KR101306663B1 - Method of manufacturing cluster shaped aluminum doped zinc oxide particles - Google Patents
Method of manufacturing cluster shaped aluminum doped zinc oxide particles Download PDFInfo
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- KR101306663B1 KR101306663B1 KR1020100101753A KR20100101753A KR101306663B1 KR 101306663 B1 KR101306663 B1 KR 101306663B1 KR 1020100101753 A KR1020100101753 A KR 1020100101753A KR 20100101753 A KR20100101753 A KR 20100101753A KR 101306663 B1 KR101306663 B1 KR 101306663B1
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Abstract
An object of the present invention is to provide a conductive zinc oxide having improved shielding performance of ultraviolet rays and infrared rays (heat rays) while maintaining high transparency to visible light using an organic solvent having a carbon chain length of 2 or more. The present invention is a conductive zinc oxide nanoparticle exhibiting a property of shielding at least 75% of ultraviolet rays, at least 85% of infrared rays while maintaining transmittance of at least 75% in the visible light region.
Description
The present invention relates to a method for producing conductive zinc oxide particles having shielding properties capable of simultaneously blocking infrared rays and ultraviolet rays, and more specifically, when synthesized, a cluster shape in which aluminum-doped zinc oxide nanoparticles of several tens of nanometers or less are aggregated. The present invention relates to a method for preparing aluminum-doped zinc oxide particles, which is significantly improved compared to conventional aluminum-doped zinc oxide.
In recent years, with increasing interest in environmental problems, in order to suppress global warming, energy saving measures for reducing power required for air conditioning have been considered.
One way to do this actively is to use energy as small as one tenth of ultraviolet light, but account for about 50% of the sun's energy and shield the infrared rays (heat rays) from the sun's high thermal effects. The way to suppress the problem is being considered.
By the way, in order for the infrared (heating) shielding material to be applied to building or vehicle glass, a certain amount of visible light transmittance must be ensured. In other words, the light in the visible region is well transmitted and the light in the infrared or ultraviolet region is required to absorb or reflect as much as possible.
Among the solar light, especially for infrared shielding, many composite polymer coating materials of PET and PMMA are used. Since polymer materials, such as PET and PMMA, are inherently inferior in durability, Since the barrier property is deteriorated and discoloration occurs, there is a problem in the transmittance of visible light. Therefore, there is a fundamental limitation in applying it to a field requiring durability such as a building material or a vehicle window. Therefore, it is desirable to use an inorganic material that can block infrared rays and ultraviolet rays as much as possible while maintaining a certain level of transmittance to visible rays for construction or vehicle, but it can effectively block infrared rays and ultraviolet rays with sufficient visible ray transmittance. Inorganic materials that can be coated at low cost have not been developed.
Meanwhile, the demand for conductive metal oxide materials is also increasing recently. Heterogeneous metal-doped conductive metal oxides such as tin-doped indium oxide (ITO), antimony-doped tin oxide (ATO), gallium-doped zinc oxide (GZO), and aluminum-doped zinc oxide (AZO) are known and these are typical conductive metal oxide materials. The materials are used for transparent conductive films and transparent electrodes such as liquid crystal displays and solar cells.
Among the most widely used ITO, there is a problem of using indium, which is an expensive metal, and in the case of ATO, the antimony used is strong, and research on conductive zinc oxide as an alternative material is being actively conducted. In order for aluminum doped zinc oxide to be widely used as a conductive material, further improvement is required in terms of electrical conductivity.
The present invention is to solve the above-mentioned problems of the prior art, it has a good transmittance to visible light and excellent blocking rate of infrared rays and ultraviolet rays can be suitably used as a material for shielding heat rays for construction or vehicles, the present invention It is an object of the present invention to provide a method for producing a cluster-shaped aluminum-doped zinc oxide particles that can replace an expensive electrode material such as ITO by improving electrical conductivity compared to conventional aluminum-doped zinc oxide particles.
As a means for achieving the above object, the present invention comprises the steps of (a) reacting an aluminum precursor and a zinc oxide precursor using a water-soluble polyol solvent to synthesize aluminum-doped zinc oxide particles, (b) synthesized aluminum-doped zinc oxide particles Filtration, (c) washing the filtered aluminum-doped zinc oxide particles, and (d) drying the washed aluminum-doped zinc oxide particles, wherein the synthesis of step (a) is carried out in an atmosphere higher than atmospheric pressure. The present invention provides a method for producing aluminum-doped zinc oxide particles having a cluster shape in which a plurality of zinc oxide particles of several tens of nanometers or less are aggregated.
In addition, in the production method according to the invention, the step (a) is characterized in that it is carried out in the autoclave.
In addition, in the method according to the invention, the reaction of step (a) is characterized in that it is carried out in an atmosphere of more than 1 atmosphere.
In the method according to the present invention, the water-soluble polyol solvent is characterized in that at least one selected from ethylene glycol, diethylene glycol, or triethylene glycol.
In the method according to the present invention, the aluminum precursor is AlCl 3 H 2 O, the zinc oxide precursor is characterized in that Zn (CH 3 COO) 2 H 2 O.
In addition, in the method according to the invention, the step (a) is characterized in that it is carried out for 5 to 24 hours at a temperature of 120 ~ 180 ℃.
In the method according to the present invention, the aluminum doping amount of the aluminum-doped zinc oxide nanoclusters is 0.1 mol% to 10 mol%, and more preferably 0.3 mol% to 3.0 mol%. .
In addition, in the method according to the present invention, the size of the cluster-shaped aluminum-doped zinc oxide particles is characterized in that 5nm ~ 350nm.
According to the present invention, clusters of clusters of aluminum-doped zinc oxide nanoparticles formed of aggregated ultrafine nanoparticles of several tens of nanometers or less can be manufactured at low cost.
In addition, the cluster-shaped aluminum-doped zinc oxide particles prepared according to the present invention exhibit good visible light transmittance (70% or more), excellent infrared ray blocking rate (80% or more), and ultraviolet ray blocking rate (90% or more), thereby coating for heat ray and ultraviolet ray shielding. It can be usefully used as a material.
In addition, the cluster-shaped aluminum-doped zinc oxide nanoparticles prepared according to the present invention has excellent electrical conductivity compared to commercially-doped aluminum-doped zinc oxide nanoparticles, and thus may be usefully used as a transparent electrode material for ITO replacement.
1 is a manufacturing process chart of the cluster-shaped aluminum-doped zinc oxide particles according to the present invention.
Figure 2 shows the chemical reaction during the synthesis of the cluster-shaped aluminum-doped zinc oxide particles according to the present invention.
Figure 3 shows the XRD analysis of the cluster-shaped aluminum-doped zinc oxide particles prepared in accordance with an embodiment of the present invention.
Figure 4 is a scanning electron micrograph of the cluster-shaped aluminum doped zinc oxide particles prepared in accordance with an embodiment of the present invention.
5 is a transmission electron micrograph of the cluster-shaped aluminum-doped zinc oxide particles prepared in accordance with an embodiment of the present invention.
FIG. 6 is a scanning electron micrograph of aluminum-doped zinc oxide nanoparticles of Hakusui Corporation used as a comparative example. FIG.
7 is a photograph comparing the solvent synthesized according to Comparative Example 4 and Example 2 with diethylene glycol as a solvent.
8 is a graph showing the transmittance of each wavelength band of the cluster-shaped aluminum-doped zinc oxide particles prepared according to the embodiment of the present invention.
9 is a graph showing the relationship between Al doping amount and transmittance of visible light, infrared light and ultraviolet light of the cluster-shaped aluminum-doped zinc oxide particles prepared according to the embodiment of the present invention.
FIG. 10 is a graph showing transmittances of wavelengths of conductive zinc oxide nanoparticles prepared according to an embodiment of the present invention, ZnO not doped with Al, and commercially available AZO of Hakusui.
Hereinafter, a method of manufacturing aluminum-doped zinc oxide nanoclusters according to the present invention will be described in detail with reference to a preferred embodiment of the present invention. However, the following examples are merely examples to help the understanding of the present invention, whereby the scope of the present invention is not reduced or limited.
1 is a manufacturing process chart of the cluster-shaped aluminum-doped zinc oxide particles according to an embodiment of the present invention. As shown in FIG. 1, the method for producing aluminum-doped zinc oxide nanoclusters according to the present invention is a synthesis step of aluminum-doped zinc oxide material (S10), a filtration step (S20), a washing step (S30), and a drying step (S40). )
The dual synthesis process (S10) is carried out through a water-soluble polyol (polyol) process, the polyol that serves as a reducing agent and solvent in the synthesis process can be used as long as it can react the zinc oxide precursor and aluminum precursor, ethylene glycol It is more preferable to use diethylene glycol and triethylene glycol alone or in combination. In the embodiment of the present invention, diethylene glycol was used alone.
As the zinc oxide precursor, zinc chloride (ZnCl 2 ), zinc acetate hydrate (Zn (CH 3 COO) 2 H 2 O), zinc nitrate hydrate (Zn (NO 3 ) 2 H 2 O), or the like may be used. In an embodiment of the present invention, zinc acetate hydrate (Zn (CH 3 COO) 2 .H 2 O) was used.
In addition, aluminum chloride hydrate (AlCl 3 H 2 O), aluminum nitrate hydrate (Zn (NO 3 ) 2 H 2 O), or the like may be used as the precursor for aluminum doping, and in the embodiment of the present invention, aluminum chloride Hydrate (AlCl 3 H 2 O) was used.
In addition, after the zinc oxide precursor and the aluminum doping precursor are added to the water-soluble polyol, the reaction should be carried out in a pressurized atmosphere. The pressurization covers the lid of the reaction vessel to form a state slightly higher than atmospheric pressure naturally by vapor pressure. Even if it is possible to synthesize the cluster-shaped zinc oxide particles, more preferably 1 psig or more. On the other hand, when the reaction is performed in an open state (ie, atmospheric pressure) without covering the lid of the reaction vessel, the mechanism is not clearly identified, but cluster-shaped zinc oxide particles are hardly synthesized. Therefore, the synthesis step (S10) is most preferably performed under a slight pressurized environment using an autoclave (autoclave).
In addition, the temperature of the synthesis step (S10) is preferably 120 ~ 190 ℃, below 120 ℃ the reaction rate of the synthesis of aluminum-doped zinc oxide is too slow, when exceeding 190 ℃ carbonization of acetate constituting the zinc precursor This happens because. In the embodiment of the present invention the synthesis was carried out at 160 ℃.
In addition, the reaction time of the synthesis step (S10) is preferably 1 to 20 hours, because less than 1 hour, the synthesis reaction is difficult to occur sufficiently, the reaction is completed after 20 hours. In the embodiment of the present invention it was reacted for 5 hours.
In addition, the size of the aluminum-doped zinc oxide particles synthesized through the synthesis process (S10) is preferably 5nm ~ 350nm, it is difficult to manufacture the particle size less than 5nm, as well as dispersion in the future coating process Since it is not easy and the particle size exceeds 350 nm, visible light transmittance and conductivity may be greatly reduced, 350 nm or less is preferable.
In addition, the filtration step (S20) can be used any method as long as it can separate the synthesized zinc oxide particles and the solvent, in the embodiment of the present invention used a separator using a centrifugal force.
In addition, the washing step (S30) may also use a variety of known methods that can easily wash the synthesized zinc oxide particles, in the embodiment of the present invention the washing step (S30) to the solvent of the alcohol It was carried out by repeating two to three times in parallel to the stirring and ultrasonic washing using.
In addition, the drying step (S40) can also be used in a variety of methods, such as natural drying, forced drying, in the embodiment of the present invention to put the synthesized particles in an oven and maintained at 70 ℃ for 1 hour the solvent used in the washing process It was completely removed.
Hereinafter, the manufacturing method of each embodiment of the present invention will be described in detail.
≪ Example 1 >
Zinc acetate hydrate in the autoclave (Zn (CH 3 COO) 2 and H 2 O) 3.29g and aluminum chloride hydrate (AlCl 3 and H 2 O) 0.0109g (approximately 0.3mol%) and di-ethylene glycol was charged into a 100ml After setting the reaction pressure to 2 psig, the reaction was carried out at 160 ℃ for 5 hours.
During the reaction time, through the reaction process as shown in Figure 2, zinc oxide is synthesized.
After the reaction was terminated, the composite was separated using a centrifugal separator, and the mixture was washed by repeating two to three times by stirring and ultrasonic washing with a solvent of alcohol. Then, it was dried for 1 hour at 70 ℃ to obtain aluminum-doped zinc oxide particles.
<Example 2>
Zinc acetate hydrate in the autoclave (Zn (CH 3 COO) 2 and H 2 O) 3.29g and aluminum chloride hydrate (AlCl 3 and H 2 O) 0.0182g (approximately 0.5mol%) and di-ethylene glycol was charged into a 100ml After setting the reaction pressure to 2 psig, the reaction was carried out at 160 ℃ for 5 hours.
After the reaction, aluminum-doped zinc oxide particles according to Example 2 were obtained through the same separation, washing, and drying process as in Example 1.
<Example 3>
3.29 g of zinc acetate hydrate (Zn (CH 3 COO) 2 H 2 O), 0.037 g of aluminum chloride hydrate (AlCl 3 H 2 O) and 100 ml of diethylene glycol were added to the autoclave. After setting the reaction pressure to 2 psig, the reaction was carried out at 160 ℃ for 5 hours.
After the reaction, aluminum-doped zinc oxide particles according to Example 3 were obtained through the same separation, washing, and drying procedures as in Example 1.
<Example 4>
Zinc acetate hydrate in the autoclave (Zn (CH 3 COO) 2 and H 2 O) 3.29g and aluminum chloride hydrate (AlCl 3 and H 2 O) 0.112g (approximately 3.0mol%) and di-ethylene glycol was charged into a 100ml After setting the reaction pressure to 2 psig, the reaction was carried out at 160 ℃ for 5 hours.
After the reaction, aluminum-doped zinc oxide particles according to Example 4 were obtained through the same separation, washing, and drying procedures as in Example 1.
<Example 5>
Zinc acetate hydrate in the autoclave (Zn (CH 3 COO) 2 and H 2 O) 3.29g and aluminum chloride hydrate (AlCl 3 and H 2 O) 0.191g (approximately 5.0mol%) and di-ethylene glycol was charged into a 100ml After setting the reaction pressure to 2 psig, the reaction was carried out at 160 ℃ for 5 hours.
After the reaction, aluminum-doped zinc oxide particles according to Example 5 were obtained through the same separation, washing, and drying process as in Example 1.
<Example 6>
Zinc acetate hydrate in the autoclave (Zn (CH 3 COO) 2 and H 2 O) was added to 3.29g and aluminum chloride hydrate (AlCl 3 and H 2 O) 0.430g (about 10.0mol%) and diethylene glycol 100ml After setting the reaction pressure to 2 psig, the reaction was carried out at 160 ℃ for 5 hours.
After the reaction, aluminum-doped zinc oxide particles according to Example 6 were obtained through the same separation, washing, and drying procedures as in Example 1.
≪ Comparative Example 1 &
Zinc acetate hydrate in the autoclave (Zn (CH 3 COO) 2 and H 2 O) 3.29g and aluminum chloride hydrate (AlCl 3 and H 2 O) 0.0036g (approximately 0.1mol%) and di-ethylene glycol was charged into a 100ml After setting the reaction pressure to 2 psig, the reaction was carried out at 160 ℃ for 5 hours.
After the reaction, aluminum-doped zinc oxide particles were obtained through the same separation, washing, and drying process as in Example 1.
Comparative Example 2
Comparative Example 2 is for comparison with the conductive zinc oxide nanoparticles prepared according to the embodiment of the present invention, and are commercially available zinc oxide (Pazet) nanoparticles manufactured by Hakusui, Japan.
≪ Comparative Example 3 &
Comparative Example 3 is for comparison with the conductive zinc oxide nanoparticles prepared according to the embodiment of the present invention, commercially doped zinc oxide nanoparticles (Pazet) nanoparticles manufactured by Hakusui, Japan, doped with aluminum The amount is 0.331 mol%.
≪ Comparative Example 4 &
Zinc in an open beaker acetate hydrate (Zn (CH 3 COO) 2 and H 2 O) 3.29g and aluminum chloride hydrate (AlCl 3 and H 2 O) 0.0112g (approximately 0.3mol%) and di-one In a 100ml glycol After that, the reaction was carried out at 160 ° C. for 5 hours.
After the reaction, aluminum-doped zinc oxide particles were obtained through the same separation, washing, and drying process as in Example 1.
Particle structure analysis
First, as a result of analyzing the particles prepared according to Examples 2 to 6 of the present invention by XRD, as shown in Figure 3, it is completely crystallized at 160 ℃, hexagonal wurtzite crystal structure (wurtzite) Have In addition, although not shown in Figure 3, the XRD analysis of the particles prepared according to Example 1 was also the same as Examples 2 to 6.
In addition, as a result of observing the shape of the conductive zinc oxide nanoparticles according to an embodiment of the present invention with a scanning electron microscope, as shown in Figure 4 (Example 1), zinc oxide nanoparticles prepared according to Example 1 of the invention It can be seen that the surface has a particle shape with a plurality of protrusions formed thereon.
As a result of observing the inside of the protruding nanoparticles through a transmission electron microscope, as shown in FIG. 5 (Example 1), each particle is agglomerated with a plurality of primary crystals of 10 ~ 20nm size (primary) It can be seen that the cluster is a 100 ~ 150nm size.
In addition, as a result of observing with a scanning electron microscope, it was confirmed that not only Example 1 of the present invention but also all the particles prepared according to the Example of the present invention has the same shape as in Example 1, Comparative Example 1 also the same result Got. That is, when the synthesis is performed under a pressure higher than atmospheric pressure in the reaction using the polyol solvent according to the embodiment of the present invention, it is possible to obtain a cluster-shaped aluminum-doped zinc oxide particles.
Figure 6 shows a photograph of the aluminum-doped zinc oxide nanoparticles of Comparative Example 3 observed with a scanning electron microscope. As shown in FIG. 6, in the case of aluminum-doped zinc oxide nanoparticles according to Comparative Example 3 (commercially available product of hakusui), the shape of a single particle is not agglomerated. It can be seen that.
On the other hand, in the case of Comparative Example 4 synthesized in an open atmosphere other than the pressurized atmosphere unlike the embodiment of the present invention, as shown in Figure 7, the state before and after the synthesis is the same. That is, the synthesis of the zinc oxide nanoparticles was not made. Therefore, even if the pressure applied is very low, it can be seen that the synthesis should be performed in a pressurized atmosphere at a higher pressure than atmospheric pressure.
Visible / infrared / ultraviolet transmittance
Figure 8 shows the transmission spectrum of the zinc oxide nanoparticles prepared according to Examples 1 to 6 of the present invention with V670 Spectrophotometer (JASCO) and the zinc oxide nanoparticles according to Comparative Examples 1 and 2.
As confirmed in FIG. 8, the UV transmittances of the zinc oxide particles according to Examples 1 to 6 and Comparative Examples 1 and 2 of the present invention do not show a large difference of less than 10%, and when Al is doped, Al It can be seen that the UV transmittance slightly increased as compared with the case without doping.
In addition, the transmittance in the visible region is all 65% or more, there is almost no difference between the Al-doped zinc oxide nanoparticles according to an embodiment of the present invention or the zinc oxide particles according to Comparative Example 2 without Al doped, rather than It can be seen that the visible light transmittance of the Al-doped zinc oxide particles according to some embodiments of the present invention is high.
On the other hand, in the near infrared region of 780 to 2500 nm, in Comparative Example 2 without Al doping, the infrared transmittance is very high, and it can be seen that the blocking effect against the near infrared rays is virtually insignificant.
In addition, in the case of Comparative Example 1 doped with 0.1 mol% of Al has an infrared blocking effect compared to the case of not doped with Al, it can be seen that the effect is minimal. Therefore, in order to be used as a coating material for heat ray shielding, the doping amount of Al is preferably at least 0.3 mol% or more.
On the other hand, Examples 1 to 6 of the present invention are significantly less infrared transmittance than Comparative Examples 1 and 2, especially in the case of Examples 3 and 4 is very low infrared transmittance, it can be seen that excellent infrared blocking effect. .
9 is a graph quantitatively showing the transmittance for each wavelength band of zinc oxide nanoparticles according to Examples 1 to 6 and Comparative Examples 1 and 2 of the present invention.
As can be seen in Figure 9, even if the Al doping amount is changed to 0 ~ 10mol% it can be seen that there is almost no difference in transmittance in the ultraviolet region of the 200 ~ 380nm wavelength band.
In addition, in the case of the transmittance in the visible light region of 380 ~ 780nm, the transmittance decreases by about 4 to 5% due to the doping of Al, the visible light transmittance of the zinc oxide nanoparticles doped with Al in accordance with an embodiment of the present invention It is almost the same level as the zinc oxide particles not doped with Al.
In contrast, the transmittance in the near-infrared region in the 780 to 2500nm wavelength range rapidly decreases from about 75% to less than 20% as the doping amount of Al increases in the Al doping amount range from 0 mol% to 1 mol%. On the other hand, when the Al doping amount exceeds 3 mol%, the infrared transmittance gradually increases from 20%, but even when 10 mol% doped Al, the near infrared transmittance is about 30%, indicating a level that can be usefully used as a near infrared ray shielding material.
That is, the zinc oxide nanoparticles according to the embodiment of the present invention almost exhibits high near-infrared blocking rate (100-infrared transmittance) of almost 80% or more, and in case of example 3, the near-infrared blocking rate shows a very high blocking effect exceeding 85%. Able to know.
10 shows the transmittance of each wavelength band of Example 3, Comparative Example 2 and Comparative Example 3. As can be seen in FIG. 10, the cluster-shaped aluminum-doped zinc oxide particles according to Example 3 of the present invention have substantially the same UV transmittance and the visible light transmittance as compared to the commercially available aluminum-doped zinc oxide particles according to Comparative Example 3. Although slightly lower than Comparative Example 3, it can be seen that the near-infrared transmittance is remarkably low. That is, the cluster-shaped aluminum-doped zinc oxide particles according to Example 3 of the present invention exhibit very excellent infrared ray blocking effect compared to Comparative Example 3, which is commercially available.
Therefore, the zinc oxide nanoparticles according to the embodiment of the present invention may be suitably used for solar blocking of vehicle or building glass.
Electrical conduction characteristic evaluation
The electrical conductivity characteristics of the zinc oxide nanoparticles according to Examples 1 and 2 and the zinc oxide nanoparticles according to Comparative Example 3 were evaluated.
In order to measure the electrical conduction properties, 0.24 g of PTFE (polytetrafluoroethylene) was added to 0.2 g of the powder of zinc oxide nanoparticles according to Examples 1, 2, and Comparative Example 3 of the present invention, and then prepared into pellets. Surface resistance was measured, and the results are shown in Table 1 below.
As can be seen in Table 1, the surface resistance of the aluminum-doped zinc oxide nanoparticles according to Examples 1 and 2 of the present invention is reduced in surface resistance compared to the aluminum-doped zinc oxide particles of Hakusuui Co., Ltd. It can be seen that the electrical conductivity is improved, in particular, the cluster-shaped aluminum-doped zinc oxide particles according to Example 2 have a significant improvement in electrical conductivity compared to Comparative Example 3, and the improvement of the electrical conductivity is Presumably due to the cluster shape of the nanoparticles according to the examples.
Therefore, the aluminum-doped zinc oxide particles according to the embodiment of the present invention can also be used for the transparent electrode to replace the ITO.
Claims (10)
(b) filtering the synthesized aluminum dope zinc oxide particles;
(c) washing the filtered aluminum dope zinc oxide particles; And
(d) drying the washed aluminum-doped zinc oxide particles;
The synthesis of step (a) is carried out in an atmosphere higher than atmospheric pressure,
The aluminum doped zinc oxide particles are formed in a cluster shape in which a plurality of zinc oxide nanoparticles of several tens of nanometers or less are aggregated.
The aluminum doped amount of the aluminum-doped zinc oxide particles is 0.1 to 10 mol% so as to produce a cluster-shaped aluminum-doped zinc oxide particles.
Step (a) is a method for producing aluminum-doped zinc oxide particles of the cluster shape, characterized in that carried out in an autoclave.
The reaction pressure of the step (a) is a method of producing a cluster-shaped aluminum-doped zinc oxide particles, characterized in that more than 1 psig.
The water-soluble polyol solvent is a method for producing aluminum-doped zinc oxide particles of the cluster shape, characterized in that at least one selected from ethylene glycol, diethylene glycol, or triethylene glycol.
The aluminum precursor is AlCl 3 H 2 O characterized in that the cluster-shaped aluminum doped zinc oxide particles production method.
The zinc oxide precursor is Zn (CH 3 COO) 2 H 2 O characterized in that the cluster-shaped aluminum doped zinc oxide particles production method.
The step (a) is a method for producing the aluminum-doped zinc oxide particles of the cluster shape, characterized in that performed for 5 to 24 hours at 120 ~ 190 ℃.
The aluminum doped zinc oxide nano-cluster of the aluminum doping amount of 0.3 to 1.0 mol% so as to produce a cluster-shaped aluminum-doped zinc oxide particles.
The size of the aluminum-doped zinc oxide nanoclusters are 5nm ~ 350nm of the cluster-shaped aluminum doped zinc oxide particles production method.
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| KR101730812B1 (en) | 2016-03-30 | 2017-04-27 | 충남대학교산학협력단 | Aluminum ion doped zinc oxide luminous material and method for continuous synthesis the same |
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| KR101730812B1 (en) | 2016-03-30 | 2017-04-27 | 충남대학교산학협력단 | Aluminum ion doped zinc oxide luminous material and method for continuous synthesis the same |
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