CN111146318A - Based on MoS2Thin layer ultraviolet light-emitting diode and manufacturing method thereof - Google Patents
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- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 229910002704 AlGaN Inorganic materials 0.000 claims abstract description 120
- 239000000758 substrate Substances 0.000 claims abstract description 64
- 238000000034 method Methods 0.000 claims abstract description 48
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 30
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims description 52
- 230000008569 process Effects 0.000 claims description 38
- 229910052782 aluminium Inorganic materials 0.000 claims description 25
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 25
- 230000001965 increasing effect Effects 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 10
- 239000000919 ceramic Substances 0.000 claims description 9
- 238000005229 chemical vapour deposition Methods 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 238000001020 plasma etching Methods 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
- 238000005530 etching Methods 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 6
- 229910021389 graphene Inorganic materials 0.000 claims description 6
- 238000001259 photo etching Methods 0.000 claims description 6
- 238000007747 plating Methods 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 230000008878 coupling Effects 0.000 claims description 4
- 238000010168 coupling process Methods 0.000 claims description 4
- 238000005859 coupling reaction Methods 0.000 claims description 4
- 230000001939 inductive effect Effects 0.000 claims description 4
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- 239000013078 crystal Substances 0.000 abstract description 4
- 238000000407 epitaxy Methods 0.000 abstract description 4
- 238000001534 heteroepitaxy Methods 0.000 abstract description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 abstract description 2
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- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 8
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Abstract
The invention provides a method based on MoS2The thin layer ultraviolet light-emitting diode based on MoS and the preparation method thereof2The thin-layer ultraviolet light-emitting diode comprises a substrate and a MoS which are arranged from bottom to top in sequence2The solar cell comprises a layer, an n-type gradient Al component AlGaN layer, an AlGaN quantum well layer, a p-type gradient Al component AlGaN layer and a p electrode, wherein the n electrode is arranged on the upper side of the n-type gradient Al component AlGaN layer, and the MoS is arranged on the upper side of the N-type gradient Al component AlGaN layer2The layers are multi-layer tiled MoS2Material. The invention is in MoS2The upper heteroepitaxy surface has no dangling bond, and the crystal quality is high. The epitaxial mode of the invention is Van der Waals epitaxy, and the epitaxial growth can be realized on various substrates. The thin-layer ultraviolet light-emitting diode based on MoS2 is small in overall thickness and wide in application field.
Description
Technical Field
The invention relates to an ultraviolet light emitting diode, in particular to a light emitting diode based on MoS2The thin layer ultraviolet light emitting diode and the manufacturing method thereof.
Background
In the prior art, Al is doped in GaN to form an AlGaN ternary material, and the forbidden bandwidth of AlGaN can be continuously changed within the range of 3.4 eV-6.2 eV by changing the Al component in a quantum well, so that the working wavelength of the AlGaN ultraviolet light-emitting diode can be changed from 365nm to 200 nm. However, as the Al composition of the AlGaN material increases, the difficulty of material epitaxy also increases, and the AlN single crystal substrate lattice-matched with the high Al composition is prohibitively expensive. In order to solve this problem, it is common practice to grow a very thick AlN buffer layer by a two-step growth method before growing the light-emitting multiple quantum well, and then to grow n-AlGaN, but n-AlGaN grown in this way has a very large number of threading dislocations and the quality of n-AlGaN in the deep ultraviolet band is poor. In addition, in order to isolate the influence of the lower layer threading dislocation relative to the light-emitting quantum well, the n-AlGaN layer is generally grown to be thicker, which also limits the development of the GaN-based deep ultraviolet LED on flexible substrates and biological substrates.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method based on MoS2The thin-layer ultraviolet light-emitting diode and the manufacturing method thereof can reduce the epitaxial growth cost and the dependence on the lattice matching substrate.
To solve the above technical problem, embodiments of the present invention provide a MoS-based device2The thin-layer ultraviolet light-emitting diode comprises a substrate and a MoS which are arranged from bottom to top in sequence2The solar cell comprises a layer, an n-type gradient Al component AlGaN layer, an AlGaN quantum well layer, a p-type gradient Al component AlGaN layer and a p electrode, wherein the n electrode is arranged on the upper side of the n-type gradient Al component AlGaN layer, and the MoS is arranged on the upper side of the N-type gradient Al component AlGaN layer2MoS with layers tiled by multiple layers2The material is formed.
Wherein the MoS2The thickness of the layer is 2-5 nm.
Wherein the n-type graded Al componentThe thickness of the AlGaN layer is 100-120nm, the Al component in the n-type gradient Al component AlGaN layer is linearly and gradually increased, and the Si doping concentration is 5' 1018cm-3。
Wherein the AlGaN quantum well layer has a thickness of 40-60 nm;
the thickness of the p-type gradient Al component AlGaN layer is 100-120nm, the Al component in the p-type gradient Al component AlGaN layer is linearly and gradually increased and gradually changed, and the Mg doping concentration is 1' 1019cm-3。
The invention also provides a method based on MoS2The preparation method of the thin-layer ultraviolet light-emitting diode comprises the following steps:
(1) MoS with the thickness of 2-5nm is grown on a substrate by using a CVD process2A layer;
(2) MoS on blanket substrate2On the layer, an n-type gradient Al component AlGaN layer with the thickness of 100-120nm is grown by utilizing an MOCVD process in a mode of linearly increasing the flow of an Al source, and the Si doping concentration of the n-type gradient Al component AlGaN layer is 5' 1018cm-3；
(3) Growing an AlGaN quantum well layer with the thickness of 40-60nm on the AlGaN layer with the n-type gradually-changed Al component by utilizing an MOCVD (metal organic chemical vapor deposition) process;
(4) growing a p-type gradient Al component AlGaN layer with the thickness of 100-120nm on the AlGaN quantum well layer by utilizing an MOCVD process in a way of linearly reducing the flow of an Al source, wherein the Mg doping concentration is 1' 1019cm-3；
(5) Etching from the top p-type gradient Al component AlGaN layer to the n-type gradient Al component AlGaN layer by adopting inductive coupling plasma or reactive ion etching to form an n-type AlGaN table top;
(6) photoetching a pattern of an n-type electrode on an n-type A1GaN table board, and evaporating the n-type electrode by using a film plating machine;
(7) photoetching a P-type electrode pattern on the P-type gradient Al component AlGaN layer, evaporating the P-type electrode by using a film plating machine, and completing MoS-based2And (3) manufacturing the thin-layer ultraviolet light-emitting diode.
Wherein MoS is grown in the step (1)2The process conditions of the layers are: the temperature of the reaction chamber is 650-850 ℃, and the pressure of the reaction chamber is keptIntroducing nitrogen gas with the flow rate of 250-300sccm into the reaction chamber with the force of 20-75Torr, coating a drop of reduced graphene oxide solution on the substrate surface of the substrate before growth, drying at 50 deg.C, and removing MO3The powder was placed in a CVD ceramic boat with the substrate mounted face down on top of the boat, and a separate ceramic boat of sulfur powder was placed in the MO3Beside the powder.
Wherein the process conditions for growing the n-type gradient Al component AlGaN layer in the step (2) are as follows: the temperature of the reaction chamber is 900-1350 ℃, the pressure of the reaction chamber is kept at 10-75Torr, an aluminum source with the flow of 50-200sccm is introduced into the reaction chamber, and the flow of the aluminum source is uniformly increased from 50sccm to 200sccm in the growth process.
The process conditions for growing the AlGaN quantum well layer in the step (3) are as follows: the temperature of the reaction chamber is 900-1350 ℃, the pressure of the reaction chamber is kept at 15-75Torr, and aluminum source with the flow rate of 120-240sccm is introduced into the reaction chamber.
The process conditions for growing the p-type gradient Al component AlGaN layer in the step (4) are as follows: the temperature of the reaction chamber is 900-1350 ℃, the pressure of the reaction chamber is kept at 10-75Torr, an aluminum source with the flow of 50-240sccm is introduced into the reaction chamber, and the flow of the aluminum source is uniformly decreased from 240sccm to 50sccm in the growth process.
The technical scheme of the invention has the following beneficial effects:
1. the invention is in MoS2The upper heteroepitaxy surface has no dangling bond, and the crystal quality is high. The traditional AlGaN-based ultraviolet light-emitting diode is generally grown on a c-plane sapphire substrate, because the sapphire substrate, GaN and AlN have large lattice mismatch and thermal mismatch, and simultaneously because a large number of dangling bonds existing on the surface of the sapphire substrate cause the upward transmission of substrate stress, the upper AlN/AlGaN generates lattice distortion and generates a large number of dislocations, and the crystallization quality of an epitaxial layer is seriously reduced. The method is adopted in MoS2Epitaxy on a layer, MoS2Is a kind of graphite alkene two-dimensional material, compares graphite alkene, and the advantage lies in: MoS2Is a direct band gap semiconductor, single layer MoS2The forbidden band width is 1.8eV, and the method has a bright application prospect in photoelectric devices. Because of the MoS2Is a similar stoneThe graphene material has no dangling bond on the surface, the stress of the substrate cannot be transferred to the upper layer, and Al atoms are in MoS2The AlGaN film with high Al component and good uniformity can be grown with very low surface migration potential barrier.
2. The epitaxial mode of the invention is Van der Waals epitaxy, and the epitaxial growth can be realized on various substrates. In MoS2Overgrowth epitaxial structure, epitaxial layer and MoS2The bonding mode is Van der Waals force, and is not a mode of bonding in a chemical bond mode when a traditional sapphire, SiC or Si substrate is grown. Since there is no direct chemical bond between the epitaxial layer and the substrate, in MoS2The epitaxial growth of AlGaN on the substrate has low requirement, and can realize the epitaxial growth of other single crystal or polycrystalline substrates.
3. The invention is based on MoS2The thin-layer ultraviolet light-emitting diode has small integral thickness and wide application field. The invention adopts the Al component gradient layer as the n-type layer and the p-type layer, and controls the gradient direction of the gradient layer by adjusting the flow of an Al source in the growth process, thereby promoting the recombination of electrons and holes in a quantum well. In the traditional light-emitting diode, an electron blocking layer is needed in a p-type region to inhibit electrons from diffusing to the p-type region beyond a quantum well.
4. Because of the MoS2The thin ultraviolet light-emitting diode has small integral thickness and simple epitaxial structure stripping process, and can be applied to the new fields of biological flexible substrates and the like.
Drawings
FIG. 1 is a MoS-based representation provided by an embodiment of the present invention2The structure of the thin layer ultraviolet light-emitting diode is shown schematically;
FIG. 2 is a triangular MoS based on growth on a sapphire substrate in the present invention2；
FIG. 3 shows a single-layer MoS grown on a sapphire substrate according to the present invention2；
FIG. 4 is a 295nm deep ultraviolet LED temperature varying PL spectrum in the invention.
Description of reference numerals:
1. a substrate; 2. MoS2A layer; 3. an n-type gradient Al component AlGaN layer; 4. an AlGaN quantum well layer; 5. an AlGaN layer of p-type gradient Al composition; 6. an n electrode; 7. and a p-electrode.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
As shown in FIG. 1, the present invention provides a MoS-based solution2The thin-layer ultraviolet light-emitting diode comprises a substrate 1 and a MoS which are arranged from bottom to top in sequence2The solar cell comprises a layer 2, an n-type gradient Al component AlGaN layer 3, an AlGaN quantum well layer 4, a p-type gradient Al component AlGaN layer 5 and a p electrode 7, wherein an n electrode 6 is arranged above the side of the n-type gradient Al component AlGaN layer 3, and the MoS is characterized in that2 Layer 2 is a multi-layer tiled MoS2A material.
Wherein the MoS2The thickness of layer 2 is 2-5 nm. The thickness of the n-type gradient Al component AlGaN layer 3 is 100-120nm, the Al component in the n-type gradient Al component AlGaN layer 3 is linearly and gradually increased, and the Si doping concentration is 5' 1018cm-3。
The AlGaN quantum well layer 4 has a thickness of 40-60 nm. The thickness of the p-type gradient Al component AlGaN layer 5 is 100-120nm, the Al component in the p-type gradient Al component AlGaN layer 5 is linearly and gradually increased, and the Mg doping concentration is 1' 1019cm-3。
The invention also provides a method based on MoS2The preparation method of the thin-layer ultraviolet light-emitting diode comprises the following steps:
(1) MoS with the thickness of 2-5nm is grown on a substrate by using a CVD process2Layer, the process conditions are as follows: the temperature of the reaction chamber is 650-850 ℃, the pressure of the reaction chamber is kept at 20-75Torr, nitrogen with the flow of 250-300sccm is simultaneously introduced into the reaction chamber, a drop of reduced graphene oxide solution is coated on the surface of the substrate before growth, and then drying is carried out at 50 ℃, and MO is obtained3The powder was placed in a CVD ceramic boat with the substrate mounted face down on top of the boat, and a separate ceramic boat of sulfur powder was placed in the MO3Beside the powder.
(2) MoS on blanket substrate2On the layer, an n-type gradient Al component AlGaN layer with the thickness of 100-120nm is grown by utilizing an MOCVD process in a mode of linearly increasing the flow of an Al source, and the Si doping concentration of the n-type gradient Al component AlGaN layer is 5' 1018cm-3；
In this step, the process conditions for growing the n-type gradient Al composition AlGaN layer are as follows: the temperature of the reaction chamber is 900-1350 ℃, the pressure of the reaction chamber is kept at 10-75Torr, an aluminum source with the flow of 50-200sccm is introduced into the reaction chamber, and the flow of the aluminum source is uniformly increased from 50sccm to 200sccm in the growth process.
(3) Growing an AlGaN quantum well layer with the thickness of 40-60nm on the AlGaN layer with the n-type gradually-changed Al component by utilizing an MOCVD (metal organic chemical vapor deposition) process;
the process conditions for growing the AlGaN quantum well layer in the step are as follows: the temperature of the reaction chamber is 900-1350 ℃, the pressure of the reaction chamber is kept at 15-75Torr, and aluminum source with the flow rate of 120-240sccm is introduced into the reaction chamber.
(4) Growing a p-type gradient Al component AlGaN layer with the thickness of 100-120nm on the AlGaN quantum well layer by utilizing an MOCVD process in a way of linearly reducing the flow of an Al source, wherein the Mg doping concentration is 1' 1019cm-3；
The process conditions for growing the p-type gradient Al component AlGaN layer in the step are as follows: the temperature of the reaction chamber is 900-1350 ℃, the pressure of the reaction chamber is kept at 10-75Torr, an aluminum source with the flow of 50-240sccm is introduced into the reaction chamber, and the flow of the aluminum source is uniformly decreased from 240sccm to 50sccm in the growth process.
(5) Etching from the top p-type gradient Al component AlGaN layer to the n-type gradient Al component AlGaN layer by adopting inductive coupling plasma or reactive ion etching to form an n-type AlGaN table top;
(6) photoetching a pattern of an n-type electrode on an n-type A1GaN table board, and evaporating the n-type electrode by using a film plating machine;
(7) photoetching a P-type electrode pattern on the P-type gradient Al component AlGaN layer, evaporating the P-type electrode by using a film plating machine, and completing MoS-based2And (3) manufacturing the thin-layer ultraviolet light-emitting diode.
The technical solution of the present invention is further illustrated below with reference to two specific examples.
Example 1, a MoS2 thin layer uv led with an emission wavelength of 320nm was fabricated on a c-plane sapphire substrate, comprising the steps of:
step one, preprocessing a substrate
Cleaning c-plane sapphire substrate, placing the substrate in a chemical vapor deposition CVD reaction chamber, and reducing the vacuum degree of the reaction chamber to 1 × 10-1Torr; introducing hydrogen into the reaction chamber, heating the substrate to 800 ℃ under the condition that the pressure of the CVD reaction chamber reaches 200Torr, and keeping the temperature for 15min to finish the heat treatment of the substrate;
step two, MoS growth2Layer(s)
A drop of reduced graphene oxide solution is suspended on the surface of a substrate base substrate on the treated substrate, and then the substrate base substrate is dried at 50 ℃, and MO is added3The powder was placed in a CVD ceramic boat and the substrate was mounted face down on top of the boat. Placing a separate ceramic boat of sulfur powder in the MO3Beside the powder, adopting CVD process at 800 deg.C in the reaction chamber, introducing nitrogen gas with flow rate of 250sccm as carrier gas, and growing MoS with thickness of 2-5nm under the condition of maintaining pressure of 20Torr2And (3) a layer.
Step three, growing an n-type gradient Al component AlGaN layer
In MoS2And simultaneously introducing three gases, namely ammonia gas with the flow rate of 1000sccm, a gallium source with the flow rate of 47sccm and an aluminum source with the flow rate of 50sccm, into the layer by adopting an MOCVD (metal organic chemical vapor deposition) process under the condition that the temperature of a reaction chamber is 1080 ℃, uniformly increasing the flow rate of the aluminum source from 50sccm to 200sccm in the growth process, and growing an n-type gradient Al component AlGaN layer with the thickness of 100nm under the condition that the pressure is kept at 30 Torr.
Step four, growing the AlGaN quantum well layer
And simultaneously introducing three gases of ammonia gas with the flow rate of 1000sccm, a gallium source with the flow rate of 60sccm and an aluminum source with the flow rate of 180sccm into the n-type gradient Al component AlGaN layer by adopting an MOCVD (metal organic chemical vapor deposition) process under the condition that the temperature of a reaction chamber is 1100 ℃, and growing the AlGaN quantum barrier with the thickness of 7nm under the condition that the pressure is kept at 35 Torr. Introducing three gases of ammonia gas with the flow rate of 1000sccm, a gallium source with the flow rate of 67sccm and an aluminum source with the flow rate of 168sccm, and growing an AlGaN quantum barrier with the thickness of 1nm under the condition of keeping the pressure of 35 Torr;
and repeating the above conditions to grow the AlGaN quantum well barrier with 8 periods.
Step five, growing a p-type gradient Al component AlGaN layer
On the AlGaN quantum well layer, ammonia gas with the flow rate of 1200sccm, a gallium source with the flow rate of 58sccm, an aluminum source with the flow rate of 200sccm and an Mg source with the flow rate of 16sccm are simultaneously introduced by adopting an MOCVD process under the condition that the temperature of a reaction chamber is 1090 ℃, and the AlGaN quantum well layer is grown to have the thickness of 120nm and the doping concentration of 1 multiplied by 10 under the condition that the pressure is kept at 40Torr19cm-3The p-type gradient Al component AlGaN layer.
Sixthly, etching and manufacturing electrodes
And etching from the top p-type gradient Al component AlGaN layer to the n-type gradient Al component AlGaN layer by adopting inductive coupling plasma or reactive ion etching to form an n-type AlGaN mesa deposition electrode. Respectively depositing n-type electrodes on the n-type gradient Al component AlGaN layer and p-type electrodes on the p-type gradient Al component AlGaN layer by adopting a metal sputtering method to finish the MoS with the luminous wavelength of 320nm on the c-plane sapphire substrate2And (5) manufacturing the thin-layer ultraviolet light-emitting diode.
Example 2 preparation of MoS having an emission wavelength of 295nm on a c-plane sapphire substrate2The thin-layer ultraviolet light-emitting diode comprises the following steps:
step one, preprocessing a substrate
Cleaning c-plane sapphire substrate, placing the substrate in a chemical vapor deposition CVD reaction chamber, and reducing the vacuum degree of the reaction chamber to 1 × 10-1Torr; introducing hydrogen gas into the reaction chamber, heating the substrate to 800 ℃ under the condition that the pressure in the CVD reaction chamber reaches 200Torr, and keeping the temperature for 15min to finish the heat treatment of the substrate.
Step two, MoS growth2Layer(s)
A drop of reduced graphene oxide solution is suspended on the surface of a substrate base substrate on the treated substrate, and then the substrate base substrate is dried at 50 ℃, and MO is added3Powder put into CVD ceramicIn the boat, and the substrates were mounted face down on the top of the boat. Placing a separate ceramic boat of sulfur powder in the MO3Beside the powder, adopting CVD process at 800 deg.C in the reaction chamber, introducing nitrogen gas with flow rate of 250sccm as carrier gas, and growing MoS with thickness of 2-5nm under the condition of maintaining pressure of 20Torr2And (3) a layer.
Step three, growing an n-type gradient Al component AlGaN layer
In MoS2And simultaneously introducing three gases, namely ammonia gas with the flow rate of 1000sccm, a gallium source with the flow rate of 37sccm and an aluminum source with the flow rate of 70sccm, into the layer by adopting an MOCVD (metal organic chemical vapor deposition) process under the condition that the temperature of a reaction chamber is 1080 ℃, uniformly increasing the flow rate of the aluminum source from 70sccm to 300sccm in the growth process, and growing an n-type gradient Al component AlGaN layer with the thickness of 100nm under the condition that the pressure is kept at 30 Torr.
Step four, growing the AlGaN quantum well layer
And simultaneously introducing three gases of ammonia gas with the flow rate of 1000sccm, a gallium source with the flow rate of 60sccm and an aluminum source with the flow rate of 180sccm into the n-type gradient Al component AlGaN layer by adopting an MOCVD (metal organic chemical vapor deposition) process under the condition that the temperature of a reaction chamber is 1100 ℃, and growing the AlGaN quantum barrier with the thickness of 7nm under the condition that the pressure is kept at 35 Torr. Introducing three gases of ammonia gas with the flow rate of 1000sccm, a gallium source with the flow rate of 67sccm and an aluminum source with the flow rate of 168sccm, and growing an AlGaN quantum barrier with the thickness of 1nm under the condition of keeping the pressure of 35 Torr;
and repeating the above conditions to grow the AlGaN quantum well barrier with 8 periods.
Step five, growing a p-type gradient Al component AlGaN layer
On the AlGaN quantum well layer, ammonia gas with the flow rate of 1200sccm, a gallium source with the flow rate of 50sccm, an aluminum source with the flow rate of 300sccm and an Mg source with the flow rate of 16sccm are simultaneously introduced by adopting an MOCVD process under the condition that the temperature of a reaction chamber is 1090 ℃, and the AlGaN quantum well layer is grown to have the thickness of 120nm and the doping concentration of 1 multiplied by 10 under the condition that the pressure is kept at 40Torr19cm-3The p-type gradient Al component AlGaN layer.
Sixthly, etching and manufacturing electrodes
Using inductively coupled plasma or reactive ionAnd the sub-etching is carried out from the top p-type gradient Al component AlGaN layer to the n-type gradient Al component AlGaN layer to form an n-type AlGaN mesa deposition electrode. Respectively depositing n-type electrodes on the n-type gradient Al component AlGaN layer and p-type electrodes on the p-type gradient Al component AlGaN layer by adopting a metal sputtering method to finish the MoS with the luminescent wavelength of 295nm on the c-plane sapphire substrate2And (5) manufacturing the thin-layer ultraviolet light-emitting diode.
As shown in fig. 2, a triangular MoS based on growth on a sapphire substrate2Wherein FIG. 2A is a triangular MOS with a magnification of 10000X2FIG. 2B is a schematic view of a triangular MOS device at a magnification of 500 ×2SEM pictures of (d). FIG. 3 shows a single layer MoS grown on a sapphire substrate2Wherein FIG. 3A is a single layer MOS with a magnification of 10000 ×2SEM picture of film, FIG. 3B is a single layer MOS at 500 Xmagnification2SEM pictures of the films. FIG. 4 shows a 295nm deep ultraviolet LED temperature varying PL spectrum.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (9)
1. Based on MoS2The thin-layer ultraviolet light-emitting diode is characterized by comprising a substrate and MoS which are arranged from bottom to top in sequence2The solar cell comprises a layer, an n-type gradient Al component AlGaN layer, an AlGaN quantum well layer, a p-type gradient Al component AlGaN layer and a p electrode, wherein the n electrode is arranged on the upper side of the n-type gradient Al component AlGaN layer, and the MoS is arranged on the upper side of the N-type gradient Al component AlGaN layer2MoS with layers tiled by multiple layers2The material is formed.
2. MoS-based according to claim 12The thin layer ultraviolet light emitting diode of (1), wherein the MoS2The thickness of the layer is 2-5 nm.
3. MoS-based according to claim 12The thin layer ultraviolet light emitting diode of (1), wherein n isThe thickness of the AlGaN layer with the n-type gradient Al component is 100-120nm, the Al component in the AlGaN layer with the n-type gradient Al component is linearly and gradually increased and gradually changed, and the doping concentration of Si is 5' 1018cm-3。
4. MoS-based according to claim 12The thin ultraviolet light emitting diode is characterized in that the AlGaN quantum well layer has a thickness of 40-60 nm;
the thickness of the p-type gradient Al component AlGaN layer 5 is 100-120nm, the Al component in the p-type gradient Al component AlGaN layer is linearly and gradually increased and gradually changed, and the Mg doping concentration is 1' 1019cm-3。
5. MoS-based according to any of claims 1 to 42The preparation method of the thin-layer ultraviolet light-emitting diode is characterized by comprising the following steps:
(1) MoS with the thickness of 2-5nm is grown on a substrate by using a CVD process2A layer;
(2) MoS on blanket substrate2On the layer, an n-type gradient Al component AlGaN layer with the thickness of 100-120nm is grown by utilizing an MOCVD process in a mode of linearly increasing the flow of an Al source, and the Si doping concentration of the n-type gradient Al component AlGaN layer is 5' 1018cm-3；
(3) Growing an AlGaN quantum well layer with the thickness of 40-60nm on the AlGaN layer with the n-type gradually-changed Al component by utilizing an MOCVD (metal organic chemical vapor deposition) process;
(4) growing a p-type gradient Al component AlGaN layer with the thickness of 100-120nm on the AlGaN quantum well layer by utilizing an MOCVD process in a way of linearly reducing the flow of an Al source, wherein the Mg doping concentration is 1' 1019cm-3；
(5) Etching from the top p-type gradient Al component AlGaN layer to the n-type gradient Al component AlGaN layer by adopting inductive coupling plasma or reactive ion etching to form an n-type AlGaN table top;
(6) photoetching a pattern of an n-type electrode on an n-type A1GaN table board, and evaporating the n-type electrode by using a film plating machine;
(7) photoetching a P-type electrode pattern on the P-type gradient Al component AlGaN layer, and evaporating P by using a film plating machineShaped electrode, finish based on MoS2And (3) manufacturing the thin-layer ultraviolet light-emitting diode.
6. MoS-based according to claim 52The preparation method of the thin-layer ultraviolet light-emitting diode is characterized in that MoS grows in the step (1)2The process conditions of the layers are: the temperature of the reaction chamber is 650-850 ℃, the pressure of the reaction chamber is kept at 20-75Torr, nitrogen with the flow of 250-300sccm is simultaneously introduced into the reaction chamber, a drop of reduced graphene oxide solution is coated on the surface of the substrate before growth, and then drying is carried out at 50 ℃, and MO is obtained3The powder was placed in a CVD ceramic boat with the substrate mounted face down on top of the boat, and a separate ceramic boat of sulfur powder was placed in the MO3Beside the powder.
7. MoS-based according to claim 52The preparation method of the thin-layer ultraviolet light-emitting diode is characterized in that the process conditions for growing the n-type gradient Al component AlGaN layer in the step (2) are as follows: the temperature of the reaction chamber is 900-1350 ℃, the pressure of the reaction chamber is kept at 10-75Torr, an aluminum source with the flow of 50-200sccm is introduced into the reaction chamber, and the flow of the aluminum source is uniformly increased from 50sccm to 200sccm in the growth process.
8. MoS-based according to claim 52The preparation method of the thin ultraviolet light emitting diode is characterized in that the technological conditions for growing the AlGaN quantum well layer in the step (3) are as follows: the temperature of the reaction chamber is 900-1350 ℃, the pressure of the reaction chamber is kept at 15-75Torr, and aluminum source with the flow rate of 120-240sccm is introduced into the reaction chamber.
9. MoS-based according to claim 52The preparation method of the thin-layer ultraviolet light-emitting diode is characterized in that the process conditions for growing the p-type gradient Al component AlGaN layer in the step (4) are as follows: the temperature of the reaction chamber is 900-1350 ℃, the pressure of the reaction chamber is kept at 10-75Torr, an aluminum source with the flow of 50-240sccm is introduced into the reaction chamber, and the flow of the aluminum source is uniformly decreased from 240sccm to 50sccm in the growth process.
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