KR101564005B1 - Method for manufacturing of ZnO - Google Patents
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- KR101564005B1 KR101564005B1 KR1020140051923A KR20140051923A KR101564005B1 KR 101564005 B1 KR101564005 B1 KR 101564005B1 KR 1020140051923 A KR1020140051923 A KR 1020140051923A KR 20140051923 A KR20140051923 A KR 20140051923A KR 101564005 B1 KR101564005 B1 KR 101564005B1
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Abstract
The present invention relates to a method for producing zinc oxide comprising stirring a solution containing a zinc salt to obtain an agitating liquid having a specific pH range, filtering the agitating liquid, and washing and drying after the filtering .
Description
The present invention relates to a method for producing zinc oxide.
One-dimensional nano-sized materials such as nanorods or nanowires are being studied extensively in electronics or optoelectronics due to their inherent optical and electrical properties.
Among them, zinc oxide (ZnO) not only has a band gap energy of 3.37 eV and a large exciton binding energy of 60 meV, but also exhibits excellent properties such as near-UV emission and piezoelectricity I am getting great interest because of betting.
However, in forming the conventional rod-shaped zinc oxide, there is a disadvantage that the spacing and alignment control of the rod are difficult and the uniformity of the rod diameter can not be ensured.
To compensate for this, various additives may be added to form rod-shaped zinc oxide. In this case, toxic components of the additive cause problems that adversely affect the human body and the environment. Furthermore, since the substrate must be provided at the time of forming the rod-shaped zinc oxide, the yield of the zinc oxide is influenced by the substrate state and it is difficult to mass-produce the zinc oxide.
In addition, as demand for various types of zinc oxide other than rod-shaped zinc oxide increases, attempts to manufacture various types of zinc oxide such as flower-shaped zinc oxide have been continued.
The present invention aims at providing a method for mass production of various types of zinc oxide by using only a reaction time and a reducing agent concentration without a substrate without using toxic additives.
One embodiment of the present invention provides a method of preparing a zinc salt, comprising: preparing a first solution comprising a zinc salt; Preparing a second solution containing a reducing agent; Stirring the first solution and the second solution to obtain an agitating liquid having a pH of 6 to 7; Filtering the mixture; And washing and drying after the filtering.
The zinc salt may be Zn (NO 3 ) 2 .6H 2 O, Zn (CH 3 COO) 2 .2H 2 O, ZnCl 2 , or ZnSO 4 .7H 2 O.
The reducing agent is selected from the group consisting of hexamethylenetetramine, substituted or unsubstituted C1 to C20 alkylamine, substituted or unsubstituted C1 to C20 alkylenediamine, substituted or unsubstituted C1 to C20 alkylenetriamine, substituted or unsubstituted C1 To C20 alkylene tetramine, or NaOH.
The reducing agent may have a molar concentration of 0.01M to 0.03M.
The first solution and the second solution may contain water as a solvent.
The stirring may be carried out for 1 hour to 3 hours.
The stirring may be carried out at a temperature of 70 ° C or more and less than 100 ° C.
The drying can be carried out at a temperature of 20 ° C to 60 ° C for 24 hours.
Another embodiment of the present invention provides a method for preparing a zinc salt, comprising: preparing a third solution comprising a zinc salt; Stirring the third solution to obtain an agitating liquid having a pH of 8 to 10; Filtering the mixture; And washing and drying the filtered zinc oxide.
The zinc salt may be Zn (NO 3 ) 2 .6H 2 O, Zn (CH 3 COO) 2 .2H 2 O, ZnCl 2 , or ZnSO 4 .7H 2 O.
The third solution may contain ammonia water as a solvent.
The ammonia water may contain water and ammonia in a volume ratio of 6: 4 to 9.5: 0.5.
The stirring may be carried out for 1 hour to 3 hours.
The stirring may be carried out at a temperature of 70 ° C or more and less than 100 ° C.
The drying can be carried out at a temperature of 20 ° C to 60 ° C for 24 hours.
The present invention does not use toxic additives and is harmless to humans and the environment, and can produce zinc oxides in various forms such as rod type and flower type without using a substrate.
1 is a flow chart of a rod type zinc oxide manufacturing method according to one embodiment.
2 is a flowchart of a flower-type zinc oxide manufacturing method according to another embodiment.
3 to 7 are scanning electron microscope (SEM) photographs of the rod-shaped zinc oxide according to Examples 1 to 5, respectively.
8 to 10 are scanning electron microscope (SEM) photographs of flower-shaped zinc oxide according to Examples 6 to 8, respectively.
11 to 13 are scanning electron microscope (SEM) photographs of the rod-shaped zinc oxide according to Comparative Examples 1 to 3, respectively.
14 and 15 are scanning electron microscope (SEM) photographs of flower-shaped zinc oxide according to Comparative Example 4 and Comparative Example 5, respectively.
16 to 20 are transmission electron microscope (TEM) photographs of the rod-shaped zinc oxide according to Examples 1 to 5, respectively.
Figs. 21 to 23 are transmission electron microscope (TEM) photographs of flower-shaped zinc oxide according to Examples 6 to 8, respectively.
24 is a result of EDAX analysis of zinc oxide according to Example 1. Fig.
25 shows the results of EDAX analysis of zinc oxide according to Example 4. Fig.
26 is a result of EDAX analysis of zinc oxide according to Example 3. Fig.
27 shows the results of EDAX analysis of zinc oxide according to Example 6. Fig.
28 shows the results of EDAX analysis of zinc oxide according to Example 7. Fig.
29 is an XRD graph of the rod-shaped zinc oxide according to Examples 1 to 3. Fig.
30 is an XRD graph of rod-shaped zinc oxide according to Examples 1, 4, and 5;
31 is an XRD graph of flower-shaped zinc oxide according to Examples 6 to 8. Fig.
Hereinafter, embodiments of the present invention will be described in detail. However, it should be understood that the present invention is not limited thereto, and the present invention is only defined by the scope of the following claims.
Unless otherwise specified herein, "alkyl group" means a C1 to C20 alkyl group, "alkenyl group" means a C2 to C20 alkenyl group, "cycloalkenyl group" means a C3 to C20 cycloalkenyl group Quot; means a C3 to C20 heterocycloalkenyl group, "an aryl group" means a C6 to C20 aryl group, an "arylalkyl group" means a C6 to C20 arylalkyl group, Refers to a
Unless otherwise specified herein, "substituted" means that at least one hydrogen atom is replaced by a halogen atom (F, Cl, Br, I), a hydroxy group, a C1 to C20 alkoxy group, a nitro group, a cyano group, A thio group, an ester group, an ether group, a carboxyl group or a salt thereof, a sulfonic acid group or a salt thereof, a phosphoric acid or a salt thereof, an amidino group, a hydrazino group, a hydrazino group, a carbonyl group, a carbamyl group, A C3 to C20 cycloalkenyl group, a C3 to C20 cycloalkynyl group, a C2 to C20 alkynyl group, a C6 to C20 aryl group, a C3 to C20 cycloalkyl group, a C3 to C20 cycloalkenyl group, Substituted by a substituent of a C2 to C20 heterocycloalkyl group, a C2 to C20 heterocycloalkenyl group, a C2 to C20 heterocycloalkynyl group, a C3 to C20 heteroaryl group, or a combination thereof.
Also, unless otherwise specified herein, "hetero" means that at least one heteroatom of N, O, S, and P is included in the formula.
"Combination" as used herein, unless otherwise specified, means mixing or copolymerization.
A rod-type zinc oxide manufacturing method according to an embodiment includes the steps of: preparing a first solution containing a zinc salt; Preparing a second solution containing a reducing agent; Stirring the first solution and the second solution to obtain an agitating liquid having a pH of 6 to 7; Filtering the mixture; And washing and drying after the filtering.
various types of rod-shaped zinc oxide can be produced without using additives including toxic components by using an agitating liquid exhibiting weak acidity of
The zinc salt may be Zn (NO 3 ) 2 .6H 2 O, Zn (CH 3 COO) 2 .2H 2 O, ZnCl 2 , or ZnSO 4 .7H 2 O. For example, the zinc salt may be Zn (NO 3 ) 2 .6H 2 O.
The reducing agent is selected from the group consisting of hexamethylenetetramine, substituted or unsubstituted C1 to C20 alkylamine, substituted or unsubstituted C1 to C20 alkylenediamine, substituted or unsubstituted C1 to C20 alkylenetriamine, substituted or unsubstituted C1 To C20 alkylene tetramine, or NaOH. For example, the reducing agent may be hexamethylenetetramine.
The reducing agent may have a molar concentration of 0.01M to 0.03M in the second solution. The nucleation reaction and the nucleation reaction can be controlled by varying the concentration of the reducing agent within the above range. Thus, various types of rod-shaped zinc oxide, for example, rod-shaped zinc oxide having a small thickness or rod- can do. If the molar concentration of the reducing agent is less than 0.01M, the reduction reaction does not occur smoothly. If the molar concentration of the reducing agent is more than 0.03M, the reducing agent is present to such an extent that the reaction can sufficiently proceed, .
The first solution and the second solution may contain water as a solvent. For example, the first solution and the second solution may be an aqueous solution. For example, the first solution may be an aqueous solution containing a zinc salt such as Zn (NO 3 ) 2 .6H 2 O, and the second solution may be an aqueous solution containing a reducing agent such as hexamethylenetetramine.
For example, the first solution can be prepared by adding a zinc salt such as Zn (NO 3 ) 2 .6H 2 O to water and shaking it for about 5 minutes to 20 minutes.
For example, the second solution can be prepared by adding a reducing agent such as hexamethylenetetramine into water and shaking it for about 5 to 20 minutes.
The stirring may be carried out at a temperature of 70 DEG C or more and less than 100 DEG C for 1 hour to 3 hours.
By varying the stirring time within the range of 1 hour to 3 hours, it is possible to produce rod-shaped zinc oxide in various forms, for example rod-shaped zinc oxide grown in various directions. As the stirring time becomes longer within 1 hour to 3 hours, the nucleation reaction becomes more dominant than the nucleation reaction, and the rod-shaped zinc oxide grows in all directions like sea urchins.
However, if the stirring time is less than 1 hour, the reaction does not proceed smoothly. If the stirring time is more than 3 hours, the reaction has already proceeded sufficiently and only a consuming reaction occurs.
On the other hand, since the stirring temperature is performed at a temperature of 70 ° C or more and less than 100 ° C, rod type zinc oxide can be produced at a low temperature without high pressure, unlike the conventional production method of producing zinc oxide under high pressure and high temperature conditions .
The filtering may be by using membrane filtration or by separating the zinc oxide particles by centrifuging the solution of the first solution and the second solution.
The drying can be carried out at a temperature of 20 ° C to 60 ° C for 24 hours. Since the drying is carried out at a low temperature range of 20 to 60 DEG C, there is an effect that the heat consumed to obtain the product is suppressed.
According to another embodiment, there is provided a method of preparing flower type zinc oxide, comprising: preparing a third solution containing a zinc salt; Stirring the third solution to obtain an agitating liquid having a pH of 8 to 10; Filtering the mixture; And washing and drying after the filtering.
Various types of flower-shaped zinc oxide can be produced without using additives including toxic components by using a weakly alkaline solution having a pH of 8 to 10. In addition, the flower-shaped zinc oxide can be produced in a simple manner in solution without a substrate by an acid and / or an alkali reaction of the precursor, so that mass production is possible.
The zinc salt may be Zn (NO 3 ) 2 .6H 2 O, Zn (CH 3 COO) 2 .2H 2 O, ZnCl 2 , or ZnSO 4 .7H 2 O. For example, the zinc salt may be a Zn (CH 3 COO) 2 · 2H 2 O.
The third solution may contain ammonia water as a solvent. For example, the third solution may be an aqueous ammonia solution. For example, the third solution may be an ammonia aqueous solution containing a zinc salt such as Zn (CH 3 COO) 2 .2H 2 O.
For example, the third solution can be prepared by adding a zinc salt such as Zn (CH 3 COO) 2 .2H 2 O to ammonia water and shaking it for about 5 minutes to 20 minutes.
For example, the ammonia water may include water and ammonia, and the water and ammonia may be contained in a volume ratio of 6: 4 to 9.5: 0.5. When the volume ratio of water and ammonia in the ammonia water is within the above range, the flower-shaped zinc oxide can be produced more easily. For example, when the ammonia is contained in an amount of less than 5% by volume based on the total volume of water and ammonia, no reduction occurs and flower-shaped zinc oxide particles are not formed.
The stirring may be carried out at a temperature of 70 DEG C or more and less than 100 DEG C for 1 hour to 3 hours.
By varying the agitation time in the range of 1 hour to 3 hours, various types of flower-shaped zinc oxide such as nonporous or porous flower-shaped zinc oxide can be produced. As the agitation time becomes longer in the range of 1 hour to 3 hours, the nucleation reaction becomes more dominant than the nucleation reaction, so that the porous flower-like zinc oxide can be obtained.
However, if the stirring time is less than 1 hour, the reaction does not proceed smoothly. If the stirring time is more than 3 hours, the reaction has already proceeded sufficiently and only a consuming reaction occurs.
On the other hand, since the agitation temperature is performed at a temperature of 70 ° C or higher to less than 100 ° C, flower type zinc oxide can be produced at a low temperature without high pressure, unlike the conventional production method of producing zinc oxide under high pressure and high temperature conditions have.
The filtering may be by using membrane filtration or by separating the zinc oxide particles by centrifuging the solution of the third solution.
The drying can be carried out at a temperature of 20 ° C to 60 ° C for 24 hours. Since the drying is carried out at a low temperature range of 20 to 60 DEG C, there is an effect that the heat consumed to obtain the product is suppressed.
The rod-shaped zinc oxide produced by the manufacturing method according to one embodiment and the flower-shaped zinc oxide produced by the manufacturing method according to another embodiment can all be applied to various fields such as organic / inorganic solar cells and organic / inorganic LED Do.
Hereinafter, preferred embodiments of the present invention will be described. However, the following examples are only a preferred embodiment of the present invention, and the present invention is not limited by the following examples.
( Rod type Preparation of zinc oxide)
Example One
0.01 M of Zn (NO 3 ) 2 .6H 2 O was added to 100 ml of water and stirred for 10 minutes to prepare a first solution.
0.01 M hexamethylenetetramine (HMT) was added to 100 ml of water and stirred for 10 minutes to prepare a second solution.
The first solution and the second solution were stirred at 90 DEG C and 300 rpm for 1 hour to obtain a solution, which was then membrane filtered and washed with distilled water.
Thereafter, it was dried at 40 DEG C for one day (24 hours) to produce rod-shaped zinc oxide.
Example 2
Rod type zinc oxide was prepared in the same manner as in Example 1 except that the first solution and the second solution were stirred for 2 hours instead of 1 hour.
Example 3
Rod type zinc oxide was prepared in the same manner as in Example 1, except that the first solution and the second solution were stirred for 3 hours instead of 1 hour.
Example 4
Rod type zinc oxide was prepared in the same manner as in Example 1 except that 0.02M hexamethylenetetramine (HMT) was added to 100 ml of water instead of 0.01M.
Example 5
A rod-shaped zinc oxide was prepared in the same manner as in Example 1 except that 0.03M hexamethylenetetramine (HMT) was added to 100 ml of water instead of 0.01M.
Comparative Example One
Rod type zinc oxide was prepared in the same manner as in Example 1 except that the first solution and the second solution were stirred for 30 minutes instead of 1 hour.
Comparative Example 2
Rod type zinc oxide was prepared in the same manner as in Example 1, except that the first solution and the second solution were stirred for 4 hours instead of 1 hour.
Comparative Example 3
Rod type zinc oxide was prepared in the same manner as in Example 1 except that 0.04M hexamethylenetetramine (HMT) was added to 100 ml of water instead of 0.01M.
( Flower type Preparation of zinc oxide)
Example 6
0.01 M of Zn (CH 3 COO) 2 .2H 2 O was added to 100 ml of ammonia water (water: ammonia = 9: 1 (v / v)) and stirred for 10 minutes to prepare a third solution.
The third solution was stirred at 90 DEG C and 300 rpm for 1 hour to obtain a solution, which was then filtered and washed with distilled water.
Thereafter, it was dried at 40 DEG C for one day (24 hours) to produce flower-shaped zinc oxide.
Example 7
The flower-shaped zinc oxide was prepared in the same manner as in Example 1, except that the third solution was stirred for 2 hours instead of 1 hour.
Example 8
The rod-shaped zinc oxide was prepared in the same manner as in Example 1 except that the third solution was stirred for 3 hours instead of 1 hour.
Comparative Example 4
The flower-shaped zinc oxide was prepared in the same manner as in Example 1, except that the third solution was stirred for 30 minutes instead of 1 hour.
Comparative Example 5
The flower-shaped zinc oxide was prepared in the same manner as in Example 1 except that the third solution was stirred for 4 hours instead of 1 hour.
Rating 1: SEM Picture
From Figs. 3 to 5, it can be seen that various types of rod-shaped zinc oxide can be produced by controlling the agitation time. In the case of FIG. 1, in the case of stirring for 1 hour, the nucleation reaction is dominant over the nucleation reaction. In the case of FIG. 2 and FIG. 3 where the stirring time is increased to 2 hours and 3 hours, It can be seen that it is becoming more and more dominant. That is, it can be seen that various types of rod-shaped zinc oxide such as a thin and elongated rod-shaped zinc oxide or an umbrella-shaped rod-shaped zinc oxide can be produced only by controlling the agitation time.
From FIGS. 3, 6, and 7, it can be seen that various types of rod-shaped zinc oxide can be produced through the control of the concentration of the reducing agent. In the case of using a 0.01 M reducing agent (hexamethylenetetramine), the nucleation reaction is dominant over the nucleation reaction in FIG. 1, but in FIG. 4 where the concentration of the reducing agent is doubled, In the case of Fig. 5 where 0.03M of reducing agent is used, as the nucleation reaction becomes more dominant, a very thick rod-type zinc oxide Can be produced.
From Figs. 8 to 10, it can be seen that flower type zinc oxide other than the rod type is produced without using the kind of the precursor (zinc salt) and the reducing agent. Further, it is also seen that when the agitation time is gradually increased, the porous flower-shaped zinc oxide is produced as the nucleation reaction becomes more prevalent.
On the other hand, in the case of FIG. 11 in which the agitation was performed for 30 minutes, it can be seen that the rod shape and the aspect ratio are not constant and the formation of the rod-shaped zinc oxide is less. Also, in the case of FIG. 12 in which the agitation is performed for 4 hours, it can be seen that the rod-shaped zinc oxide is entangled with each other, and characteristic features such as sea urchins disappear.
In the case of Fig. 13 where 0.04M of reducing agent is used, it can be seen that the size and the thickness of the rod-shaped zinc oxide are increased but the morphology is not changed.
In the case of Fig. 14, which was stirred for 30 minutes, it was found that the flower-shaped zinc oxide was less formed except for the middle portion. In addition, in the case of FIG. 15 in which stirring is performed for 4 hours, it can be seen that no change occurs in the morphology.
Evaluation 2: TEM Picture
16 to 23, it can be confirmed that the same elapsed time as in the
Rating 3: EDAX analysis
24 to 28, it can be confirmed that the zinc oxide produced by the production method according to the present invention does not contain any impurities.
Rating 4: XRD analysis
It can be seen from FIGS. 29 and 30 that as the agitation time is increased or the concentration of the reducing agent is increased, the nucleation reaction becomes more dominant than the nucleation reaction.
It can be seen from Fig. 31 that x-axis and z-axis growth is more prominent than the y-axis, and the shape of zinc oxide is flower-shaped.
Rating 5: pH analysis
The pH of the thickener according to Examples 1 to 8 was measured several times using a pH meter, and the results are shown in Table 1 below. In the case of Examples 1 to 5, weak acids are shown, while in Examples 6 to 8, weak alkalinity is shown.
It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the present invention as defined by the following claims. As will be understood by those skilled in the art. It is therefore to be understood that the above-described embodiments are illustrative in all aspects and not restrictive.
Claims (15)
Preparing a second solution comprising a reducing agent having a molar concentration of 0.01M to 0.03M;
Stirring the first solution and the second solution to obtain an agitating liquid having a pH of 6 to 7;
Filtering the mixture; And
Washing and drying after the filtering
Gt; wherein < / RTI >
Wherein the zinc salt is Zn (NO 3 ) 2 .6H 2 O, Zn (CH 3 COO) 2 .2H 2 O, ZnCl 2 , or ZnSO 4 .7H 2 O.
The reducing agent is selected from the group consisting of hexamethylenetetramine, substituted or unsubstituted C1 to C20 alkylamine, substituted or unsubstituted C1 to C20 alkylenediamine, substituted or unsubstituted C1 to C20 alkylenetriamine, substituted or unsubstituted C1 To C20 alkylene tetramine, or NaOH.
Wherein the first solution and the second solution comprise water as a solvent.
Wherein the stirring is performed for 1 hour to 3 hours.
Wherein the stirring is performed at a temperature of 70 ° C or more and less than 100 ° C.
Wherein the drying is performed at a temperature of 20 캜 to 60 캜 for 24 hours.
Stirring the third solution for 1 hour to 3 hours to obtain an agitating liquid having a pH of 8 to 10;
Filtering the mixture; And
Washing and drying after the filtering
Lt; / RTI >
Wherein the third solution contains ammonia water as a solvent,
Wherein the ammonia water comprises water and ammonia in a volume ratio of 6: 4 to 9.5: 0.5.
Wherein the zinc salt is Zn (NO 3 ) 2 .6H 2 O, Zn (CH 3 COO) 2 .2H 2 O, ZnCl 2 , or ZnSO 4 .7H 2 O.
Wherein the stirring is performed at a temperature of 70 ° C or more and less than 100 ° C.
Wherein the drying is carried out at a temperature of 20 캜 to 60 캜 for 24 hours.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20170099797A (en) * | 2016-02-24 | 2017-09-01 | 경희대학교 산학협력단 | A Method for preparing metal oxide nanoparticle and metal hydroxide nanoparticle in aqueous solution |
| KR101842751B1 (en) * | 2015-12-07 | 2018-03-28 | 경희대학교 산학협력단 | method for preparing zinc oxide nanoparticle, and zinc oxide nanoparticle prepared by the same |
| KR102272709B1 (en) * | 2020-03-27 | 2021-07-02 | 한국화학연구원 | Synthesis device for multiple reaction modules of ZnO nonowires |
-
2014
- 2014-04-29 KR KR1020140051923A patent/KR101564005B1/en active IP Right Grant
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101842751B1 (en) * | 2015-12-07 | 2018-03-28 | 경희대학교 산학협력단 | method for preparing zinc oxide nanoparticle, and zinc oxide nanoparticle prepared by the same |
| KR20170099797A (en) * | 2016-02-24 | 2017-09-01 | 경희대학교 산학협력단 | A Method for preparing metal oxide nanoparticle and metal hydroxide nanoparticle in aqueous solution |
| KR101946145B1 (en) | 2016-02-24 | 2019-02-11 | 경희대학교 산학협력단 | A Method for preparing metal oxide nanoparticle and metal hydroxide nanoparticle in aqueous solution |
| KR102272709B1 (en) * | 2020-03-27 | 2021-07-02 | 한국화학연구원 | Synthesis device for multiple reaction modules of ZnO nonowires |
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