KR101650084B1 - Method for preparing silver oxide using cathodic electrochemical synthesis and silver oxide nanoparticles prepared thereby - Google Patents
Method for preparing silver oxide using cathodic electrochemical synthesis and silver oxide nanoparticles prepared thereby Download PDFInfo
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- KR101650084B1 KR101650084B1 KR1020150085202A KR20150085202A KR101650084B1 KR 101650084 B1 KR101650084 B1 KR 101650084B1 KR 1020150085202 A KR1020150085202 A KR 1020150085202A KR 20150085202 A KR20150085202 A KR 20150085202A KR 101650084 B1 KR101650084 B1 KR 101650084B1
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- C01G5/00—Compounds of silver
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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Abstract
(A) supplying an aqueous solution containing silver nitrate and sodium sulfate to an electrolytic bath having an oxidizing electrode and a reducing electrode; (b) depositing silver oxide particles by applying a potential to the oxidation electrode and the reduction electrode; And (c) recovering the silver oxide precipitated in the step (b), and an oxide particle produced thereby.
According to the method for producing silver oxide using electrochemical synthesis according to the present invention, high-purity silver oxide particles can be produced with high yield by a simple process of applying electric potential above the threshold potential of water molecules, and the concentration of silver ions and the potential Can be controlled to control the particle size, shape and yield of silver oxide.
Description
The present invention relates to a method for producing silver oxide using electrochemical synthesis in a reducing electrode and silver oxide nanoparticles produced thereby.
In general, silver oxide exists in various forms such as Ag 2 O, AgO, Ag 2 O 3, or Ag 3 O 4. Of these, Ag 2 O is most stable and has a band gap energy of 1.4 eV Are well known as p-type semiconductors.
Such Ag 2 O (hereinafter, referred to as silver oxide) has been attracting attention due to its catalytic, electrochemical, electrical and optical properties depending on the type of crystal structure, and such silver oxide has been widely used for hydroquinone and carbon monoxide It can be used as a catalyst such as catalytic oxidation or water splitting reaction or as an ammonia detection sensor for a photovoltaic cell or a fuel cell or a reduction electrode for a zinc- have.
The silver oxide has morphologically various forms such as a cube type, a rhombicuboctahedra type, and a
Various studies have been carried out to produce silver oxide exhibiting such characteristics. Various studies have been conducted on the silver oxide nanostructures using chemical, reactive sputtering, thermal deposition or electrochemical methods. There have been various attempts to manufacture thin films.
For example, in the prior art documents (
However, the methods disclosed in
As another example, in the prior art documents (Non-Patent
However, in the method of manufacturing silver oxide disclosed in
Therefore, there is a need for research on a method capable of solving the disadvantages of the above production methods and capable of producing silver oxide of high purity.
The inventors of the present invention have found that when a potential is applied to an aqueous solution containing silver nitrate (AgNO 3 ) and sodium sulfate (Na 2 SO 4 ) Ag 2 O) particles were precipitated to produce high-purity silver oxide nanoparticles.
Accordingly, the present invention provides a method for producing silver oxide using electrochemical synthesis in a reducing electrode and a technical content of the silver oxide nanoparticle produced thereby.
(A) supplying an aqueous solution containing silver nitrate and sodium sulfate to an electrolytic bath having an oxidizing electrode and a reducing electrode, (b) applying an electric potential to the oxidizing electrode and the reducing electrode to precipitate the silver oxide And (c) recovering the silver oxide precipitated in the step (b). The present invention also provides a method for producing silver oxide by electrochemical synthesis in a reducing electrode.
In one embodiment, the oxidizing electrode and the reducing electrode may be made of silver (Ag), copper (Cu), gold (Au), or platinum (Pt).
In one embodiment, the concentration of silver nitrate in step (a) is from 1 to 50 mM, the concentration of sodium sulfate is from 0.1 to 1 M, and the potential can be greater than 2 V.
In one embodiment, the weight ratio (silver oxide / silver) of the silver oxide precipitated in step (b) and the silver particles deposited on the reducing electrode may be 1 to 23.
In one aspect of the present invention, silver oxide particles produced by the above method are provided.
In one embodiment, the silver oxide particles may be a hexapod structure or a polyhedral structure of
According to the method for producing silver oxide using electrochemical synthesis in the reducing electrode according to the present invention, high-purity silver oxide particles can be produced with high yield by a simple process of applying a potential higher than 2 V, The particle size, shape and yield of silver oxide can be controlled by adjusting the dislocation potential.
In addition, the method for producing silver oxide according to the present invention can be applied for various metal oxide production.
1 is a process diagram showing each step of the method for producing silver oxide according to the present invention.
Figure 2 shows the XRD pattern analysis results of the precipitates prepared according to Examples 1 and 5.
FIG. 3 is a graph showing the results of measurement of the electron state and band gap energy of silver oxide prepared according to Example 1 and Example 5. FIG.
Fig. 4 is a graph showing the FE-SEM image and particle size of the surface of the silver oxide particles prepared according to Examples 1 to 5; Fig.
Fig. 5 is a TEM image of the silver oxide particles prepared in Example 2, (b) an enlarged image of (a), (c) a SAED pattern image of electron diffraction, (d) And (e) a crystal grain.
6 is an FE-SEM image of a surface of silver oxide particles prepared according to Examples 6 to 8. FIG.
7 is a graph showing weight ratios of silver oxide silver particles (Ag 2 O / Ag) particles of silver oxide particles prepared according to Examples 1 to 5 and Comparative Examples.
(A) supplying an aqueous solution containing silver nitrate and sodium sulfate (Na 2 SO 4 ) to an electrolytic bath having an oxidizing electrode and a reducing electrode, (b) And (c) recovering the silver oxide precipitated in the step (b). The silver oxide fine particles are precipitated in the step (b).
In the step (a), an aqueous solution containing silver nitrate and sodium sulfate is supplied to an electrolytic bath having an oxidizing electrode and a reducing electrode for preparing silver oxide.
At this time, the oxidizing electrode and the reducing electrode can be used without restrictions as long as they can supply current with high efficiency. An electrode made of a material such as silver (Ag), copper (Cu), gold (Au), or platinum But are not limited thereto.
The aqueous solution to be supplied to the electrolytic bath may be configured to contain silver nitrate at a concentration of 1 to 50 mM and sodium sulfate at a concentration of 0.1 to 1 M.
In the step (b), a potential is applied to the oxidizing electrode and the reducing electrode to deposit silver oxide particles.
The principle of precipitation of the silver oxide particles in this step can be performed on a simple principle as shown in the following formulas (1) and (2).
[Chemical Formula 1]
2H 2 O + 2e - -> H 2 + 2OH -
(2)
2Ag + + 2OH - - > Ag 2 O + H 2 O
When a voltage is applied to the oxidizing electrode and the reducing electrode of the electrolytic bath to which the aqueous solution is supplied, an electrochemical potential is generated, and a potential is applied to the aqueous solution. As a result of the applied potential, The water molecules are reduced to electrolysis (electrolysis) to produce hydroxide ions (OH - ).
The generated hydroxide ion reacts with silver ion (Ag + ) as shown in
The precipitated silver oxide particles are formed by bonding silver oxide fine particles having a size of about 10 nm precipitated by an electrochemical method and can form silver oxide particles having a hexafod structure or a polyhedral structure of group VI.
At this time, the particle size, shape and yield of precipitated silver oxide can be controlled by the intensity of the potential applied and the concentration of silver ions (Ag + ).
More specifically, the precipitated silver oxide particles have a tendency that the applied potential affects the growth of the size of the oxidized silver hexafod particles, and the size of the silver oxide particles decreases as the applied potential increases.
The potential is electrolysis of water, the potential is applied when the water particles are electrolyzed in excess of possible threshold potential of hydrogen ions (H +) and hydroxide ions (OH -) are is formed, the hydrogen produced as a result of the electrolysis of water This is caused by an abrupt increase in the concentration of molecules, which is caused by the hydrogen gas interfering with the growth of the grain size due to the introduction of hydrogen gas into the region where silver oxide precipitation occurs and the continuous growth of the silver oxide particles is inhibited.
The morphological characteristics of the silver oxide particles may be influenced by the concentration of silver ions (Ag + ) formed by dissolving silver nitrate in the aqueous solution supplied to the aqueous solution. When the concentration of silver ions (Ag + ) is low, When the concentration of silver ions (Ag + ) increases, silver oxide particles having a complete hexapod structure are formed, and the size of silver oxide particles formed also tends to increase in proportion thereto.
The reason for this characteristic is that the precipitation rate of silver oxide is increased in proportion to the concentration of silver ion (Ag + ).
The generated silver oxide particles can grow in the (100) direction or in the (111) direction, and when the ratio R of the (100) direction growth and the (111) direction growth is 0.58 or less, Silver oxide particles can be formed. When the ratio R is 1.73 or more, it can be formed in the form of octahedron.
When the ratio R is 0.58 < R < 1.73, polyhedron silver oxide particles having a (111) plane and a (100) plane exposed may be formed. Particularly in a silver (Ag) crystal having an isotropic face-centered cubic structure, a state of dynamic equilibrium forms a convex polyhedron bounded by (111) plane and (100) plane. In contrast, when a concentration gradient is formed by silver ions (Ag + ), the stability of the interfacial morphology is lost and branches are formed. Finally, silver oxide particles having a hexafod structure of
Therefore, the growth rate of the silver oxide increases due to the abrupt increase in the concentration of the silver ion (Ag + ). As a result, the interface shape of the silver oxide loses its stability and the unbalanced state is induced to form a bridge, The oxidation of the structure is the formation of silver particles.
In addition, the formation ratio of the silver oxide precipitated around the reducing electrode and the silver particle deposited on the surface of the reducing electrode varies depending on the applied potential, and the higher the dislocation is, the more precipitated silver oxide increases, Which is proportional to the size of the film.
As described above, the ratio (Ag 2 O / Ag) of the precipitated silver oxide particles and the silver particles deposited on the reducing electrode may be 1 to 23. At this time, the weight ratio (Ag 2 O / Ag) of the precipitated silver oxide particles to the silver particles deposited on the reducing electrode increases until it reaches approximately 23, and exhibits a characteristic of 23 even when the potential increases continuously.
This is because a region where a hydroxide ion (OH - ) concentration is increased while a water molecule is electrolyzed by an applied electric potential to form a precipitate of silver oxide is formed, so that even if the dislocation increases, the weight ratio of silver oxide / silver particles does not change As a result of this, a potential is applied so that the potential applied exceeds 2 V exceeding the threshold potential at which electrolysis of water is possible, and a potential within 10 V where the Ag 2 O / Ag ratio is 23 is added So as to produce silver oxide particles.
When a potential in the above range is applied, precipitation of silver oxide by an electrochemical synthesis method occurs more strongly than precipitation of silver particles on a reduction electrode, and silver oxide precipitates more strongly and silver oxide particles can be produced very efficiently by precipitating silver oxide particles.
In the step (c), the precipitated silver oxide particles are recovered, and the aqueous solution containing the precipitated silver oxide particles as described above may be dried or centrifugally separated by various known methods to recover the silver oxide particles.
In addition, in this step, the silver oxide particles prepared as described above may be further washed with ultrapure water or distilled water to remove impurities contained in the silver oxide particles.
In one aspect of the present invention, there is provided a silver oxide powder produced by the method described above.
The silver oxide particles may have an average particle size of 0.5 to 2 占 퐉 and may be composed of crystals comprising a hexapod structure or a polyhedral structure of
According to the method for producing silver oxide using the electrochemical method according to the present invention as described above, a silver oxide precipitate is formed around the reducing electrode by a simple process of applying a potential above the threshold potential of water molecules, And the particle size, shape and yield of silver oxide can be controlled by adjusting the concentration of silver ions and the potential applied thereto.
In addition, the method for producing silver oxide using the electrochemical method according to the present invention can not only manufacture silver oxide particles with high purity very efficiently but also can be applied to the production of various metal oxides such as CuO, ZnO, MgO, and FeO .
Hereinafter, the present invention will be described in more detail with reference to examples.
The embodiments presented are only a concrete example of the present invention and are not intended to limit the scope of the present invention.
Example 1. Preparation of silver oxide by adding a potential of 4 V
To prepare the silver oxide particles, an electrolytic cell equipped with two electrodes made of a rod-shaped silver (Ag) sample (diameter: 3.175 mm, 99.9%, Alfa) spaced 3 cm apart serving as an oxidizing electrode and a reducing electrode was used.
An aqueous solution at 25 캜 containing 20 mM silver nitrate (AgNO 3 , purity 99.9%, Kojima chemicals) and 0.4 M sodium sulfate (Na 2 SO 4 , purity 99% or more, Junsei) was supplied to the electrolytic bath.
Electric current was supplied to the electrolytic cell for 10 minutes to form a potential difference, and a potential of 4 V was applied to induce electrolysis of the water. As a result, a brownish colored precipitate was formed around the reducing electrode, and a light ash-colored substance was deposited on the reducing electrode.
The aqueous solution containing the precipitate was centrifuged to obtain a precipitate. Ultrapure water was added to the precipitate to wash it, followed by centrifugation again to obtain a washed precipitate to prepare silver oxide particles.
Example 2. Preparation of silver oxide by adding a potential of 5 V
Silver oxide particles were prepared in the same manner as in Example 1, except that electrolysis of water was induced by applying a potential of 5 V to the electrolytic bath.
Example 3 Preparation of silver oxide by applying a potential of 6 V
Silver oxide particles were prepared in the same manner as in Example 1 except that the electrolytic bath was subjected to a potential of 6 V to induce electrolysis of water.
Example 4. Preparation of silver oxide by applying a potential of 8 V
Silver oxide particles were prepared in the same manner as in Example 1, except that the electrolytic bath was subjected to an electric potential of 8 V to induce electrolysis of water.
Example 5. Preparation of silver oxide by applying a potential of 10 V
Silver oxide particles were prepared in the same manner as in Example 1, except that the electrolytic bath was subjected to a potential of 10 V to induce electrolysis of water.
Example 6 To an aqueous solution containing 1 mM silver nitrate and sodium sulfate was added a potential of 5 V to prepare silver oxide
Silver oxide particles were prepared in the same manner as in Example 1, except that electrolysis of water was induced by applying a voltage of 5 V for 10 minutes to an aqueous solution containing 1 mM silver nitrate and 0.4 M sodium sulfate.
Example 7 An aqueous solution containing 5 mM of silver nitrate and sodium sulfate was added to a potential of 5 V to prepare silver oxide
Silver oxide particles were prepared in the same manner as in Example 1, except that electrolysis of water was induced by applying a voltage of 5 V for 10 minutes to an aqueous solution containing 5 mM of silver nitrate and 0.4 M of sodium sulfate.
Example 8 An aqueous solution containing 10 mM of silver nitrate and sodium sulfate was added to a potential of 5 V to prepare silver oxide
The silver oxide particles were prepared in the same manner as in Example 1 except that electrolysis of water was induced by applying a potential of 5 V for 10 minutes to an aqueous solution containing 10 mM of silver nitrate and 0.4 M of sodium sulfate.
Comparative Example. Electrolysis of the aqueous solution by applying a potential of 2 V
Electrolysis of the water was induced by applying an electric potential of 2 V for 10 minutes to the electrolytic cell supplied with the same aqueous solution as in Example 1. As a result, only silver deposition was observed around the reducing electrode and on the surface of the reducing electrode.
Test Example 1. Analysis of the chemical composition of the obtained precipitate
For the chemical composition analysis of the precipitates prepared according to Examples 1 and 5, XRD pattern analysis was performed and the XRD pattern analysis results are shown in FIG. For XRD pattern analysis, X-ray diffraction (XRD, X'PERT, PANalytical, Cu K radiation) was used.
As shown in Fig. 2, an XRD pattern (Fig. 2 (a)) in a precipitate produced by supplying a potential of 4 V and an XRD pattern (Fig. 2 (b)) in a precipitate produced by supplying a potential of 10 V Was the same as the XRD pattern (FIG. 2 (c)) of the cubic Ag 2 O (JCPDS 41-1104) showing a cubic lattice structure. It was confirmed that the precipitate prepared was silver oxide.
In order to analyze the chemical composition of the precipitate prepared according to Examples 1 and 5, the electronic state and band gap energy of the precipitate were measured by XPS and UV-Vis measurement, and the measurement results are shown in FIG. The electron state of the precipitate powder was measured by X-ray photoelectron spectroscopy (XPS, Multilab 2000, Thermo Scientific, Al Ka radiation), and the band gap energy of the precipitate particles was measured by ultraviolet visible .
3 (a)) and 529.5 eV (Fig. 3 (b)) of Ag (3d 5/2 ) and O (1s) peaks, respectively, (Ag 2 O) coincided with the 3d energy level of the ion and the 1s energy level of the oxygen ion, and it was confirmed that the precipitate particles were composed of silver (I) oxide (Ag 2 O).
Test Example 2. Morphological Characterization of Silver Oxide Particles
In order to analyze the morphological characteristics of the silver oxide particles prepared according to Examples 1 to 5, field emission scanning electron microscopy (FE-SEM, MIRA II LMH, Tescan) and electric field pre- The silver oxide particles prepared by using a microscope (field emission transmission electron microscopy, FET-TEM, JEM 2100F model, JEOL, operating at 200 kV) were photographed and the size of the prepared silver oxide particles was measured. .
As shown in the FE-SEM image of FIG. 4, the silver oxide particles prepared according to Example 1 (FIG. 4A), Example 2 (FIG. 4B) and Example 3 (FIG. Can be confirmed to show a hexapod structure of
Further, as shown in Fig. 4 (f), the average particle size of the silver oxide particles produced according to Examples 1 to 5 was 1.84 占 퐉 for Example 1, 1.36 占 퐉 for Example 2, The average particle size of the oxidized silver hexafod particles was found to be smaller as the electric potential applied was increased to 0.87 μm in Example 4, 0.63 μm in Example 4 and 0.6 μm in Example 5. From these results, it was confirmed that the applied electric potential affects the growth of the size of hexahedral silver oxide particles.
As described above, as the dislocation increases, the reason why the silver oxide decreases in the average particle size of hexapod is predicted to occur due to the abrupt increase in the concentration of hydrogen molecules produced as a result of the electrolysis of water, It was predicted that hydrogen gas would be introduced to inhibit the continuous growth of the silver oxide particles, and that the growth of the particle size would be caused by the obstruction of the hydrogen gas.
As a result of measuring the lattice constant of the silver oxide based on the XRD pattern analysis results, the lattice constant of the silver oxide particles prepared according to Example 1 and Example 5 was 4.726 Å, and the lattice constant of commercial silver oxide was 4.726 Å (JCPDS Data).
It can be seen that the intensity of the (111) peak in the XRD pattern is dominant in the silver oxide hexapod particles, and that the silver oxide particles are bounded by the equivalent (111) plane.
In addition, since the prepared silver oxide crystals exhibit a lattice structure in which an equivalent (111) plane is exposed when silver atoms are positively charged on the surface, the nanoparticles exposed to the neutral (100) plane in the photocatalytic reaction It can be confirmed that it is more efficient in the photocatalytic reaction.
In order to more efficiently understand the growth mechanism of silver oxide particles, the silver oxide particles prepared according to Example 2 were subjected to field emission transmission electron microscopy (FE-TEM) and high resolution scanning electron microscope (HR-TEM ) Was used to observe silver hexafodide oxide particles. The observation result is shown in Fig.
FIG. 5 (a) is a TEM image of silver hexoxide particles prepared according to Example 2, and FIG. 5 (b) is a TEM image of bridges of silver oxide hexaphod particles prepared according to Example 2. FIG. As shown in FIGS. 5 (a) and 5 (b), it can be seen that the silver oxide hexafod particles prepared according to Example 2 were formed by massing fine particles having a size of 10 nm like a building block. And it can be predicted that the rough surface of the silver oxide hexapod particles is caused by the crystallization mechanism of the atypical meso-size junction from the typical ionic bond.
FIG. 5 (c) is an electron diffraction pattern image showing an electron diffraction pattern of a selected region of silver oxide hexafod particles prepared according to Example 2, showing an electron diffraction pattern image of a region selected from the legs of silver oxide hexafod particles prepared according to Example 2 It can be seen that the ion diffraction pattern exhibits the property of a polycrystalline ring consisting of a number of diffracted light spots which cause bragg reflection of each regular crystal. It can be predicted that the oxidized silver hexafod particles produced in this way are essentially polycrystalline and composed of large amounts of 10 nm sized silver oxide microparticles.
5 (d) is an HR-TEM image showing the edge of the leg of the silver oxide produced according to Example 2, showing the crystallographic orientation of the leg of the silver oxide hexafod particle in the building block .
As shown in Fig. 5 (d), the plane spacing of the (111) and (200) lattice planes in the cubic silver oxide silver lattice was measured at 0.271 nm and 0.235 nm, and the 111 pair twin planes It can be confirmed that it exists. It can also be seen that the (111), (11-1) and (200) planes are parallel to the planes of (111), (11-1) And the (200) face were exposed.
Further, as shown in Fig. 5 (e), it was predicted that hexapod was mainly grown from the equivalent (111) plane and the (200) plane and formed along the equivalent (100) direction.
Test Example 3: Ag ion (Ag + Analysis of Morphological Changes of Silver Oxide Particles
The surfaces of the silver oxide particles produced according to Examples 6 to 8 were photographed using a scanning electron microscope, and the results of the photographing are shown in FIG.
As shown in Fig. 6, it can be confirmed that the silver oxide particles of Example 6 (Fig. 6 (a)) having the smallest silver ion concentration exhibit the shape of a polyhedron, and the silver oxide particles produced according to Example 7 (FIG. 6 (c)) produced according to Example 8 exhibits a substantially complete hexapod form, compared to silver nanoparticles (FIG. 6 (b) And the shape of the silver oxide particles formed as the silver ion concentration increases is changed into a nearly complete hexapod form.
In addition, it can be seen that the size of silver oxide particles increases in proportion to the concentration of silver ions. As the concentration of silver nitrate increases from 10 mM to 20 mM (Fig. 2 (e)), the average size of silver oxide hexafod particles It can be confirmed that it is increased from 1 mu m or less to 1.36 mu m. It was confirmed that the morphological changes of the silver oxide hexapod polyhedra to silver oxide hexafod particles were influenced by the silver ion concentration and the precipitation rate of the silver oxide particles was proportional to the silver ion concentration.
In addition, the morphological change from cubic to octahedral can be determined by the ratio of the growth rate to the (111) direction versus (100) direction. When the particles grow at a high rate and change in concentration occurs, And the legs grow. In such a non-equilibrium condition, hexahedral silver oxide particles are formed.
Test Example 4. Analysis of yield according to the applied potential
The silver (Ag) particles deposited on the prepared silver oxide and the reducing electrode according to Examples 1 to 5 and Comparative Example were weighed to analyze the effect of the production yield by the electric potential applied for the oxidation silver oxide, / Silver (Ag 2 O / Ag) particles is shown in FIG.
As shown in FIG. 7, in the case of the comparative example, it was confirmed that silver oxide particles were not formed, and silver oxide particles were generated from the point where the applied potential exceeded 2 V.
Also, it can be seen that the weight ratio of silver oxide / silver particles increases as the potential applied for the production of silver oxide increases. From these results, it can be seen that as the dislocation increases, the precipitation of silver oxide increases and the generation of silver oxide particles is proportional to the size of dislocation.
However, when the potential of 8 V was applied, it was confirmed that the weight ratio of the silver oxide / silver particles reached 23, but even when the potential was increased to 8 V or more, the ratio remained about 23 there was.
This is mainly due to the increase of the hydroxide ion (OH - ) concentration during the electrolysis of the water molecule by the applied electric potential, so that the area where the precipitation of silver oxide is formed is formed, and the weight ratio of silver oxide / silver particles changes I was able to predict the phenomenon that did not happen.
Claims (8)
(b) depositing silver oxide particles by applying a potential to the oxidation electrode and the reduction electrode; And
(c) recovering the precipitated silver oxide in step (b)
Wherein the weight ratio (silver oxide / silver) of the silver oxide precipitated in the step (b) and the silver particles deposited on the reducing electrode is 1 to 23.
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| JP2001262206A (en) * | 2000-03-22 | 2001-09-26 | Tanaka Kikinzoku Kogyo Kk | Method for producing silver oxide and method for producing silver powder |
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| JP4462019B2 (en) | 2004-11-24 | 2010-05-12 | 昭栄化学工業株式会社 | Silver oxide powder, method for producing the same, and conductor paste |
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