (ZnCl 2 ), zinc sulfate (ZnSO 4 ), zinc acetate (Zn (CH 3 CO 2 ) 2 ), zinc citrate (Zn 3 [O 2 CCH 2 C OH) (CO 2) CH 2 CO 2] 2), zinc nitrate (Zn (NO 3) 2) , zinc nitrate hexahydrate (Zn (NO 3) 2 · 6H 2 O) and zinc ahseteyiteuyi hydrate (Zn (OOCCH 3 ) 2 < 2 > 2H 2 O), but the present invention is not limited thereto.
The alkylamine may have 6 to 20 carbon atoms, and hexylamine, heptylamine, octylamine, oleylamine and the like may be used, but the present invention is not limited thereto.
The present invention is characterized in that zinc oxide nanoparticles are produced in an aqueous solution using an alkylamine as an oxidizing agent and a stabilizer.
In the present invention, alkylamine acts as an oxidizing agent to control the reaction rate so that zinc oxide (ZnO) can be formed by adjusting pH.
pH can affect nanoparticle production. According to the present invention, it is preferable to conduct the reaction under a basic condition of pH 9 or more in terms of uniform size and dispersion degree (stability in colloidal solution stability). A more preferred pH is 10 to 10.5, in which case nanoparticles having a size of about 250 nm can be prepared.
Also, in the present invention, the alkylamine serves as a stabilizer for keeping the formed zinc oxide to maintain the nano size.
In the synthesis of zinc oxide nanoparticles, morphological control is particularly important because of their physical and chemical properties such as optical properties, catalytic activity and magnetic properties being highly dependent on the morphology. To date, the synthesis of ZnO nanoparticles having various shapes including spherical, rod, linear, plate, belt, cone, spring, ring and cage has been reported.
The zinc oxide nanoparticles prepared according to the present invention are characterized by having a hierarchical structure of two well-defined hexagonal nanorods of different sizes.
Although there have been some reports on the synthesis of hierarchical zinc oxide nanostructures using electrochemical and hydrothermal methods, this is the first to synthesize hierarchical zinc oxide nanostructures in aqueous phase.
The present inventors produced single crystal ZnO nanoparticles by reacting Zn (NO 3 ) 2 with octylamine in aqueous phase. As a result of transmission electron microscopy (TEM) and electron diffraction pattern (ED), it was confirmed that the ZnO nanoparticles were single crystalline.
In addition, the inventors of the present invention have confirmed that aggregation of about 600 nm in size is a single crystal hexagonal nanoporous zinc oxide nanoparticle having a size of about 250 nm in the growth state of zinc oxide nanoparticles.
The method for producing the zinc oxide nanoparticles of the present invention can be carried out according to the following reaction formula 1 in one embodiment.
To act as a weak base to increase the pH of the reaction scheme 1, an alkylamine is reacted in the following reaction solution, Zn of (NO 3) 2 and hydroxide ions react with the Zn (OH) 2 are generated, Zn (OH) 2 As a result of the sol-gel reaction, zinc oxide (ZnO) is produced.
[Reaction Scheme 1]
Zn (NO 3 ) 2 + 2OH - → Zn (OH) 2 + 2NO 3 -
Zn (OH) 2 → ZnO + H 2 O
The reaction proceeds in one step, yielding a yield of at least 90%. The conventional method of preparing zinc oxide nanoparticles in an aqueous solution has a two-step process in which an aggregate is prepared in an aqueous solution and then subjected to a heat treatment at a high temperature, and the yield is as low as 80% or less.
The pH of the reaction solution is decreased by the above reaction, and we confirmed this fact by monitoring the pH value of the reaction during the synthesis (FIG. 2A).
When NaOH instead of alkylamine was used to increase the pH in the reaction solution, XRD analysis showed that a ZnO crystal structure was formed from a part of Zn (OH) 2 (see FIG. 2B). That is, alkylamine can also act to increase the pH of the reaction solution like NaOH.
The method for producing zinc oxide nanoparticles of the present invention is characterized in that zinc oxide nanoparticles are self-assembled into hexagonal nanorods based on an oriented attachment mechanism.
Depending on the reaction temperature and the concentration of Zn (NO 3 ) 2 in the method of preparing zinc oxide nanoparticles, the size, shape, and degree of agglomeration of the zinc oxide nanoparticles may vary.
That is, the self-assembly of nanoparticles can increase at high reaction temperatures.
When the reaction temperature is low, the size of the generated nanoparticles is not uniform and the production efficiency may be decreased. As the temperature increases, the size becomes uniform and the reaction speed becomes faster. In consideration of this point, the reaction temperature is preferably 50 to 70 ° C, but not necessarily limited to 100 ° C or less.
The size of the zinc oxide nanoparticles can also be controlled by varying the amount of the zinc precursor while maintaining other conditions.
The concentration of the zinc precursor is preferably 0.15 to 0.3 M.
When the concentration exceeds 0.3 M, micro-sized nanoparticles are prepared, and when the concentration is less than 0.15 M, the non-uniformity of the nanoparticle size may increase.
In the production process of the present invention, the weight ratio of alkylamine to zinc precursor in aqueous solution is preferably 1: 1.5 to 1: 3. If the ratio is more than 1: 3, the amount of the alkylamine may be excessive, and the morphology of the nanoparticles may be irregular. If the ratio is less than 1: 1.5, the stabilization effect by the alkylamine is insufficient.
The zinc oxide nanoparticles of the present invention are characterized in that two hexagonal nanorods of different sizes have a hierarchical structure.
The present inventors have designated the zinc oxide nanoparticles as "zinc oxide nanobots".
The zinc oxide nanoparticles of the present invention have a hierarchical structure of hexagonal nanorods of different sizes, and can exhibit excellent optical properties and catalytic activity. For example, it is possible to increase the proportion of highly reactive corner portions in the catalytic reaction and optically absorb visible light in the visible region, specifically in the region of 370 nm to 600 nm.
The zinc oxide nanoparticle manufacturing method of the present invention is expected to be extended to large scale synthesis of other metal oxide nanoparticles such as TiO 2 and CeO 2 .
According to the present invention, zinc oxide nanoparticles can be produced simply and safely with high production efficiency.
According to the present invention, zinc oxide nanoparticles having excellent optical properties, catalytic activity, and magnetic properties can be prepared and applied to the display, the information communication industry, and the optical device field including semiconductors.
1 is an XRD pattern (a) of ZnO nanoparticles synthesized by heating an aqueous solution containing Zn (NO 3 ) 2 and octylamine at 60 ° C. for 2 hours according to Example 1 of the present invention, and FIG. And (c) are SEM images, and (d) are TEM images and ED patterns.
Figure 2 shows (a) the pH value recorded from an aqueous solution containing Zn (NO 3 ) 2 and octylamine after heating at 60 ° C for another reaction time according to an embodiment of the present invention, (b) 3 ) 2 and NaOH in the aqueous solution.
FIG. 3 is a SEM image showing the morphological evolution of ZnO nanovat synthesized according to the present invention. The reaction time is (a) 45 minutes, (b) 120 minutes, (c) .
4 is an SEM image of the sample prepared under the same conditions as in Fig. 1 except that (a) the reaction time is 121 minutes, (b) the aqueous solution containing the large porous particles and octylamine shown in Fig. (C) an SEM image of a sample prepared by heating the aqueous solution containing the large porous particles shown in Fig. 4 (a) at 60 DEG C for 2 hours, and d) SEM image of a sample synthesized by heating the aqueous solution containing large porous particles and NaOH shown in Fig. 4A at 60 DEG C for 2 hours.
5 is an SEM image of ZnO nanowires prepared under the same conditions as in Fig. 1 except that 0.4 g of (a) and 0.5 g of Zn (NO 3 ) 2 of various weights were used.
6 is an SEM image of ZnO nanowires prepared under the same conditions as in FIG. 1 except that (a) synthesis was performed at various temperatures of (a) 70 ° C and (d) 50 ° C.
FIG. 7 shows the (a) UV-vis spectrum and (b) the photoluminescence spectrum (PL spectra) of ZnO nanovat shown in FIG.
8 is a TGA thermogram of the octylamine stabilized ZnO nanovolts shown in FIG.
9 is an SEM image of a sample prepared under the same conditions as in Fig. 1, except that it was synthesized in the presence of 0.2 g of Zn (NO 3 ) 2 .
Hereinafter, the present invention will be described in more detail with reference to the following examples and experimental examples. However, the following Examples and Experimental Examples are for illustrating the present invention, and the scope of the present invention is not limited by the following Examples and Experimental Examples.
≪ Example 1 >
0.297 g of Zn (NO 3 ) 2 and 0.8 g of octylamine were dissolved in 10 mL of deionized water, heated slowly to 60 ° C, and aged by magnetic stirring at the same temperature for 2 hours. Acetone (35 mL) was added to precipitate the nanoparticles, followed by centrifugation to recover the ZnO nanoparticles. Octylamine, Zn (NO 3 ) 2 (≥99%), and sodium hydroxide (NaOH, ≥98%) were purchased from Aldrich and used without further purification. Water was deionized water purified using ion exchange.
≪ Example 2 >
ZnO nanoparticles were obtained in the same manner as in Example 1 except that 0.4 g of Zn (NO 3 ) 2 was used. As shown in FIG. 5A, ZnO nanoparticles having an average size of 500 nm were synthesized.
≪ Example 3 >
ZnO nanoparticles were obtained in the same manner as in Example 1 except that 0.5 g of Zn (NO 3 ) 2 was used. As shown in FIG. 5B, a large hierarchical structure formed by coalescence of ZnO nanoparticles was observed.
<Example 4>
ZnO nanoparticles were obtained in the same manner as described in Example 1, except that the synthesis was carried out at a temperature of 70 ° C.
≪ Example 5 >
ZnO nanoparticles were obtained in the same manner as described in Example 1, except that the synthesis was carried out at a temperature of 50 ° C.
≪ Comparative Example 1 &
ZnO nanoparticles were obtained in the same manner as in Example 1 except that 0.2 g of Zn (NO 3 ) 2 was used.
Table 1 below shows the process conditions and the yields of Examples 1 to 5 and Comparative Example 1. < tb > < TABLE >
As shown in Table 1, the ZnO nanoparticles of Example 1 had a high yield of 91.68%, whereas the ZnO nanoparticles of Comparative Example 1 had a low yield of 84.2%.
The following experiment was performed on the ZnO nanoparticles of Example 1 above.
≪ Experimental Example 1 > TEM and SEM analysis
TEM and high-resolution TEM (HRTEM) images were obtained using a JEM-2100F microscope operated at 200 kV. A scanning electron microscope (SEM) image was obtained using a LEO SUPRA 55 microscope.
FIG. 1B is a characteristic SEM image of the ZnO nanoparticles, indicating that the ZnO nanoparticles in the form of bolts were successfully synthesized in the aqueous phase.
1C is a high-resolution SEM image of the ZnO nanoparticles. It is clear that the ZnO nanoparticles of Example 1 have a hierarchical structure consisting of two well-defined hexagonal nanorods of different sizes.
Referring to FIG. 1C, the diameter and length of the first hexagonal nanorod are 250 and 170 nm, respectively, and the diameter and length of the second hexagonal nanorod are 230 and 180 nm, respectively. The presence of tertiary hexagonal nanorods was not observed at the top of the secondary nanorods or at the bottom of the primary nanorods.
FIG. 1d is a TEM image of a top surface of ZnO nanoparticles and corresponding electron diffraction (ED) (illustration), wherein the ZnO nanoparticles of the present invention are composed of two well-defined hexagonal nanorods of different sizes It has an enemy structure. The ED pattern consists of a spot of six-fold rotational symmetry, the product is a single crystal with hexagonal-wurzite crystal structure, and the top and bottom surfaces of ZnO are surrounded by (111) .
The transmission electron microscope (TEM) and electron diffraction pattern (ED) analysis of the ZnO nanoparticles revealed that the ZnO nanoparticles prepared according to the present invention are single crystalline.
<Experimental Example 2> XRD pattern analysis
A powder X-ray diffraction (XRD) pattern of the product was obtained using a Rigaku D-MAX / A diffractometer at 35 kV and 35 mA.
The powder XRD patterns show the presence of diffraction peaks at 31.8 °, 34.5 °, 36.3 °, and 47.6 °, which can be assigned to the (100), (002), (101) and (102) (Fig. 1A, P63mc , a = 3.253 A, Joint Committee on Powder Diffraction Standards [JCPDS] file no. 80-0074). No diffraction peaks corresponding to the impure crystalline phase were observed in the above Fig.
≪ Experimental Example 3 > UV-vis spectrum analysis
The UV-vis spectra of the product were recorded using a Jasco UV-vis spectrometer in the 250800 nm range. The results are shown in Fig. 7A.
Figure 7a shows the recorded UV-vis absorption spectrum from an aqueous suspension of zinc oxide nanoparticles. A strong absorption peak at 400 nm was observed. The room temperature photoluminescence spectrum of the ZnO nanoparticles is shown in FIG. 7B. The presence of a broad blue band emission at about 469 nm suggests that it may be due to a single ionized oxygen deficiency and other defects.
≪ Experimental Example 4 > TGA and fluorescence spectrum analysis
The yield of the ZnO nanoparticles of Example 1 was calculated using TGA in a nitrogen atmosphere at a heating rate of 20 ° C / min. A TGA Q5000 IR thermal analyzer was used for this purpose.
As shown in FIG. 8, according to the present invention, the octylamine-stabilized ZnO nanoparticles showed a weight loss of about 1.1% at a temperature as high as 410 ° C. Based on calculations using TGA data, it was found that the percent yield of ZnO nanoparticles of Example 1 was greater than 91%.
Fluorescence spectra were also obtained using QM-4-2005SE (PTI, USA).
<Experimental Example 5> Analysis of growth pattern of zinc oxide nanoparticles
To understand the growth behavior of the zinc oxide nanoparticles of the present invention, a portion of the reaction solution was taken at various reaction steps and analyzed using SEM analysis.
3 is an SEM image of zinc oxide nanoparticles sampled at 45, 120, 121 and 125 minutes. At the initial stage of the reaction ( t = 45 min), a large amount of small nanoparticles having a size of about 40 nm was observed (see FIG. 3A). In the sample taken at t = 120 min, small nanoparticles began to aggregate and produced aggregates with sizes larger than 600 nm (see Fig. 3b). At t = 121 min, the aggregates formed hierarchical hexagonal pelletized porous particles of size greater than 450 nm (see Figure 3c). At t = 125 min, the surface of the particles was smoothed and dense, indicating that single crystal hexagonal nanoporous zinc oxide nanoparticles were formed (see FIG. 3D).
In addition, the method for preparing oxide particles of the present invention can produce hexagonal nanoporous zinc oxide nanoparticles by oriented-attachment.
The reaction was stopped at a reaction time of 121 minutes, and the product was washed with acetone to remove residual reagent to obtain a hierarchical hexagonal-shaped, rod-shaped porous particle having a size of about 450 nm (see FIG.
When the aqueous solution containing the porous particles and octylamine was heated at 60 ° C for 2 hours, the particle size was reduced to a small extent and the edges of the nanoparticles were sharpened (see FIG. 4b) .
However, the present inventors have found that when large porous particles are aged only in the aqueous phase (Fig. 4C) and aged in an aqueous base solution using NaOH to increase the pH (see Fig. 4d) I have not observed any shape changes. Thus, it can be seen that octylamine is an essential component of direct attachment of ZnO nanoparticles.
<Experimental Example 6> Analysis of effect of reaction temperature
When ZnO nanoparticles were synthesized at a reaction temperature of 50 ° C, small ZnO nanoparticles were produced.
When performed at a reaction temperature of 70 ° C, larger zinc oxide nanoparticles (> 750 nm in size) were synthesized (see FIG. 6a). This demonstrates that the reaction temperature is important for the controlled growth of ZnO nanoparticles.
<Experimental Example 7> Analysis of influence of concentration of zinc precursor
In one embodiment of the present invention, larger ZnO nanoparticles having an average size of 500 nm were synthesized when increasing the amount of Zn (NO 3 ) 2 in Example 1 of the present invention to 0.4 g (see FIG. 5 a) ).
Alternatively, when the amount of Zn (NO 3 ) 2 was increased to 0.5 g, a large hierarchical structure formed by coalescence of ZnO nanoparticles was observed (see FIG. 5B).
On the other hand, when the amount of Zn (NO 3 ) 2 was reduced to 0.2 g, irregular forms of agglomerates larger than 650 nm in size were produced (see FIG. 9).
Referring to FIG. 1C, the diameters and lengths of the first hexagonal nanorods are 250 and 170 nm, respectively, and the diameter and length of the second hexagonal nanorod are 230 and 180 nm, respectively. The zinc oxide nanoparticles of the present invention have different diameters Of the hexagonal nanorods of FIG.
Claims (9)
The weight ratio of alkylamine to zinc precursor in the aqueous solution is 1: 1.5 to 1: 3,
Wherein the concentration of the zinc precursor is 0.15 M to 0.3 M.
Wherein the zinc precursor is zinc chloride (ZnCl 2), zinc sulfate (ZnSO 4), zinc acetate (Zn (CH 3 CO 2) 2), zinc sites rate (Zn 3 [O 2 CCH 2 C (OH) (CO 2) CH 2 CO 2] 2), zinc nitrate (Zn (NO 3) 2) , zinc nitrate hexahydrate (Zn (NO 3) 2 · 6H 2 O) and zinc ahseteyiteuyi hydrate (Zn (OOCCH 3) 2 · 2H 2 O Wherein the zinc oxide nanoparticles are at least one compound selected from the group consisting of zinc oxide nanoparticles and zinc oxide nanoparticles.
Wherein the alkylamine has 6 to 20 carbon atoms.
And the reaction temperature is 50 to 70 ° C.
Wherein the pH of the aqueous solution is 9 or more.
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| KR102214129B1 (en) * | 2019-08-20 | 2021-02-08 | 진수언 | Method for preparing self-assembled porous 3-dimensional zinc oxide nanoparticle structures using a microfluidic device, porous zinc oxide nanoparticles prepared thereby, self-assembled aggregates of zinc oxide nanoparticles prepared thereby, self-assembled porous 3-dimensional zinc oxide nanoparticle structures prepared thereby and bioink comprising the same |
| WO2024057297A1 (en) * | 2022-09-12 | 2024-03-21 | Lppm Universitas Andalas | Bacillus sp. strain uaacbes 01l bacterial isolate as a bioreductor in green biosynthesis of zink oxide nanoparticles |
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| WO2008118422A1 (en) | 2007-03-26 | 2008-10-02 | The Trustees Of Columbia University In The City Of New York | Metal oxide nanocrystals: preparation and uses |
| KR101426281B1 (en) | 2012-06-22 | 2014-08-05 | 인텔렉추얼디스커버리 주식회사 | ZnO NANOSTRUCTURED MATERIALS AND MANUFACTURING METHOD THEREOF |
| KR101564005B1 (en) * | 2014-04-29 | 2015-10-27 | 한국과학기술원 | Method for manufacturing of ZnO |
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| WO2008118422A1 (en) | 2007-03-26 | 2008-10-02 | The Trustees Of Columbia University In The City Of New York | Metal oxide nanocrystals: preparation and uses |
| KR101426281B1 (en) | 2012-06-22 | 2014-08-05 | 인텔렉추얼디스커버리 주식회사 | ZnO NANOSTRUCTURED MATERIALS AND MANUFACTURING METHOD THEREOF |
| KR101564005B1 (en) * | 2014-04-29 | 2015-10-27 | 한국과학기술원 | Method for manufacturing of ZnO |
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