CN111668326B - Based on CuAlO 2 /SiC ultraviolet photodiode and preparation method - Google Patents
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- 238000004519 manufacturing process Methods 0.000 claims abstract description 24
- 238000007664 blowing Methods 0.000 claims abstract description 6
- 238000004544 sputter deposition Methods 0.000 claims description 65
- 238000010438 heat treatment Methods 0.000 claims description 50
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- 238000000137 annealing Methods 0.000 claims description 18
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- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 12
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- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
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- 239000007769 metal material Substances 0.000 claims description 9
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- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 6
- 238000005229 chemical vapour deposition Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000001294 propane Substances 0.000 claims description 6
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- 238000003980 solgel method Methods 0.000 claims description 6
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- 238000002834 transmittance Methods 0.000 description 1
- 238000000825 ultraviolet detection Methods 0.000 description 1
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Abstract
The invention discloses CuAlO 2 the/SiC ultraviolet photodiode comprises a top electrode and a bottom electrode, wherein P-type crystal CuAlO is sequentially arranged between the two electrodes from the top electrode to the bottom electrode 2 A film, an I-type SiC film and an N-type SiC substrate, and also discloses a CuAlO 2 Firstly, cleaning an N-type SiC substrate, and blowing the cleaned N-type SiC substrate to dry for later use; growing an intrinsic SiC homogeneous epitaxial layer on the cleaned N-type SiC substrate; p-type crystal CuAlO on intrinsic SiC homogeneous epitaxial layer 2 Growing a heteroepitaxial layer; in P-type crystal CuAlO 2 Manufacturing a top electrode on the heteroepitaxial layer; making a bottom electrode on the lower surface of the N-type SiC substrate to finally form CuAlO 2 The invention has the advantages of good photoelectric response, good stability, sensitive reaction and good repeatability of the processing technology.
Description
Technical Field
The invention belongs to the technical field of ultraviolet photoelectric detection application, and particularly relates to CuAlO 2 The invention also relates to a CuAlO ultraviolet photodiode 2 A preparation method of a SiC ultraviolet photodiode.
Background
Ultraviolet detection technology is one of the rapidly developed photoelectric detection technologies in recent years. The ultraviolet detector has important application in missile early warning, water quality monitoring, disaster weather forecast and other aspects. Silicon carbide (4H-SiC) as a representative of third-generation wide bandgap semiconductor materials has the properties of large forbidden band width, high breakdown electric field, high thermal conductivity, high electronic saturation mobility, small dielectric constant and the like, so that the silicon carbide has great application potential in the fields of ultraviolet photoelectric detection devices, power electronics, lasers and the like.
The 4H-SiC PIN type ultraviolet detector has the characteristics of low noise, high photoelectric responsivity and the like. Typically, P-type doping of silicon carbide is Al-doping thereof due to ionization of Al at room temperatureThe energy is high, and complete ionization can not be realized at room temperature, so that the doping concentration of the P-type silicon carbide is not high. And CuAlO 2 The film is a semiconductor material with excellent photoelectric property, is a transparent conductive oxide film with wide forbidden band (the forbidden band width is 3.5eV), and has larger forbidden band width and higher hole concentration compared with P-type silicon carbide. The invention designs a p-CuAlO-based material 2 The ultraviolet photodiode of the/n-SiC heterojunction thin film has good photoelectric response, good stability, sensitive reaction, good repeatability of the processing technology and huge application prospect.
Disclosure of Invention
The invention aims to provide CuAlO 2 the/SiC ultraviolet photodiode has good photoelectric response, good stability, sensitive reaction and good repeatability of the processing technology.
Another object of the present invention is to provide a CuAlO 2 A preparation method of a/SiC ultraviolet photodiode.
The first technical scheme adopted by the invention is that CuAlO 2 the/SiC ultraviolet photodiode comprises a top electrode and a bottom electrode, wherein P-type crystal CuAlO is sequentially arranged between the two electrodes from the top electrode to the bottom electrode 2 A film, an I-type SiC film, and an N-type SiC substrate.
The first technical aspect of the present invention is also characterized in that,
the top electrode and the bottom electrode are made of a mixture of any one of Au, Al, Ni, Cu and Pb metal materials, or an alloy containing one or any one of the mixed metal materials, or an ITO conductive compound.
The N-type SiC substrate is a nitrogen-doped SiC material; the type I crystal SiC film is an unintentionally doped SiC layer with the doping concentration of 10 15 cm ～3 。
P-type crystal CuAlO 2 The film doping concentration is 10 17 ～10 18 cm ～3 。
The second technical scheme adopted by the invention is that CuAlO 2 The preparation method of the/SiC ultraviolet photodiode is implemented according to the following steps:
Step 1, cleaning an N-type SiC substrate, and drying the substrate after cleaning for later use;
step 4, obtaining P type crystal CuAlO in the step 3 2 Manufacturing a top electrode on the heteroepitaxial layer;
The second technical aspect of the present invention is also characterized in that,
the cleaning process in the step 1 comprises the following steps: and cleaning the sample by using a cleaning solution, hydrofluoric acid, alcohol and deionized water in sequence.
And 2, when the intrinsic SiC homogeneous epitaxial layer is grown on the N-type SiC substrate in the step 2, utilizing chemical vapor deposition equipment, taking silane as a Si source gas, propane as a C source gas and hydrogen as a carrier gas, wherein the hydrogen flow is 40-60slm, the C/Si ratio is 1.0-1.5, the growth temperature is 1520-1600 ℃, and the growth time is 2-5 min.
Performing P-type crystal CuAlO on the intrinsic SiC homogeneous epitaxial layer in step 2 2 Growth of heteroepitaxial layers with Cu (NO) 3 ) 2 ·5H 2 O as Cu source, Al (NO) 3 ) 3 ·9H 2 Taking O as an Al source, taking polyvinyl alcohol PVA as a stabilizer, and carrying out P-type crystal CuAlO on an intrinsic SiC homogeneous epitaxial layer by adopting a sol-gel method 2 And (3) growing the heteroepitaxial layer, specifically comprising the following steps:
step 3.1, preparing a solution: taking Cu (NO) according to a molar ratio of 1:1 respectively 3 ) 2 ·5H 2 O and Al (NO) 3 ) 3 ·9H 2 O to Cu (NO) 3 ) 2 ·5H 2 O and Al (NO) 3 ) 3 ·9H 2 Adding polyvinyl alcohol PVA and deionized water into the mixture of O to ensure that the concentration of the polyvinyl alcohol PVA in the solution is 0.05 mol/L-0.15 mol/L;
step 3.2, heating and stirring the solution obtained in the step 3.1 in a water bath, controlling the temperature of the water bath to be 80-90 ℃, controlling the heating time to be 3-5 h, and cooling to room temperature after heating to obtain sol;
step 3.3, spin-coating the sol prepared in the step 3.2 on an intrinsic SiC homogeneous epitaxial layer, wherein the spin-coating speed is controlled to be 2500-3000 rpm during spin-coating, the spin time is controlled to be 30-45 s, and a sample obtained after spin-coating is subjected to heat treatment for 5-10 min in an air environment, wherein the heat treatment temperature is 300-400 ℃;
step 3.4, after the heating treatment, after the sample is cooled to room temperature in the air, carrying out secondary spin coating and heat treatment, and controlling the prepared CuAlO by adjusting the repeated times of the spin coating and the heat treatment 2 The thickness of the heteroepitaxial layer;
step 3.5, placing the sample obtained after the spin coating and the heat treatment in an Ar gas environment for annealing treatment, wherein the annealing temperature is 900-1100 ℃, and the annealing time is 4-6 h to obtain p-type crystal CuAlO 2 A heteroepitaxial layer.
Step 4, adopting a magnetron sputtering method to perform P-type crystal CuAlO 2 And manufacturing a top electrode on the heteroepitaxial layer, which comprises the following steps:
step 4.1, taking Ti as a sputtering target material, and obtaining the P-type crystal CuAlO in the step 3 2 Sputtering the surface of the heteroepitaxial layer to form a Ti layer, wherein the sputtering time is controlled to be 0.1-2 hours, the pressure is controlled to be 0.1-10 Pa, and the sputtering power is controlled to be 100-200W;
step 4.2, sputtering Au serving as a sputtering target material on the surface of the Ti layer to form an Au layer, controlling the sputtering time to be 0.1-2 hours, controlling the deposition pressure to be 2-4 Pa and the sputtering power to be 10-20 mW, and realizing the purpose of forming CuAlO on the P-type crystal 2 And preparing a top electrode on the heteroepitaxial layer.
step 5.1, sputtering Ni serving as a target on the surface of the N-type SiC substrate on one surface on which the intrinsic SiC homogeneous epitaxial layer does not grow to form a Ni layer, wherein the sputtering time is controlled to be 0.1-2 hours, the pressure intensity is controlled to be 0.1-10 Pa, and the sputtering power is controlled to be 100-200 watts;
and 5.2, sputtering Au serving as a sputtering target material on the surface of the Ni layer to form an Au layer, controlling the deposition time to be 0.1-2 hours, controlling the deposition pressure to be 2-4 Pa and the sputtering power to be 10-20 mW, namely preparing a bottom electrode on the N-type SiC substrate to finally obtain CuAlO 2 the/SiC ultraviolet photodiode.
The invention has the beneficial effects that CuAlO 2 The first time, the SiC ultraviolet photodiode adopts CuAlO with excellent optical performance 2 The material fully exerts the characteristics of extremely high light transmittance of the material in a deep ultraviolet light region and a visible light region; meanwhile, the SiC material has large forbidden bandwidth and higher critical breakdown electric field intensity, so that the CuAlO of the invention 2 the/SiC ultraviolet photodiode has higher voltage withstanding level. Under the extreme conditions of high temperature, high pressure, high frequency, high radiation and the like, the CuAlO of the invention is adopted 2 The novel PIN ultraviolet photoelectric detector of the/SiC ultraviolet photoelectric diode not only has better detection performance than the prior PIN ultraviolet photoelectric detector, but also greatly improves the reliability of the device, thereby being more suitable for the extreme environment;
CuAlO 2 the preparation method of the/SiC ultraviolet photodiode can increase the width of a space charge region, increase photon-generated carriers and improve the photoelectric conversion efficiency by the design of the thickness and the doping concentration of the type I SiC layer. Meanwhile, the I-type SiC film can reduce junction capacitance, shorten response time and improve frequency response characteristics; in addition, the increase of the type I SiC thin film can share most of the reverse bias voltage, and is advantageous for suppressing dark current. Thus, compared to a SiC MSM photodetector, CuAlO 2 the/SiC ultraviolet photodiode has larger photoelectric responsivity and faster response speed.
Drawings
FIG. 1 shows CuAlO of the present invention 2 The structural schematic diagram of the PIN structure ultraviolet photodiode of/SiC;
FIG. 2 shows CuAlO of the present invention 2 A flow chart of a preparation method of the UV photodiode with the/SiC PIN structure.
In the figure, 1. top electrode, 2.P type crystal CuAlO 2 A film, 3.I type SiC film, 4.N type SiC substrate,5. a bottom electrode.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to CuAlO 2 The structure of the/SiC ultraviolet photodiode is shown in figure 1, and comprises a top electrode 1 and a bottom electrode 5, wherein P-type crystal CuAlO is sequentially arranged between the two electrodes from the top electrode 1 to the bottom electrode 5 2 A film 2, an I-type SiC film 3, and an N-type SiC substrate 4.
The top electrode 1 and the bottom electrode 5 are made of a mixture of any one of Au, Al, Ni, Cu and Pb metal materials, or an alloy containing one or any one of the mixed metal materials, or an ITO conductive compound.
The N-type SiC substrate 4 is a nitrogen-doped SiC material; the type I crystal SiC film is an unintentionally doped SiC layer with the doping concentration of 10 15 cm ～3 。
P-type crystal CuAlO 2 The film 2 has a doping concentration of 10 17 ～10 18 cm ～3 。
CuAlO 2 The preparation method of the/SiC ultraviolet photodiode is shown in a flow chart of fig. 2 and is specifically implemented according to the following steps:
step 1, cleaning an N-type SiC substrate 4, and drying the cleaned N-type SiC substrate by blowing for later use;
step 4, obtaining P type crystal CuAlO in the step 3 2 Manufacturing a top electrode on the heteroepitaxial layer;
The cleaning process in the step 1 comprises the following steps: and cleaning the sample by using a cleaning solution, hydrofluoric acid, alcohol and deionized water in sequence.
When the intrinsic SiC homogeneous epitaxial layer is grown on the N-type SiC substrate 4 in the step 2, chemical vapor deposition equipment is utilized, silane is used as a Si source gas, propane is used as a C source gas, and hydrogen is used as a carrier gas, wherein the hydrogen flow is 40-60slm, the C/Si ratio is 1.0-1.5, the growth temperature is 1520-1600 ℃, and the growth time is 2-5 min.
Performing P-type crystal CuAlO on the intrinsic SiC homogeneous epitaxial layer in step 2 2 Growth of heteroepitaxial layers with Cu (NO) 3 ) 2 ·5H 2 O as Cu source, Al (NO) 3 ) 3 ·9H 2 Taking O as an Al source, taking polyvinyl alcohol PVA as a stabilizer, and carrying out P-type crystal CuAlO on an intrinsic SiC homogeneous epitaxial layer by adopting a sol-gel method 2 Growing the heteroepitaxial layer, specifically as follows:
step 3.1, preparing a solution: taking Cu (NO) according to a molar ratio of 1:1 respectively 3 ) 2 ·5H 2 O and Al (NO) 3 ) 3 ·9H 2 O to Cu (NO) 3 ) 2 ·5H 2 O and Al (NO) 3 ) 3 ·9H 2 Adding polyvinyl alcohol PVA and deionized water into the mixture of O to ensure that the concentration of the polyvinyl alcohol PVA in the solution is 0.05 mol/L-0.15 mol/L;
step 3.2, heating and stirring the solution obtained in the step 3.1 in a water bath, controlling the temperature of the water bath to be 80-90 ℃, controlling the heating time to be 3-5 h, and cooling to room temperature after heating to obtain sol;
step 3.3, spin-coating the sol prepared in the step 3.2 on an intrinsic SiC homogeneous epitaxial layer, wherein the spin-coating speed is controlled to be 2500-3000 rpm during spin-coating, the spin time is controlled to be 30-45 s, and a sample obtained after spin-coating is subjected to heat treatment for 5-10 min in an air environment, wherein the heat treatment temperature is 300-400 ℃;
step 3.4, after the heating treatment, after the sample is cooled to room temperature in the air, carrying out secondary spin coating and heat treatment, and controlling the prepared CuAlO by adjusting the repeated times of the spin coating and the heat treatment 2 The thickness of the heteroepitaxial layer;
step 3.5, placing the sample obtained after the spin coating and the heat treatment in an Ar gas environment for annealing treatment, wherein the annealing temperature is 900-1100 ℃, and the annealing time is 4-6 h to obtain the productp-type crystalline CuAlO 2 A heteroepitaxial layer.
Step 4, adopting a magnetron sputtering method to perform P-type crystal CuAlO 2 And manufacturing a top electrode on the heteroepitaxial layer, which comprises the following steps:
step 4.1, taking Ti as a sputtering target material, and obtaining the P-type crystal CuAlO in the step 3 2 Sputtering the surface of the heteroepitaxial layer to form a Ti layer, wherein the sputtering time is controlled to be 0.1-2 hours, the pressure is controlled to be 0.1-10 Pa, and the sputtering power is controlled to be 100-200W;
step 4.2, sputtering Au serving as a sputtering target material on the surface of the Ti layer to form an Au layer, controlling the sputtering time to be 0.1-2 hours, controlling the deposition pressure to be 2-4 Pa and the sputtering power to be 10-20 mW, and realizing the purpose of forming CuAlO on the P-type crystal 2 And preparing a top electrode on the heteroepitaxial layer.
step 5.1, sputtering Ni serving as a target on the surface of the N-type SiC substrate on one surface on which the intrinsic SiC homogeneous epitaxial layer does not grow to form a Ni layer, wherein the sputtering time is controlled to be 0.1-2 hours, the pressure intensity is controlled to be 0.1-10 Pa, and the sputtering power is controlled to be 100-200 watts;
And 5.2, sputtering Au serving as a sputtering target material on the surface of the Ni layer to form an Au layer, controlling the deposition time to be 0.1-2 hours, controlling the deposition pressure to be 2-4 Pa and the sputtering power to be 10-20 mW, namely preparing a bottom electrode on the N-type SiC substrate to finally obtain CuAlO 2 A SiC UV photodiode.
Example 1
The invention relates to CuAlO 2 The structure of the/SiC ultraviolet photodiode is shown in figure 1, and comprises a top electrode 1 and a bottom electrode 5, wherein P-type crystal CuAlO is sequentially arranged between the two electrodes from the top electrode 1 to the bottom electrode 5 2 A film 2, an I-type SiC film 3, and an N-type SiC substrate 4.
The top electrode 1 and the bottom electrode 5 are made of a mixture of any one of Au, Al, Ni, Cu and Pb metal materials, or an alloy containing one or any one of the mixed metal materials, or an ITO conductive compound.
An N-type SiC substrate 4 ofA nitrogen-doped SiC material; the type I crystal SiC film is an unintentionally doped SiC layer with the doping concentration of 10 15 cm ～3 。
P-type crystal CuAlO 2 The film 2 has a doping concentration of 10 17 cm ～3 。
CuAlO 2 The preparation method of the/SiC ultraviolet photodiode is shown in a flow chart of fig. 2 and is specifically implemented according to the following steps:
step 1, cleaning an N-type SiC substrate 4, and drying the cleaned N-type SiC substrate by blowing for later use;
step 4, obtaining P type crystal CuAlO in the step 3 2 Manufacturing a top electrode on the heteroepitaxial layer;
The cleaning process in the step 1 comprises the following steps: and cleaning the sample by using a cleaning solution, hydrofluoric acid, alcohol and deionized water in sequence.
When the growth of the intrinsic SiC homogeneous epitaxial layer is carried out on the N-type SiC substrate 4 in the step 2, chemical vapor deposition equipment is utilized, silane is used as a Si source gas, propane is used as a C source gas, and hydrogen is used as a carrier gas, wherein the hydrogen flow is 40slm, the C/Si ratio is 1.0, the growth temperature is 1520 ℃, and the growth time is 2 min.
Performing P-type crystal CuAlO on the intrinsic SiC homogeneous epitaxial layer in step 2 2 Growth of heteroepitaxial layers with Cu (NO) 3 ) 2 ·5H 2 O as Cu source, Al (NO) 3 ) 3 ·9H 2 Taking O as an Al source, taking polyvinyl alcohol PVA as a stabilizer, and carrying out P-type crystal CuAlO on an intrinsic SiC homogeneous epitaxial layer by adopting a sol-gel method 2 Growing the heteroepitaxial layer, specifically as follows:
step 3.1, preparing a solution: taking Cu (NO) according to a molar ratio of 1:1 respectively 3 ) 2 ·5H 2 O and Al (NO) 3 ) 3 ·9H 2 O to Cu (NO) 3 ) 2 ·5H 2 O and Al (NO) 3 ) 3 ·9H 2 Adding polyvinyl alcohol PVA and deionized water into the mixture of O to ensure that the concentration of the polyvinyl alcohol PVA in the solution is 0.05 mol/L;
step 3.2, heating and stirring the solution obtained in the step 3.1 in a water bath, controlling the temperature of the water bath to be 80 ℃, controlling the heating time to be 3 hours, and cooling to room temperature after heating to obtain sol;
3.3, spin-coating the sol prepared in the step 3.2 on an intrinsic SiC homogeneous epitaxial layer, wherein the spin-coating speed is controlled to be 2500rpm during spin-coating, the spin time is controlled to be 30s, and a sample obtained after spin-coating is subjected to heat treatment for 5min in an air environment, wherein the heat treatment temperature is 300 ℃;
step 3.4, after the heating treatment, after the sample is cooled to room temperature in the air, carrying out secondary spin coating and heat treatment, and controlling the prepared CuAlO by adjusting the repeated times of the spin coating and the heat treatment 2 The thickness of the heteroepitaxial layer;
step 3.5, placing the sample obtained after the spin coating and the heat treatment in an Ar gas environment for annealing treatment, wherein the annealing temperature is 900 ℃, and the annealing time is 4h to obtain p-type crystal CuAlO 2 A heteroepitaxial layer.
Step 4, adopting a magnetron sputtering method to perform P-type crystal CuAlO 2 And manufacturing a top electrode on the heteroepitaxial layer, which comprises the following steps:
step 4.1, taking Ti as a sputtering target material, and obtaining P-type crystal CuAlO in step 3 2 Sputtering the surface of the heteroepitaxial layer to form a Ti layer, wherein the sputtering time is controlled to be 0.1 hour, the pressure is controlled to be 0.1Pa, and the sputtering power is controlled to be 100 watts;
step 4.2, forming an Au layer on the surface of the Ti layer by sputtering with Au as a sputtering target material, controlling the sputtering time to be 0.1 hour, controlling the deposition pressure to be 2Pa and the sputtering power to be 10mW, and realizing the purpose of forming the P-type crystal CuAlO 2 A top electrode is prepared on the heteroepitaxial layer.
step 5.1, sputtering Ni serving as a target on the surface of the N-type SiC substrate on one surface on which the intrinsic SiC homogeneous epitaxial layer does not grow to form a Ni layer, wherein the sputtering time is controlled to be 0.1 hour, the pressure is controlled to be 0.1Pa, and the sputtering power is controlled to be 100 watts;
step 5.2, Au is used as a sputtering target material to form an Au layer on the surface of the Ni layer in a sputtering mode, the deposition time is controlled to be 0.1 hour, the deposition pressure is controlled to be 2Pa, the sputtering power is 10mW, the bottom electrode is prepared on the N-type SiC substrate, and finally CuAlO is obtained 2 the/SiC ultraviolet photodiode.
Example 2
The invention relates to CuAlO 2 The structure of the/SiC ultraviolet photodiode is shown in figure 1, and comprises a top electrode 1 and a bottom electrode 5, wherein P-type crystal CuAlO is sequentially arranged between the two electrodes from the top electrode 1 to the bottom electrode 5 2 A film 2, an I-type SiC film 3, and an N-type SiC substrate 4.
The top electrode 1 and the bottom electrode 5 are made of Au.
The N-type SiC substrate 4 is a nitrogen-doped SiC material; the type I crystal SiC film is an unintentionally doped SiC layer with the doping concentration of 10 15 cm ～3 。
P-type crystal CuAlO 2 The film 2 has a doping concentration of 10 18 cm ～3 。
CuAlO 2 The preparation method of the/SiC ultraviolet photodiode is shown in a flow chart of fig. 2 and is specifically implemented according to the following steps:
step 1, cleaning an N-type SiC substrate 4, and drying the cleaned N-type SiC substrate by blowing for later use;
step 4, obtaining P type crystal CuAlO in the step 3 2 Manufacturing a top electrode on the heteroepitaxial layer;
The cleaning process in the step 1 comprises the following steps: and cleaning the sample by using a cleaning solution, hydrofluoric acid, alcohol and deionized water in sequence.
When the intrinsic SiC homogeneous epitaxial layer is grown on the N-type SiC substrate 4 in the step 2, chemical vapor deposition equipment is utilized, silane is used as a Si source gas, propane is used as a C source gas, and hydrogen is used as a carrier gas, wherein the hydrogen flow is 60slm, the C/Si ratio is 1.5, the growth temperature is 1600 ℃, and the growth time is 5 min.
Performing P-type crystal CuAlO on the intrinsic SiC homogeneous epitaxial layer in step 2 2 Growth of heteroepitaxial layers with Cu (NO) 3 ) 2 ·5H 2 O as Cu source, Al (NO) 3 ) 3 ·9H 2 Taking O as an Al source, taking polyvinyl alcohol PVA as a stabilizer, and carrying out P-type crystal CuAlO on an intrinsic SiC homogeneous epitaxial layer by adopting a sol-gel method 2 Growing the heteroepitaxial layer, specifically as follows:
step 3.1, preparing a solution: taking Cu (NO) according to a molar ratio of 1:1 respectively 3 ) 2 ·5H 2 O and Al (NO) 3 ) 3 ·9H 2 O to Cu (NO) 3 ) 2 ·5H 2 O and Al (NO) 3 ) 3 ·9H 2 Adding polyvinyl alcohol PVA and deionized water into the mixture of O to ensure that the concentration of the polyvinyl alcohol PVA in the solution is 0.15 mol/L;
step 3.2, heating and stirring the solution obtained in the step 3.1 in a water bath, controlling the temperature of the water bath to be 90 ℃, controlling the heating time to be 5 hours, and cooling to room temperature after heating to obtain sol;
step 3.3, spin-coating the sol prepared in the step 3.2 on an intrinsic SiC homogeneous epitaxial layer, wherein the spin-coating speed is controlled to be 3000rpm and the spin time is 45s during spin-coating, and heat-treating a sample obtained after spin-coating in an air environment for 10min at the heat-treating temperature of 400 ℃;
Step 3.4, after the heating treatment, after the sample is cooled to room temperature in the air, carrying out secondary spin coating and heat treatment, and controlling the prepared CuAlO by adjusting the repeated times of the spin coating and the heat treatment 2 The thickness of the heteroepitaxial layer;
step 3.5 spin coating and heat treatingAfter finishing the treatment, the obtained sample is placed in an Ar gas environment for annealing treatment, the annealing temperature is 1100 ℃, the annealing time is 6 hours, and the p-type crystal CuAlO is obtained 2 A heteroepitaxial layer.
Step 4, adopting a magnetron sputtering method to perform P-type crystal CuAlO 2 And manufacturing a top electrode on the heteroepitaxial layer, which comprises the following steps:
step 4.1, taking Ti as a sputtering target material, and obtaining the P-type crystal CuAlO in the step 3 2 Sputtering the surface of the heteroepitaxial layer to form a Ti layer, wherein the sputtering time is controlled to be 2 hours, the pressure is controlled to be 10Pa, and the sputtering power is controlled to be 200 watts;
step 4.2, forming an Au layer on the surface of the Ti layer by sputtering with Au as a sputtering target material, controlling the sputtering time to be 2 hours, controlling the deposition pressure to be 4Pa and the sputtering power to be 20mW, and realizing the purpose of forming the CuAlO in the P-type crystal 2 And preparing a top electrode on the heteroepitaxial layer.
step 5.1, sputtering Ni serving as a target on the surface of the N-type SiC substrate on one surface on which the intrinsic SiC homogeneous epitaxial layer does not grow to form a Ni layer, wherein the sputtering time is controlled to be 2 hours, the pressure intensity is controlled to be 10Pa, and the sputtering power is controlled to be 200 watts;
And 5.2, sputtering Au serving as a sputtering target material on the surface of the Ni layer to form an Au layer, controlling the deposition time to be 2 hours, controlling the deposition pressure to be 4Pa and the sputtering power to be 20mW, thus realizing the preparation of the bottom electrode on the N-type SiC substrate and finally obtaining CuAlO 2 A SiC UV photodiode.
Example 3
The invention relates to CuAlO 2 The structure of the/SiC ultraviolet photodiode is shown in figure 1, and comprises a top electrode 1 and a bottom electrode 5, wherein P-type crystal CuAlO is sequentially arranged between the two electrodes from the top electrode 1 to the bottom electrode 5 2 A film 2, an I-type SiC film 3, and an N-type SiC substrate 4.
The top electrode 1 and the bottom electrode 5 are made of a mixture of metal materials of Ni, Cu and Pb.
The N-type SiC substrate 4 is a nitrogen-doped SiC material; the type I crystal SiC film is an unintentionally doped SiC layer with doping concentrationIs 10 15 cm ～3 。
P-type crystal CuAlO 2 The film 2 has a doping concentration of 10 18 cm ～3 。
CuAlO 2 The preparation method of the/SiC ultraviolet photodiode is shown in a flow chart of fig. 2 and is specifically implemented according to the following steps:
step 1, cleaning an N-type SiC substrate 4, and drying the cleaned N-type SiC substrate by blowing for later use;
step 4, obtaining P type crystal CuAlO in the step 3 2 Manufacturing a top electrode on the heteroepitaxial layer;
The cleaning process in the step 1 comprises the following steps: and cleaning the sample by using a cleaning solution, hydrofluoric acid, alcohol and deionized water in sequence.
When the intrinsic SiC homogeneous epitaxial layer is grown on the N-type SiC substrate 4 in the step 2, a chemical vapor deposition device is utilized, silane is used as an Si source gas, propane is used as a C source gas, and hydrogen is used as a carrier gas, wherein the hydrogen flow is 50slm, the C/Si ratio is 1.3, the growth temperature is 1580 ℃, and the growth time is 4 min.
Performing P-type crystal CuAlO on the intrinsic SiC homogeneous epitaxial layer in step 2 2 Growth of heteroepitaxial layers with Cu (NO) 3 ) 2 ·5H 2 O as Cu source, Al (NO) 3 ) 3 ·9H 2 Taking O as an Al source, taking polyvinyl alcohol PVA as a stabilizer, and carrying out P-type crystal CuAlO on an intrinsic SiC homogeneous epitaxial layer by adopting a sol-gel method 2 Growing the heteroepitaxial layer, specifically as follows:
step 3.1, preparing a solution: taking Cu (NO) according to a molar ratio of 1:1 respectively 3 ) 2 ·5H 2 O and Al (NO) 3 ) 3 ·9H 2 O to Cu (NO) 3 ) 2 ·5H 2 O and Al (NO) 3 ) 3 ·9H 2 Adding polyvinyl alcohol PVA and deionized water into the mixture of O to ensure that the concentration of the polyvinyl alcohol PVA in the solution is 0.1 mol/L;
Step 3.2, heating and stirring the solution obtained in the step 3.1 in a water bath, controlling the temperature of the water bath to be 85 ℃, controlling the heating time to be 4h, and cooling to room temperature after heating to obtain sol;
step 3.3, spin-coating the sol prepared in the step 3.2 on an intrinsic SiC homogeneous epitaxial layer, wherein the spin-coating speed is 2800rpm and the spin time is 40s during spin-coating, and heat-treating a sample obtained after spin-coating in an air environment for 8min at the heat-treatment temperature of 350 ℃;
step 3.4, after the heating treatment, after the sample is cooled to room temperature in the air, carrying out secondary spin coating and heat treatment, and controlling the prepared CuAlO by adjusting the repeated times of the spin coating and the heat treatment 2 The thickness of the heteroepitaxial layer;
step 3.5, placing the sample obtained after the spin coating and the heat treatment in an Ar gas environment for annealing treatment, wherein the annealing temperature is 1000 ℃, and the annealing time is 5 hours to obtain p-type crystal CuAlO 2 A heteroepitaxial layer.
Step 4, adopting a magnetron sputtering method to perform P-type crystal CuAlO 2 And manufacturing a top electrode on the heteroepitaxial layer, which comprises the following steps:
step 4.1, taking Ti as a sputtering target material, and obtaining the P-type crystal CuAlO in the step 3 2 Sputtering the surface of the heteroepitaxial layer to form a Ti layer, wherein the sputtering time is controlled to be 1 hour, the pressure intensity is controlled to be 5Pa, and the sputtering power is controlled to be 150 watts;
Step 4.2, forming an Au layer on the surface of the Ti layer by sputtering with Au as a sputtering target material, controlling the sputtering time to be 1 hour, controlling the deposition pressure to be 3Pa and the sputtering power to be 15mW, and realizing the purpose of forming the CuAlO in the P-type crystal 2 And preparing a top electrode on the heteroepitaxial layer.
step 5.1, sputtering Ni serving as a target on the surface of the N-type SiC substrate on one surface on which the intrinsic SiC homogeneous epitaxial layer does not grow to form a Ni layer, wherein the sputtering time is controlled to be 1 hour, the pressure intensity is controlled to be 0.1-10 Pa, and the sputtering power is controlled to be 150 watts;
and 5.2, sputtering Au serving as a sputtering target material on the surface of the Ni layer to form an Au layer, controlling the deposition time to be 1 hour, controlling the deposition pressure to be 3Pa and the sputtering power to be 18mW, thus realizing the preparation of the bottom electrode on the N-type SiC substrate and finally obtaining CuAlO 2 the/SiC ultraviolet photodiode.
Claims (10)
1. CuAlO 2 the/SiC ultraviolet photodiode is characterized by comprising a top electrode (1) and a bottom electrode (5), wherein P-type crystal CuAlO is sequentially arranged between the top electrode (1) and the bottom electrode (5) from the top electrode (1) to the bottom electrode (5) 2 A film (2), an I-type SiC film (3), and an N-type SiC substrate (4).
2. CuAlO according to claim 1 2 the/SiC ultraviolet photodiode is characterized in that the top electrode (1) and the bottom electrode (5) are made of one or a mixture of any of Au, Al, Ni, Cu and Pb metal materials, or are made of an alloy containing any of the mixed metal materials, or are made of an ITO conductive compound.
3. CuAlO according to claim 1 2 the/SiC ultraviolet photodiode is characterized in that the N-type SiC substrate (4) is a nitrogen-doped SiC material; the type I SiC film is an unintentionally doped SiC layer with the doping concentration of 10 15 cm -3 。
4. CuAlO according to claim 1 2 the/SiC ultraviolet photodiode is characterized in that the P-type crystal CuAlO 2 The film (2) has a doping concentration of 10 17 ～10 18 cm -3 。
5. CuAlO 2 The preparation method of the/SiC ultraviolet photodiode is characterized by comprising the following steps:
step 1, cleaning an N-type SiC substrate (4), and drying the cleaned substrate by blowing for later use;
step 2, growing an intrinsic SiC homogeneous epitaxial layer on the N-type SiC substrate (4) cleaned in the step 1;
step 3, performing P-type crystal CuAlO on the intrinsic SiC homogeneous epitaxial layer obtained in the step 2 2 Growing a heteroepitaxial layer;
step 4, obtaining P type crystal CuAlO in the step 3 2 Manufacturing a top electrode on the heteroepitaxial layer;
step 5, manufacturing a bottom electrode (5) on the lower surface of the N-type SiC substrate (4), and finally forming CuAlO 2 the/SiC ultraviolet photodiode.
6. CuAlO according to claim 5 2 The preparation method of the/SiC ultraviolet photodiode is characterized in that the cleaning process in the step 1 is as follows: and cleaning the sample by using a cleaning solution, hydrofluoric acid, alcohol and deionized water in sequence.
7. CuAlO according to claim 5 2 The preparation method of the/SiC ultraviolet photodiode is characterized in that when an intrinsic SiC homogeneous epitaxial layer is grown on the N-type SiC substrate (4) in the step 2, chemical vapor deposition equipment is utilized, silane is used as a Si source gas, propane is used as a C source gas, and hydrogen is used as a carrier gas, wherein the hydrogen flow is 40-60slm, the C/Si ratio is 1.0-1.5, the growth temperature is 1520-1600 ℃, and the growth time is 2-5 min.
8. CuAlO according to claim 5 2 The preparation method of the/SiC ultraviolet photodiode is characterized in that P-type crystal CuAlO is carried out on the intrinsic SiC homogeneous epitaxial layer in the step 3 2 Growth of heteroepitaxial layers with Cu (NO) 3 ) 2 ·5H 2 O as Cu source, Al (NO) 3 ) 3 ·9H 2 Taking O as an Al source, taking polyvinyl alcohol PVA as a stabilizer, and carrying out P-type crystal CuAlO on an intrinsic SiC homogeneous epitaxial layer by adopting a sol-gel method 2 And (3) growing the heteroepitaxial layer, specifically comprising the following steps:
step 3.1, preparing a solution: taking Cu (NO) respectively according to a molar ratio of 1:1 3 ) 2 ·5H 2 O and Al (NO) 3 ) 3 ·9H 2 O to Cu (NO) 3 ) 2 ·5H 2 O and Al (NO) 3 ) 3 ·9H 2 Adding polyvinyl alcohol PVA and deionized water into the mixture of O to ensure that the concentration of the polyvinyl alcohol PVA in the solution is 0.05 mol/L-0.15 mol/L;
step 3.2, heating and stirring the solution obtained in the step 3.1 in a water bath, controlling the temperature of the water bath to be 80-90 ℃, controlling the heating time to be 3-5 h, and cooling to room temperature after heating to obtain sol;
step 3.3, spin-coating the sol prepared in the step 3.2 on an intrinsic SiC homogeneous epitaxial layer, wherein the spin-coating speed is controlled to be 2500-3000 rpm during spin-coating, the spin time is controlled to be 30-45 s, and a sample obtained after spin-coating is subjected to heat treatment for 5-10 min in an air environment, wherein the heat treatment temperature is 300-400 ℃;
step 3.4, after the heating treatment, after the sample is cooled to room temperature in the air, carrying out secondary spin coating and heat treatment, and controlling the prepared CuAlO by adjusting the repeated times of the spin coating and the heat treatment 2 The thickness of the heteroepitaxial layer;
step 3.5, placing the sample obtained after the spin coating and the heat treatment in an Ar gas environment for annealing treatment, wherein the annealing temperature is 900-1100 ℃, and the annealing time is 4-6 h to obtain p-type crystal CuAlO 2 A heteroepitaxial layer.
9. CuAlO according to claim 8 2 The preparation method of the/SiC ultraviolet photodiode is characterized in that in the step 4, a magnetron sputtering method is adopted to perform P-type crystal CuAlO 2 And manufacturing a top electrode on the heteroepitaxial layer, which comprises the following steps:
step 4.1, taking Ti as a sputtering target material, and obtaining the P-type crystal CuAlO in the step 3 2 Sputtering the surface of the heteroepitaxial layer to form a Ti layer, wherein the sputtering time is controlled to be 0.1-2 hours, the pressure is controlled to be 0.1-10 Pa, and the sputtering power is controlled to be 100-200W;
step 4.2, sputtering Au as a sputtering target material to form an Au layer on the surface of the Ti layer, and sputteringThe emission time is controlled to be 0.1-2 hours, the deposition pressure is controlled to be 2-4 Pa, the sputtering power is 10-20 mW, and the P-type crystal CuAlO is realized 2 And preparing a top electrode on the heteroepitaxial layer.
10. CuAlO according to claim 9 2 The preparation method of the/SiC ultraviolet photodiode is characterized in that in the step 5, a bottom electrode (5) is manufactured on the lower surface of the N-type SiC substrate (4) by adopting a magnetron sputtering method, and the method specifically comprises the following steps:
step 5.1, sputtering Ni serving as a target on the surface of the N-type SiC substrate on one surface on which the intrinsic SiC homogeneous epitaxial layer does not grow to form a Ni layer, wherein the sputtering time is controlled to be 0.1-2 hours, the pressure intensity is controlled to be 0.1-10 Pa, and the sputtering power is controlled to be 100-200 watts;
And 5.2, sputtering Au serving as a sputtering target material on the surface of the Ni layer to form an Au layer, controlling the deposition time to be 0.1-2 hours, controlling the deposition pressure to be 2-4 Pa and the sputtering power to be 10-20 mW, namely preparing a bottom electrode on the N-type SiC substrate to finally obtain CuAlO 2 A SiC UV photodiode.
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