KR20100106680A - Method of manufacturing zinc-oxde thin film and zinc-oxide based light emitting device - Google Patents
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Abstract
Description
The present invention relates to a zinc oxide (ZnO) thin film and a zinc oxide based light emitting device, and more particularly, to a method for manufacturing a zinc oxide thin film and a zinc oxide based light emitting device using a surfactant.
Bulbs and fluorescent lights used for indoor and outdoor lighting consume a lot of power, and fluorescent lamps cause serious environmental problems due to mercury.
In order to solve these problems, lighting apparatuses using light emitting diodes (LEDs) have been developed. Currently, mass-produced light emitting diodes are based on gallium nitride (GaN).
However, gallium nitride (GaN) -based light emitting diodes have their source material and technology monopolized by several top companies, including Nichia. Therefore, domestic and foreign companies and research institutes are concentrating their research capabilities on developing light emitting diodes other than gallium nitride based light emitting diodes.
Most attention as a next generation light emitting diode to replace gallium nitride (GaN) is a light emitting diode based on zinc oxide (ZnO).
Zinc oxide is a group II-VI compound semiconductor of Wurzite (Hexagonal) structure having a band gap of about 3.37 eV at room temperature, and can be manufactured by various methods such as MBE, CVD, PLD, sputtering, and organometallic chemical vapor deposition.
Zinc oxide (ZnO) has an exciton binding energy of 60 meV compared to gallium nitride (GaN), which is much higher than the gallium nitride exciton binding energy of 21-25 meV, and can form zinc oxide film on the same substrate. Wet etching is possible.
On the other hand, when manufacturing a zinc oxide thin film layer by using an organometallic chemical vapor deposition (MOCVD) method, the growth in the c-axis direction is thermodynamically stable, the relatively lateral growth is difficult.
Various methods have been proposed to solve this problem.
B.P. Zhang and four others attempted to obtain a zinc oxide thin film layer under various conditions of growth temperature to form a zinc oxide thin film layer on a sapphire substrate [Thin solid films, 449, 12 (2004)]. However, as can be seen from the above document, the growth of the thin film layer is made under low temperature, which has a disadvantage in that crystallinity is poor and control of growth variables is difficult.
In addition, techniques using the characteristics of the substrate have been tried to obtain a zinc oxide thin film.
C.Neuman and seven others obtained a zinc oxide thin film through a crystal layer in which zinc was transported by argon and flowed through nitrogen oxide gas on a single crystal zinc oxide bulk substrate. However, this uses a simple chemical vapor deposition method.
The above thin film manufacturing method is a method for obtaining a single layer of zinc oxide on a substrate and has a disadvantage in that it is difficult to use in a structure such as a light emitting diode or a light emitting laser having a high quality multilayer structure.
SUMMARY OF THE INVENTION An object of the present invention is to provide a method for preparing a zinc oxide thin film layer in which a surfactant is introduced into a reactor so that the growth of the zinc oxide thin film layer using an organometallic chemical vapor deposition method may occur well in a horizontal direction.
Another object of the present invention is to provide a method for manufacturing a zinc oxide based light emitting device in which a surfactant is introduced into a reactor in the formation of each thin film layer when fabricating a light emitting device having a multilayer structure using an organometallic chemical vapor deposition method.
Method of manufacturing a zinc oxide thin film according to an embodiment of the present invention for achieving the above object comprises providing a substrate, forming a zinc oxide thin film layer on the substrate, the formation of the zinc oxide thin film layer is It is characterized by achieving by introducing a surfactant on the substrate.
In addition, the method of manufacturing a zinc oxide based light emitting device according to another embodiment of the present invention comprises the steps of providing a substrate, forming an n-type zinc oxide thin film layer on the substrate, forming an active layer on the n-type zinc oxide thin film layer And forming a p-type zinc oxide thin film layer on the active layer, wherein at least one of the n-type zinc oxide thin film layer, the zinc oxide active layer, and the p-type zinc oxide thin film layer is achieved by introducing a surfactant. It features.
Specific details of other embodiments are included in the detailed description and the drawings.
According to the zinc oxide thin film and the zinc oxide based light emitting device manufacturing method of the present invention as described above has the following effects.
First, the horizontal growth of the zinc oxide thin film can be achieved by introducing a surfactant such as cadmium in the reaction process during the organic metal chemical vapor deposition (MOCVD) of zinc oxide.
Second, when manufacturing a zinc oxide based light emitting device by using a surfactant, it is possible to manufacture a light emitting device having excellent light emission characteristics by reducing the defect concentration such as vacancy or interstitial atoms in the thin film. .
The effects of the present invention are not limited to the above-mentioned effects, and other effects not mentioned will be clearly understood by those skilled in the art from the description of the claims.
Advantages and features of the present invention and methods for achieving them will be apparent with reference to the embodiments described below in detail with the accompanying drawings. However, the present invention is not limited to the embodiments disclosed below, but may be embodied in various different forms, and the present embodiments merely make the disclosure of the present invention complete, and are common in the art to which the present invention pertains. It is provided to fully inform those skilled in the art of the scope of the invention, which is to be defined only by the scope of the claims. Like reference numerals refer to like elements throughout.
Hereinafter, a method of manufacturing a zinc oxide thin film and a zinc oxide based light emitting device according to a preferred embodiment of the present invention will be described in detail with reference to the accompanying drawings. In the following description, well-known functions or constructions are not described in detail to avoid unnecessarily obscuring the subject matter of the present invention.
1 is a view showing a zinc oxide thin film layer formed on a substrate according to an embodiment of the present invention.
As shown in FIG. 1, a method of manufacturing a zinc oxide thin film according to an embodiment of the present invention includes providing a substrate, and subsequently forming a zinc oxide thin film layer on the substrate, wherein the formation of the zinc oxide thin film layer is performed on a substrate. It can be achieved by introducing a surfactant into the phase.
In the present invention, the
The zinc oxide thin film layer 5 is formed on the
The material constituting the zinc oxide thin film layer 5 may be zinc oxide (ZnO) or zinc oxide (ZnO) to which at least one of magnesium (Mg) and beryllium (Be) is added.
When the zinc oxide thin film layer 5 is an n-type zinc oxide semiconductor, the dopant used in depositing the zinc oxide thin film may be aluminum (Al), gallium (Ga), or indium (In).
However, the dopant material is not limited to the above, and any material capable of forming a donor level may be used.
When the zinc oxide thin film layer 5 is made of p-type zinc oxide, the dopant used for depositing the zinc oxide thin film is phosphorus (P), lithium (Li), sodium (Na), potassium (K), cesium (Cs). ), Antimony (Sb), nitrogen (N) or lead (Pb).
However, the dopant material is not limited to the above, and any material capable of forming an acceptor level may be used.
The method of forming the zinc oxide thin film layer 5 may be at least one selected from a sputtering method, an ion plating method, an electron gun (e-gun), and an organic chemical vapor deposition method (MOCVD) method. .
The step of forming the zinc oxide thin film layer 5 may be performed using a surfactant, in which case the surfactant is one selected from cadmium (Cd), sodium (Na), sulfur (S) and phosphorus (P). It can be abnormal.
In this case, the surfactant may be injected only during a part of the initial reaction or may be injected periodically. In addition, the thin film may be implanted during or before growth.
2 is a graph showing vapor pressure characteristics according to temperatures of cadmium (Cd), zinc (Zn), indium (In), and gallium (Ga).
As shown in FIG. 2, cadmium (Cd) is a substance present in the form of an oxide at room temperature and atmospheric pressure, and it can be seen that vapor pressure is higher than zinc (Zn) under the same temperature.
In addition, it can be seen that at the same pressure state can exist in the vapor state even at low temperatures. In other words, it can be seen that cadmium may be present in more vapor form than zinc at the same temperature during organometallic chemical vapor deposition.
3 is a view showing the principle that cadmium (Cd) acts as a surfactant when forming a zinc oxide thin film layer according to an embodiment of the present invention.
As shown in FIG. 2, cadmium, which is present in more vapor form than zinc at the same temperature, binds to dangling bonds present on the zinc oxide surface during deposition, as illustrated in FIG. 3. The migration of deposition atoms in the lateral direction can be facilitated.
As shown in FIG. 3, dangling bonds of the thin film, zinc oxide crystals, and cadmium are combined. Cadmium sites, which held the dangling bonds in the initial state, are difficult to bond with zinc, so that the next thin film layer occupies positions other than the cadmium sites.
In this way, cadmium having a high vapor pressure at the same temperature tends to be in a vapor state, and when vaporized, zinc, oxygen, or the like can bind to the site again, and thus cadmium can act as a surfactant. That is, when cadmium is introduced for the first time, cadmium binds to a dangling bond by a predetermined amount, but as time increases, the dangling bond is bound to zinc oxide due to a higher vapor pressure than zinc oxide, and has a characteristic of vaporizing.
Therefore, it is possible to induce horizontal growth of zinc oxide during initial crystal formation or thin film formation, and to prevent distorted growth in the vertical direction.
4 is a view showing a laminated structure of a zinc oxide based light emitting device manufactured in another embodiment of the present invention.
The method for manufacturing a zinc oxide based light emitting device as shown in FIG. 4 includes providing a substrate, followed by forming an n-type zinc oxide thin film layer on the substrate, followed by a zinc oxide active layer having a multi-quantum well structure on the n-type thin film layer. Forming a p-type zinc oxide thin film layer on the zinc oxide active layer, wherein at least one of the n-type zinc oxide thin film layer, the zinc oxide active layer, and the p-type zinc oxide active layer is introduced by a surfactant. Can be formed.
As shown in FIG. 4, in order to apply external power to the top surface of the n-type zinc oxide thin film layer 20 and the top of the p-type zinc oxide
At least one of the n-type zinc oxide thin film layer 20, the active layer 30, the p-type zinc oxide
In this case, the surfactant may be injected only during a part of the initial reaction or may be injected periodically. In addition, the thin film may be implanted during or before growth.
In the present invention, the
The n-type zinc oxide thin film layer 20 is deposited on the
In addition, the dopant used in the n-type zinc oxide thin film layer 20 may be aluminum (Al), gallium (Ga), or indium (In).
The step of forming the n-type zinc oxide thin film layer 20 may be performed using a surfactant, in which case the surfactant is at least one selected from cadmium (Cd), sodium (Na), sulfur (S) and phosphorus (P). This can be However, the present invention is not limited thereto, and any material having a higher vapor pressure than zinc may be used.
FIG. 5 illustrates a zinc oxide active layer having a multiple quantum well structure.
The zinc oxide
In this case, the material used for the barrier layer is Mg x Zn 1 - x O ( 0≤x≤1), Be x Zn 1 - x O (0≤x≤1), Be x Mg y Zn 1 -x- y O (0 ≦ x, y ≦ 1, 0 ≦ x + y ≦ 1).
In addition, the material used for the well layer is Mg x Zn 1 - x O (0≤x≤1), Be x Zn 1 - x O (0≤x≤1), Be x Mg y Zn 1-xy O (0 It may be one or more materials selected from ≤ x,
In this case, when the materials used for the barrier layer and the well layer are the same, the larger the x or y is used, the band gap is increased and used as the material of the barrier layer.
In order to manufacture the two-dimensional quantum structure, the lateral growth must be well made and the crystallinity must be secured. When cadmium is used as a surfactant, the lateral growth is well achieved, so that a zinc oxide active layer having a high quality multi-quantum well structure is formed. Can be formed.
The p-type zinc oxide
In addition, dopants used in the p-type zinc oxide
The method of manufacturing a zinc oxide based light emitting device according to the present invention may include forming a buffer layer (not shown) between providing a substrate and forming an n-type zinc oxide thin film layer.
The buffer layer (not shown) is an element layer for alleviating stress caused by lattice constant mismatch between the
In the formation of the buffer layer (not shown), at least one selected from cadmium (Cd), sodium (Na), sulfur (S), and phosphorus (P) may be introduced into the surfactant. For example, when the buffer layer is formed, a surfactant is introduced on the surface of the
The material used for the buffer layer may be at least one selected from zinc oxide (ZnO), magnesium oxide (MgO), cadmium oxide (CdO), MgZnO, and CdZnO. However, it is not limited thereto.
Hereinafter, a preparation example of a zinc oxide thin film and a multi-quantum well structured zinc oxide active layer using cadmium as a surfactant will be provided to help understanding of the present invention. However, the following experimental examples are only for helping understanding of the present invention, and the present invention is not limited to the following experimental examples.
Example 1 Method of Forming Undoped Zinc Oxide Thin Film Layer
Using organometallic chemical vapor deposition (MOCVD), the pressure range in the reactor for the growth of undoped zinc oxide thin films can be from 10 -2 torr to atmospheric pressure. In Example 1, the pressure was maintained at 50 torr.
The temperature in the reactor is preferably maintained at least 400 ° C.
In the undoped zinc oxide thin film growth, DEZn was used as the source of zinc, DMCd was used as the source of cadmium, and O 2 gas was used as the source of oxygen. The temperature in the reactor was raised to a thin film growth temperature (800 ° C.), followed by injection of oxygen, DEZn, and DMCd.
Each source was injected at a flow rate of 13.4 μmol / min for DEZn, 727 nmol / min for DMCd, and 0.335 mol / min for O 2 . At this time, the thin film growth temperature was grown at least 400 ℃ to allow the cadmium (Cd) to evaporate during the thin film growth.
Since the actual chemical reaction in the reactor is a reaction between DEZn and O 2, the reaction formula is shown below.
[Scheme]
DEZn (C 4 H 10 Zn) + 7O 2 → 4CO 2 + ZnO + 5H 2 O
Cadmium is connected to dangling bonds during the growth of zinc oxide thin films, and when zinc (Zn) arrives, cadmium is released and evaporates. As the zinc oxide thin film grows as described above, as the cadmium is continuously injected, the zinc oxide thin film which is not escaped is grown.
<Example 2: n-type zinc oxide thin film layer forming method>
Using organometallic chemical vapor deposition (MOCVD), the pressure range in the reactor for the growth of n-type zinc oxide thin film can be from 10 -2 torr to atmospheric pressure. In Example 2, the pressure was maintained at 50 torr.
The temperature in the reactor is preferably maintained at least 400 ° C.
When growing n-type zinc oxide thin film, DEZn is used as the source of zinc, DMCd is used as the source of cadmium, DEGa is used as the source of gallium (Ga) as the n-type dopant, and O is used as the source of oxygen. 2 gases were used.
The temperature in the reactor was raised to the thin film growth temperature (800 ° C.), and oxygen, DEZn, DMCd, and DEGa were injected.
Each source was injected at a flow rate of 13.4 μmol / min for DEZn, 727 nmol / min for DMCd, 2.55 nmol / min for DEGa, and 0.335 mol / min for O 2 . At this time, the thin film growth temperature was grown at least 400 ℃ to allow the cadmium (Cd) to evaporate during the thin film growth.
Since the actual chemical reaction in the reactor is a reaction between DEZn and O 2, the reaction formula is shown below.
[Scheme]
DEZn (C 4 H 10 Zn) + 7O 2 → 4CO 2 + ZnO + 5H 2 O
In this case, as gallium (Ga) is injected into the dopant source, gallium (Ga) is substituted in the place of zinc (Zn), and as the donor level is formed, the n-type electrical characteristics are exhibited. Cadmium (Cd) is connected to dangling bonds during the growth of the zinc oxide thin film, and when zinc (Zn) arrives, it acts as a place and evaporates.
As described above, as the cadmium was continuously injected during the growth of the zinc oxide thin film, the n-type zinc oxide thin film was grown.
Example 3: p-type zinc oxide thin film layer formation method
Using the organometallic chemical vapor deposition (MOCVD) method, the pressure range in the reactor for p-type zinc oxide thin film growth can be from 10 -2 torr to atmospheric pressure. In Example 3, the pressure was maintained at 50 torr.
The temperature in the reactor is preferably maintained at least 400 ° C.
During the growth of p-type zinc oxide thin films, DEZn is the source of zinc, DMCd is the source of cadmium, TMSb is the source of antimony (Sb) as the p-type dopant, and O 2 is the source of oxygen. Gas was used.
After raising the temperature in the reactor to the film growth temperature (800 ° C.), oxygen, DEZn, DMCd, and TMSb were injected. Each source was injected at a flow rate of 20.1 μmol / min for DEZn, 727 nmol / min for DMCd, 722 nmol / min for TMSb, and 0.335 mol / min for O2.
At this time, the thin film was grown at least 400 ℃ to allow the cadmium to evaporate during thin film growth.
Since the actual chemical reaction in the reactor is a reaction between DEZn and O 2, the reaction formula is shown below.
[Scheme]
DEZn (C 4 H 10 Zn) + 7O 2 → 4CO 2 + ZnO + 5H 2 O
In this case, as antimony (Sb) is injected into the dopant source, antimony is substituted in the zinc sites and p-type electrical characteristics are formed by forming an acceptor level.
Cadmium is connected to dangling bonds during zinc oxide thin film growth, and when zinc reaches, it leaves its place and evaporates.
As described above, as the cadmium was continuously injected during the growth of the zinc oxide thin film, the p-type zinc oxide thin film was grown.
Example 4 Formation of Zinc Oxide Active Layer of Multi Quantum Well Structure
Using organometallic chemical vapor deposition (MOCVD), the pressure range in the reactor can be from 10 -2 torr to atmospheric pressure during the growth of a multi-quantum well structured zinc oxide active layer. In Example 4, the pressure was maintained at 50 torr.
The temperature in the reactor is preferably maintained at least 400 ° C.
In order to form a multiple quantum well structure, a barrier layer made of a material having a large band gap and a well layer made of a material having a small band gap should be periodically deposited.
Material of the barrier layer was composed of Mg x Be y Zn 1 -x- y O (0≤x, y≤1, 0≤x + y≤1). In order to improve the quality of a thin film when forming a barrier layer, a material having a large band gap among multiple quantum well structures, a cadmium source was simultaneously injected during thin film growth.
At this time, the barrier layer thin film was grown at least 400 ℃ to allow the cadmium to evaporate during the thin film growth.
Since the actual chemical reaction in the reactor is a reaction between DEZn and O 2, the reaction formula is shown below.
[Scheme]
DEZn (C 4 H 10 Zn) + 7O 2 → 4CO 2 + ZnO + 5H 2 O
At this time, the band gap increases as magnesium (Mg) or beryllium (Be) is substituted for zinc. Cadmium is connected to dangling bonds during the growth of the barrier layer thin film, which leaves its place and evaporates when zinc arrives.
The well material was Mg x Be y Zn 1 -x- y O (0≤x, y≤1, 0≤x + y≤1) as the material of the barrier layer. The cadmium source was injected at the same time as.
As described above, when the barrier layer or the well layer thin film was grown, cadmium was continuously injected to grow a zinc oxide active layer having a multi-quantum well structure.
The above embodiment describes the best possible case, and unlike the above, it may be applied to the case where the injection is performed only during the first part or periodically. In addition, it can be applied both when the thin film is grown or injected before growth.
6A and 6B are scanning electron microscopy (magnification) photographs showing enlarged thin films formed when no surfactant is used and when cadmium (Cd) is used as a surfactant.
As shown in FIGS. 6A and 6B, when a zinc oxide thin film layer was formed using cadmium as a surfactant, defects caused by pores or invasive atoms rarely occurred in the thin film layer, and thus the surface state was remarkably improved.
FIG. 7 is a graph showing experimental results of evaluating PL (Photo-Luminescence) characteristics in order to investigate the crystallinity of a zinc oxide thin film using cadmium as a surfactant.
As shown in FIG. 7, the zinc oxide thin film manufactured by using cadmium as a surfactant has a stronger intensity of band edge peak (near 380 nm) and thin film defects than the zinc oxide thin film prepared without the addition of cadmium. It can be seen that the intensity of the peak (near 500 to 650 nm) due to the related deep level is also reduced.
This is because the zinc oxide thin film layer manufactured using cadmium as a surfactant has a significant decrease in defect concentration due to voids or invasive atoms in the thin film, thereby improving optical characteristics.
The zinc oxide based light emitting device according to the present invention is applicable to the entire industry in which a light emitting diode is currently used and can replace a light emitting device based on gallium nitride (GaN).
Although embodiments of the present invention have been described above with reference to the accompanying drawings, those skilled in the art to which the present invention pertains may implement the present invention in other specific forms without changing the technical spirit or essential features thereof. I can understand that.
It is therefore to be understood that the above-described embodiments are illustrative in all aspects and not restrictive. The scope of the present invention is shown by the following claims rather than the detailed description, and all changes or modifications derived from the meaning and scope of the claims and their equivalents should be construed as being included in the scope of the present invention. .
1 is a view showing a zinc oxide thin film layer formed on a substrate according to an embodiment of the present invention.
2 is a graph showing the relationship between temperature and vapor pressure of cadmium (Cd), zinc (Zn), indium (In), and gallium (Ga).
3 is a view showing the principle that cadmium (Cd) acts as a surfactant when forming a zinc oxide thin film according to an embodiment of the present invention.
4 is a diagram illustrating a laminated structure of a zinc oxide based light emitting device according to an embodiment of the present invention.
5 is a diagram illustrating a zinc oxide active layer of a multi-quantum well structure according to an embodiment of the present invention.
6A and 6B are scanning electron microscopy (magnification) photographs showing enlarged thin films formed when and without cadmium as a surfactant.
7 is a graph showing light emission characteristics of a zinc oxide thin film when cadmium is used as a surfactant and when it is not used.
<Description of Symbols for Main Parts of Drawings>
3,10,70: Substrate 5: Zinc oxide thin film layer
20,80: n-type zinc oxide thin film layer 30, 90: active layer
40: p-type zinc oxide thin film layer 50: n-type metal electrode
60: p-type metal electrode
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101064517B1 (en) * | 2010-11-22 | 2011-09-15 | 한국과학기술연구원 | Method for growth of zinc oxide thin films and thin film solar cell using the same |
| US9305778B2 (en) | 2012-11-16 | 2016-04-05 | Samsung Electronics Co., Ltd. | Controlled manufacturing method of metal oxide semiconductor and metal oxide semiconductor structure having controlled growth crystallographic plane |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP4284103B2 (en) | 2003-05-08 | 2009-06-24 | シャープ株式会社 | Oxide semiconductor light emitting device |
| JP5096844B2 (en) * | 2007-08-30 | 2012-12-12 | スタンレー電気株式会社 | Method for producing ZnO-based compound semiconductor layer |
| JP5399640B2 (en) | 2008-03-06 | 2014-01-29 | スタンレー電気株式会社 | Manufacturing method of ZnO-based semiconductor device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101064517B1 (en) * | 2010-11-22 | 2011-09-15 | 한국과학기술연구원 | Method for growth of zinc oxide thin films and thin film solar cell using the same |
| US9305778B2 (en) | 2012-11-16 | 2016-04-05 | Samsung Electronics Co., Ltd. | Controlled manufacturing method of metal oxide semiconductor and metal oxide semiconductor structure having controlled growth crystallographic plane |
| US9748095B2 (en) | 2012-11-16 | 2017-08-29 | Samsung Electronics Co., Ltd. | Controlled manufacturing method of metal oxide semiconductor and metal oxide semiconductor structure having controlled growth crystallographic plane |
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