CN110957205A - Preparation method of ohmic contact transparent electrode on p-type GaN - Google Patents
Preparation method of ohmic contact transparent electrode on p-type GaN Download PDFInfo
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- 238000000151 deposition Methods 0.000 claims abstract description 4
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- 239000002243 precursor Substances 0.000 claims description 47
- 229910052751 metal Inorganic materials 0.000 claims description 21
- 239000002184 metal Substances 0.000 claims description 21
- 229910052725 zinc Inorganic materials 0.000 claims description 19
- 239000011701 zinc Substances 0.000 claims description 19
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 18
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 18
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- 239000000084 colloidal system Substances 0.000 claims description 16
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- 238000003756 stirring Methods 0.000 claims description 12
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 150000003751 zinc Chemical class 0.000 claims description 6
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
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- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical group OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 claims description 3
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- 229920002873 Polyethylenimine Polymers 0.000 description 10
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- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02697—Forming conducting materials on a substrate
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
- H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
- H01L21/288—Deposition of conductive or insulating materials for electrodes conducting electric current from a liquid, e.g. electrolytic deposition
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention provides a preparation method of an ohmic contact transparent electrode material on p-type GaN. The method adopts a macromolecule auxiliary deposition method to grow an Al-doped ZnO film, and then adopts annealing treatment to obtain the required AZO electrode layer film. The electrode layer film has the advantages of simple growth method, low cost, large-area growth, small resistivity and high light transmittance, and can form good ohmic contact with p-type GaN.
Description
Technical Field
The invention relates to a preparation method of an ohmic contact transparent electrode on p-type GaN.
Background
Third generation semiconductors (i.e., wide bandgap semiconductors, with a bandgap greater than 2.2eV) represented by group III nitrides have great application prospects, wherein GaN materials have been widely used in the field of optoelectronic devices. In order to fabricate a high-performance device, an electrode layer forming an ohmic contact with the GaN material is very necessary. The good ohmic contact can effectively reduce the series resistance in the device, thereby reducing the starting voltage and the working current of the device, reducing the heat generation of the device and improving the performance of the device. However, since the valence band top of p-type GaN is far away from the vacuum level (7.4eV), it is difficult for general conductive materials to achieve such a high work function, and once the work functions are not matched, schottky contact is formed at the contact interface, and the contact resistance of schottky contact is much larger than that of ohmic contact, so that it is difficult to realize ohmic contact of p-type GaN in an actual device. The commonly used electrode materials at present comprise metal electrodes such as Ni/Au, Ni/Pd and the like. However, the metal electrode still has many problems, such as high cost, non-transparency, and thus, the light emitting efficiency of the device is affected. Transparent oxide semiconductor electrodes have attracted extensive interest to researchers. Compared with common tin-doped indium oxide, aluminum-doped zinc oxide (AZO) has better application prospect because AZO has smaller resistivity, better light transmission, lower cost of aluminum and zinc, and environmental friendliness. At present, a plurality of methods are used for researching the preparation of the AZO electrode, including magnetron sputtering, pulsed laser deposition, electron beam evaporation and the like, but the method for preparing the film has higher cost, including equipment cost and raw material cost. It is also difficult to grow large area films, such as magnetron sputtering method of growing films of a few inches at the maximum, and pulsed laser deposition, electron beam evaporation method of growing films of a few centimeters at the maximum. The invention adopts a macromolecule auxiliary deposition method, and aims to provide a novel low-cost large-area AZO film growth process for preparing transparent electrode layers in various optoelectronic devices.
Disclosure of Invention
The invention aims to provide a preparation method of a metal-doped zinc oxide film with low cost and large-area growth.
The technical scheme for realizing the purpose of the invention is as follows:
a preparation method of a p-type GaN ohmic contact transparent electrode adopts a macromolecule auxiliary deposition method to grow a metal-doped ZnO electrode layer, and comprises the following steps:
(1) preparing a precursor solution, namely respectively preparing a zinc precursor solution comprising zinc salt, PEI, EDTA and deionized water and a doped metal precursor solution comprising doped metal salt, PEI, EDTA and deionized water; respectively carrying out superfine filtration on the obtained precursor solution to obtain a zinc precursor colloid and a doped metal precursor colloid;
(2) mixing the precursor colloid obtained in the step (1), mixing the two precursor colloids according to a required molar ratio to obtain a precursor source, and uniformly stirring;
(3) uniformly coating the obtained precursor source on the surface of a p-type GaN film, and drying at the temperature of 40-150 ℃ to solidify colloid;
(4) and annealing at 500-800 ℃ in an air atmosphere for 1-2 h to obtain the required metal-doped ZnO electrode film.
Preferably, in the zinc precursor solution, the molar ratio of zinc, PEI and EDTA is (0.9-1.1): (0.9-1.1): (1-1.2).
Preferably, in the doped metal precursor solution, the molar ratio of the doped metal, the PEI and the EDTA is (0.9-1.1): (0.9-1.1): (1-1.2).
Preferably, the zinc salt is zinc acetate dihydrate.
Preferably, the preparation method of the zinc precursor solution comprises the following steps: adding zinc salt and PEI into deionized water in a mixing manner, uniformly stirring, then adding EDTA, and uniformly stirring to form a zinc precursor solution.
Preferably, the doping metal is aluminum, gallium or indium.
Preferably, when the doping metal is aluminum, the method for preparing the precursor solution of the doping metal comprises the following steps: adding aluminum nitrate nonahydrate and PEI into deionized water in a mixing manner, uniformly stirring, then adding EDTA, uniformly stirring, and slowly adding ammonia water with the concentration of 10% -30% to enable the pH value of the solution to be 7-8, so as to form a precursor solution doped with metallic aluminum.
Preferably, the amount ratio of the doping metal to the zinc in the step (2) is (3-20): 100.
preferably, step (3) is performed by a spin coater or a spray coater.
Compared with the prior art, the invention has the following technical effects:
the raw materials and experimental instruments used by the method are relatively cheap, so that the production cost can be reduced.
2, the invention adopts polyethyleneimine and ethylene diamine tetraacetic acid to assist in preparing precursor solution, and can generate compactAfter annealing, the Fermi pinning effect appears at the interface of the continuous film material, so that ohmic contact is formed, and the performance parameters of the AZO film electrode layer prepared by the method can reach: forming good ohmic contact with p-type GaN and having resistivity of 1.47 × 10-3Omega cm, specific contact resistance 1.08X 10-1Ω·cm2And the light transmittance is higher than 90% in the whole visible light wave band.
3, the method provided by the invention can easily prepare a large-area film, and theoretically, the film with any area can grow.
4, the precursor source prepared by the invention is a metal organic chelate, has stable performance, can be stored for years under a common state without deterioration, can be used for a long time after a batch of precursors are prepared, and simultaneously can be used for separately preparing the precursors of aluminum and zinc, so that when the aluminum doping amount in a final product needs to be changed, a precursor solution does not need to be prepared, only the mixing ratio between the two precursors needs to be changed, and the application is more convenient.
Drawings
FIG. 1 is a current-voltage relationship curve of AZO transparent electrode films prepared at different annealing temperatures according to example 1 of the present invention;
FIG. 2 is a current-voltage relationship curve of AZO transparent electrode films prepared under different aluminum ion doping concentrations in example 1 of the present invention;
FIG. 3 is a specific contact resistance curve of an AZO transparent electrode film obtained by annealing at 600 ℃ and doping aluminum ions with a concentration of 9% in example 1 of the present invention;
FIG. 4 is a graph showing the transmittance of an AZO transparent electrode film having an Al ion doping concentration of 9% when annealed at 600 ℃ in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail below with reference to examples of implementation and the accompanying drawings, but the embodiments of the present invention are not limited thereto.
Example 1
Synthesizing a zinc precursor solution: 2.2 g of zinc acetate dihydrate and 3 g of PEI (polyethyleneimine) are mixed and added into every 40 ml of deionized water, and the mixture is stirred for more than 30 minutes to be uniformly mixed. Then adding 4 g of EDTA (ethylene diamine tetraacetic acid), and uniformly mixing the EDTA and the EDTA by stirring for more than 30 minutes to form a zinc precursor solution, which is marked as solution A. And (3) carrying out superfine filtration on the solution A to remove acetate ions in the solution A so as to obtain a colloid A.
Synthesizing an aluminum precursor solution: 3.7 g of aluminum nitrate nonahydrate and 3 g of PEI are mixed in every 40 ml of deionized water and stirred uniformly. Then 4 g of EDTA is added and evenly stirred, and meanwhile, 10% ammonia water is slowly added to make the pH value of the solution be 8, so that an aluminum precursor solution is formed and is marked as solution B. And (4) carrying out superfine filtration on the solution B to remove nitrate ions in the solution B to obtain colloid B.
By operating according to the above stoichiometry, precursor sources of any desired dose can be obtained. The resulting precursor source for each batch, where the metal ion concentration needs to be quantitatively tested, can be determined using inductively coupled plasma emission spectroscopy. And mixing the two colloids according to the molar concentration of Al, Zn (3-20) and 100, and stirring the mixed solution for more than 30 minutes to obtain a precursor colloid mixed solution.
A two-inch p-type GaN film is selected as the substrate, but the substrate is not limited to p-type GaN material, and other substrates commonly used in microelectronics and optoelectronic devices, such as Si sheets and the like, can also be used as the substrate material of the invention. The size of the substrate is also not limited to two inches, and larger substrates need only be coated with an appropriate amount of glue during glue spreading. And (3) dripping the precursor colloid mixed solution on the substrate in a proper amount, and uniformly spinning by using a spin coater to uniformly coat the precursor colloid on the surface of the substrate. The rotation speed of the spin coater is 6000 rpm, and the rotation time is 1 minute. Under the condition of the spin coating, the thickness of the finally obtained AZO film layer is about 30 nanometers. The glue homogenizing process is repeated to obtain other thicknesses. After the completion of the glue homogenizing, the mixture is dried for 10 minutes at the temperature of 60 ℃ in the air atmosphere to solidify the glue. And then annealing at 500-800 ℃ for 2 hours in a heating furnace in an air atmosphere at a high temperature to finally obtain the required AZO film.
And testing the electrical property of the AZO transparent electrode film. The test sample is an AZO film grown on p-type GaN, a pattern is defined by utilizing photoetching, and the AZO film is formed into a required shape and size by utilizing wet etching. In the current and voltage test shown in fig. 1 and 2, a plurality of square electrodes of 10 × 10mm are formed on the AZO thin film, the distance between the two square electrodes is 10mm, bias voltages are respectively applied to the two adjacent square electrodes during the test, and the magnitude of the current passing between the two square electrodes is measured.
Fig. 1 shows aluminum: and when the concentration ratio of zinc ions is 9:100, applying bias voltage to two of the four leads on the electrode film in the test according to the current-voltage relation curve of the AZO transparent electrode film at different annealing temperatures, and measuring the current between the other two leads. It can be seen that under forward and reverse bias, the current and voltage are in good linear relationship, which indicates that the AZO electrode layer obtained in the invention and the p-type GaN form good ohmic contact.
FIG. 2 shows the annealing temperature conditions at 600 ℃ for different aluminum: and when the concentration ratio of zinc ions is higher, the current-voltage relation curve of the AZO transparent electrode film also shows that the AZO electrode layer and the p-type GaN form good ohmic contact.
FIG. 3 is a graph showing specific contact resistance of the AZO transparent electrode thin film obtained when annealing is performed at 600 ℃ and the aluminum ion doping concentration is 9%. The testing process is to etch and prepare a plurality of annular grooves with different sizes on the AZO film and test the specific resistance of the annular grooves with different groove intervals. The radius of the annular inner circle is 100 mu m, and the distance between the grooves is 5-30 mu m. During testing, bias voltages are respectively applied to the AZO film on the inner circle and the AZO film outside the groove. The contact resistance was measured as a function of the trench width. The results show that the specific contact resistance is 1.08X 10-1Ω·cm2。
As the GaN material grows on the single-side polished sapphire substrate, the light transmittance of the GaN material is poor, in order to represent the light transmittance performance of a sample, transparent quartz glass is adopted as the substrate, and a growth process consistent with that of other samples is adopted on the substrate to prepare the AZO film. And the transmittance of light of different wavelengths ranging from 350nm to 700nm through the AZO film was tested. FIG. 4 is a light transmittance curve of the AZO transparent electrode film obtained by annealing at 600 ℃ and doping aluminum ions with a concentration of 9%, wherein the light transmittance in a visible light region is higher than 90%, and the film has good transparency.
Claims (9)
1. A preparation method of an ohmic contact transparent electrode on p-type GaN is characterized by comprising the following steps: a macromolecule assisted deposition method is adopted to grow a metal-doped ZnO electrode layer, and the steps are as follows:
(1) preparing a precursor solution, namely respectively preparing a zinc precursor solution comprising zinc salt, PEI, EDTA and deionized water and a doped metal precursor solution comprising doped metal salt, PEI, EDTA and deionized water; respectively carrying out superfine filtration on the obtained precursor solution to obtain a zinc precursor colloid and a doped metal precursor colloid;
(2) mixing the precursor colloid obtained in the step (1), mixing the two precursor colloids according to a required molar ratio to obtain a precursor source, and uniformly stirring;
(3) uniformly coating the obtained precursor source on the surface of a p-type GaN film, and drying at the temperature of 40-150 ℃ to solidify colloid;
(4) and annealing at 500-800 ℃ in an air atmosphere for 1-2 h to obtain the required metal-doped ZnO electrode film.
2. The method for preparing the transparent electrode in ohmic contact on p-type GaN according to claim 1, wherein in the zinc precursor solution, the molar ratio of zinc, PEI and EDTA is (0.9-1.1): (0.9-1.1): (1-1.2).
3. The method for preparing the transparent electrode in ohmic contact on p-type GaN according to claim 1, wherein in the doped metal precursor solution, the molar ratio of the doped metal, PEI and EDTA is (0.9-1.1): (0.9-1.1): (1-1.2).
4. The method for preparing an ohmic contact transparent electrode on p-type GaN according to claim 1, wherein the zinc salt is zinc acetate dihydrate.
5. The method for preparing an ohmic contact transparent electrode on p-type GaN according to claim 1 or 4, wherein the method for preparing the zinc precursor solution comprises: adding zinc salt and PEI into deionized water in a mixing manner, uniformly stirring, then adding EDTA, and uniformly stirring to form a zinc precursor solution.
6. The method of claim 1, wherein the doped metal is aluminum, gallium or indium.
7. The method for preparing an ohmic contact transparent electrode on p-type GaN according to claim 5, wherein when the doped metal is aluminum, the method for preparing the precursor solution of the doped metal comprises: adding aluminum nitrate nonahydrate and PEI into deionized water in a mixing manner, uniformly stirring, then adding EDTA, uniformly stirring, and slowly adding ammonia water with the concentration of 10% -30% to enable the pH value of the solution to be 7-8, so as to form a precursor solution doped with metallic aluminum.
8. The method for preparing the ohmic contact transparent electrode on the p-type GaN according to claim 1, wherein the amount ratio of the doped metal to the zinc substance in the step (2) is (3-20): 100.
9. the method for preparing an ohmic contact transparent electrode on p-type GaN according to claim 1, characterized in that step (3) is carried out by coating with a spin coater or a spray coater.
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| 吴兆丰 等: "铝共掺杂调制ＺｎＯ∶Ｍｎ纳米棒阵列的磁学和电学特性", 《功能材料》 * |
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| CN110957205B (en) | 2022-06-07 |
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