CN115084234A - Gallium oxide pn diode based on P-type doping concentration gradually changed from center to periphery and preparation method - Google Patents

Gallium oxide pn diode based on P-type doping concentration gradually changed from center to periphery and preparation method Download PDF

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CN115084234A
CN115084234A CN202210864505.7A CN202210864505A CN115084234A CN 115084234 A CN115084234 A CN 115084234A CN 202210864505 A CN202210864505 A CN 202210864505A CN 115084234 A CN115084234 A CN 115084234A
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gallium oxide
type semiconductor
semiconductor layer
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layer
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郑雪峰
洪悦华
张翔宇
何云龙
苑子健
马晓华
郝跃
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Xidian University
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Abstract

The invention discloses a gallium oxide Pn diode based on a structure with a P-type doping concentration gradually changed from the center to the periphery and a preparation method thereof, and mainly solves the problem that the reverse breakdown voltage of a device is improved and the forward on-resistance and power consumption of the device are seriously increased in the prior art. It from bottom to top includes: the high-density GaN-based high-voltage power semiconductor device comprises cathode ohmic metal (1), a GaN substrate (2), a GaN drift layer (3), a P-type semiconductor layer (4), a high-doping-concentration P-type semiconductor layer (5) and an anode (6), wherein the P-type semiconductor layer is formed by depositing a plurality of semiconductor materials with different doping concentrations on the GaN drift layer in sequence from the center to the periphery in a gradually increasing order, so that the peak electric field at the edge of the GaN drift layer and in the P-type semiconductor layer is reduced, good ohmic contact is formed at the same time, the device is reduced in on-resistance while reverse breakdown voltage is increased.

Description

Gallium oxide pn diode based on P-type doping concentration gradually changed from center to periphery and preparation method
Technical Field
The invention belongs to the technical field of semiconductor devices, and particularly relates to a method for manufacturing a gallium oxide pn diode, which can be used for electronic systems of communication, power electronics, signal processing and aerospace.
Technical Field
Gallium oxide is a novel ultra-wide bandgap semiconductor material, and the gallium oxide semiconductor material can be used for preparing a high-power device due to the characteristics of the wide bandgap of 4.6-4.9eV and the high critical breakdown field strength of 8 MV/cm. With the continuous progress of scientific technology, in the fields of communication, power electronics, signal processing, aerospace and the like, the performance of the traditional third-generation semiconductor GaN and SiC power devices cannot meet the requirement of higher working performance, and the gallium oxide power devices have lower on-resistance, lower power consumption and higher Bari plus merit figure under the same breakdown voltage.
At present, gallium oxide power devices mainly comprise diodes and triodes, wherein the diodes mainly comprise schottky diodes and heterojunction pn diodes. The pn diode is a p-n junction formed by a p-type semiconductor and an n-type semiconductor, forms space charge layers on both sides of the interface, is favorable for minority carrier operation, and is widely used for various rectifying circuits, detecting circuits, voltage stabilizing circuits and modulating circuits.
Due to the difficulty of achieving gallium oxide P-type doping, heterojunction pn-diodes are currently made mainly using other P-type semiconductor materials, such as nickel oxide, copper oxide, tin oxide in combination with n-type gallium oxide. Two very important device parameters for measuring the performance of a diode are reverse breakdown voltage and on-resistance, and the larger the reverse breakdown voltage is, or the smaller the on-resistance is, the better the performance of the device is. However, the forward characteristic and breakdown voltage of the gallium oxide diode at present are far from the limit of gallium oxide, and the barying plus optimum value BFOM of a gallium oxide device is far lower than an ideal value, so that the high-power output performance of the gallium oxide device is influenced, and the application of the gallium oxide device in the high-voltage field is limited.
Ma Xiao Hua et al, in patent document 202111069074.7 entitled "high breakdown voltage gallium oxide power diode and method for making same", propose to use thin NiO layer with P-type characteristic and beta-Ga 2 O 3 The drift layer forms a heterogeneous PN junction structure to reduce the peak electric field at the edge of the device, improve the interface characteristic of anode metal and gallium oxide, reduce reverse leakage current and improve the breakdown voltage of the gallium diode.
Luxing et al, in patent document 201710057175.X, a gallium oxide-based hetero PN junction diode and a method for manufacturing the same, propose to form a hetero PN junction by using an amorphous or polycrystalline p-type oxide semiconductor layer and a monocrystalline n-type doped gallium oxide voltage-resistant layer, so as to reduce reverse leakage current and improve the breakdown voltage of the gallium diode.
Although the two methods can improve the reverse breakdown voltage of the device, the forward on-resistance of the device is also seriously increased while the reverse breakdown voltage of the device is improved, and the barying optimum value of the device cannot be improved to the maximum.
Disclosure of Invention
The invention aims to provide a gallium oxide pn diode based on p-type doping concentration gradually changed from the center to the periphery and a preparation method thereof aiming at overcoming the defects of the prior art, so that the reverse breakdown voltage is improved, the on-resistance is reduced, and the barying plus merit value BFOM of a gallium oxide device is improved.
The technical idea of the invention is as follows: the p-type doping concentration of a p-type semiconductor layer in the pn junction is gradually changed from the center to the periphery, so that after the low-doped gallium oxide drift layer is contacted with the p-type semiconductor layer with the gradually changed doping concentration, the p-type semiconductor with high doping concentration at the periphery relieves the peak electric field at the edge of the gallium oxide drift layer and the p-type semiconductor with low doping concentration at the center relieves the peak electric field in the p-type semiconductor layer, and the breakdown voltage of the device is improved; meanwhile, ohmic contact is easier to form after the anode metal is contacted with the p-type semiconductor layer with high doping concentration, and the Bariga optimal value BFOM of the gallium oxide device is improved.
According to the above thought, the technical scheme of the invention is as follows:
1. a gallium oxide pn diode based on P-type doping concentration gradually changed from the center to the periphery comprises the following components from bottom to top: cathode ohmic metal, a gallium oxide substrate, a gallium oxide drift layer, a P-type semiconductor layer, a high-doping concentration P-type semiconductor layer and anode metal. The P-type semiconductor layer is a gradient doped P-type semiconductor layer formed by depositing multiple circles of semiconductor materials with different doping concentrations in a gradient manner from the center to the periphery in sequence from low to high, so that the reverse breakdown voltage of the device is improved, the on-resistance of the device is reduced, and the Bari plus optimum value of a gallium oxide device is improved.
Preferably, the thickness of the gradient doped P-type semiconductor layer is 5-30nm, and the gradient doping concentration ranges from 1 × 10 16 cm -3 Gradation to 1 × 10 19 cm -3 。
Preferably, the cathode ohmic metal is Ti/Au metal, the thickness of the first layer of Ti close to the gallium oxide substrate layer is 20-50nm, and the thickness of the second layer of Au metal is 100-400 nm;
preferably, the thickness of the gallium oxide substrate is 300-650 mu m, and the effective doping carrier concentration is 10 18 -10 20 cm -3 The doping ion species is Si ions or Sn ions.
Preferably, the gallium oxide drift layer has a thickness of 3 to 15 μm and a dopant carrier concentration of 10 16 -10 18 cm -3 。
Preferably, the P-type semiconductor material selectable in the gradually-doped P-type semiconductor layer and the high-doping-concentration P-type semiconductor layer comprises nickel oxide, copper oxide and tin oxide, the thickness of the high-doping-concentration P-type semiconductor layer is 3-20nm, and the doping carrier concentration is 10 19 -10 20 cm -3 。
Preferably, the anode metal is Ni/Au metal, the thickness of the first layer of metal Ni is 45-60nm, and the thickness of the second layer of metal Au is 200-400 nm.
2. A manufacturing method of a gallium oxide pn diode based on P-type doping concentration gradually changed from the center to the periphery is characterized by comprising the following steps:
1) sequentially cleaning the gallium oxide substrate by acetone-isopropanol-deionized water;
2) epitaxially forming a gallium oxide drift layer on the front side of the cleaned gallium oxide substrate by adopting a hydride vapor phase epitaxy technology (HVPE) method, depositing ohmic cathode metal on the back side by adopting magnetron sputtering in an argon atmosphere, and carrying out ohmic annealing on the ohmic cathode metal;
3) depositing a P-type semiconductor layer with gradually-changed doping concentration on the gallium oxide drift layer:
3a) performing primary photoetching on the front surface of the gallium oxide drift layer to form a circular pattern;
3b) setting the magnetron sputtering process conditions of 100-150W of power, 5-50 percent of oxygen to argon, 10-90 minutes of processing time, 4-10mtorr of pressure and 25 ℃ of ambient temperature;
3c) forming a circular P-type material with lower doping concentration by adopting magnetron sputtering deposition according to the circular pattern subjected to primary photoetching, and stripping off the P-type material deposited on the gallium oxide drift layer without the photoetching pattern;
3d) performing secondary photoetching on the front surface of the gallium oxide drift layer to form a circular ring pattern, increasing the proportion of oxygen to argon in a magnetron sputtering process, depositing a circular ring wrapping a circular P-type material deposited at the previous time by magnetron sputtering according to the circular ring pattern subjected to the secondary photoetching, wherein the P-type doping concentration is higher than that of the previous deposition, and stripping off the P-type material deposited at the position without the photoetching pattern on the gallium oxide drift layer;
3e) carrying out n times of photoetching on the front surface of the gallium oxide drift layer to form a ring pattern, improving the proportion of oxygen to argon in a magnetron sputtering process, depositing a ring wrapping a ring P-type material deposited by the previous n-1 deposition by adopting magnetron sputtering according to the ring pattern subjected to n times of photoetching, wherein the P-type doping concentration is higher than that of the previous n-1 deposition, and stripping off the P-type material deposited on the gallium oxide drift layer without the photoetching pattern; repeating the steps until the total width of the P-type material formed by deposition according to the photoetching pattern is equal to the width of the anode metal, forming a P-type semiconductor layer with doping concentration from the center to the periphery from low to high, wherein n is an integer greater than 2;
4) depositing a high-doping-concentration P-type semiconductor layer on the front surface of the P-type semiconductor layer with the doping concentration from the center to the periphery from low to high:
4a) forming a pattern on the front surface of the P-type semiconductor layer by adopting a photoetching process;
4b) setting magnetron sputtering process conditions: the power is 100-150W, the proportion of oxygen to argon is 50-80%, the processing time is 10-90 minutes, the pressure is 4-10mtorr, and the ambient temperature is 25 ℃;
4c) depositing a high-doping-concentration P-type semiconductor layer on the P-type semiconductor layer by magnetron sputtering according to the photoetching pattern under the process condition set in the step 4 b);
5) and forming an anode pattern on the front surface of the high-doping-concentration P-type semiconductor layer by adopting a photoetching process, and depositing anode metal by adopting electron beam evaporation according to the anode pattern to finish the manufacture of the device.
Compared with the traditional gallium oxide pn diode, the invention has the following advantages because the P-type semiconductor layer with gradually changed doping concentration from the center to the periphery is adopted:
firstly, after the peripheral high-doping-concentration semiconductors in the P-type semiconductor layer with the gradually-changed doping concentration from the center to the periphery contact with the edge of the gallium oxide drift layer, the peak electric field at the edge of the gallium oxide drift layer can be relieved, and the reverse breakdown voltage of the device is improved.
Secondly, the semiconductor with low doping concentration in the center of the P-type semiconductor layer with gradually changed doping concentration from the center to the periphery can relieve the internal peak electric field of the P-type semiconductor and improve the reverse breakdown voltage of the device.
Third, the high doping concentration p-type semiconductor layer can form excellent ohmic contact after contacting with the anode metal above the p-type semiconductor layer, thereby reducing the on-resistance.
Drawings
FIG. 1 is a schematic diagram of a prior art gallium oxide pn diode structure;
FIG. 2 is a schematic diagram of a gallium oxide pn diode with gradually changing P-type doping concentration from the center to the periphery according to the present invention;
FIG. 3 is a flow chart of an implementation of the present invention to fabricate the gallium oxide pn diode of FIG. 2.
The specific implementation mode is as follows:
in order to more clearly illustrate the technical solutions in the embodiments of the present invention, the present invention will be further described with reference to the embodiments and the accompanying drawings used in the technical description of the present invention. However, it will be apparent to one skilled in the art that the present invention may be practiced in other embodiments that depart from these specific details.
Referring to fig. 2, the gallium oxide pn diode based on the gradual change of P-type doping concentration from the center to the periphery of the invention comprises: the cathode ohmic metal 1, the gallium oxide substrate 2, the gallium oxide drift layer 3, the P-type semiconductor layer 4 with gradually-changed doping concentration, the P-type semiconductor layer 5 with high doping concentration and the anode metal 6. Wherein:
the cathode ohmic metal 1 is positioned on the back of the gallium oxide substrate 2, the metal is Ti/Au, the thickness of Ti is 20nm, and the thickness of Au is 400 nm;
the thickness of the gallium oxide substrate 2 is 650 μm, and the doping concentration thereof is 2 × 10 19 cm -3 ；
The gallium oxide drift layer 3 is arranged on the gallium oxide substrate 2, the thickness of the gallium oxide drift layer is 10 mu m, and the doping concentration of the gallium oxide drift layer is 1 multiplied by 10 16 cm -3 ；
The P-type semiconductor 4 with the gradually-changed doping concentration is positioned on the gallium oxide drift layer 3, and the doping concentration gradually increases from the center to the periphery by adopting NiO materials with various different doping concentrations, so that the reverse breakdown voltage of the device is improved, the on-resistance of the device is reduced, and the Bari plus optimum value of the gallium oxide device is improved. For example, three kinds of NiO materials with the thickness of 27nm can be adopted, wherein the doping concentration of the circular NiO material at the center is 1 multiplied by 10 18 cm -3 The doping concentration of the NiO material of the first inner ring is 5 multiplied by 10 18 cm -3 The doping concentration of the NiO material of the outer ring of the second circle is 1 multiplied by 10 19 cm -3 ；
The P-type semiconductor layer 5 with high doping concentration is positioned on the P-type semiconductor 4 with gradually changed doping concentration, the thickness of the P-type semiconductor layer is 5nm, and the doping concentrationIs 1 × 10 19 cm -3 ；
The anode metal 6 is positioned on the p-type semiconductor layer 5 with high doping concentration, the metal is Ni/Au, the thickness of Ni is 45nm, and the thickness of Au is 400 nm.
Referring to fig. 3, the present invention provides the following three embodiments for fabricating the device structure of fig. 2:
the first embodiment is as follows: and manufacturing a gallium oxide pn diode comprising a p-type semiconductor layer which is formed by three NiO materials with different doping concentrations and the doping concentration of which is gradually increased from the center to the periphery.
The method comprises the following steps: and cleaning the gallium oxide substrate.
The thickness is 650 mu m, and the effective doping carrier concentration is 10 18 cm -3 And a gallium oxide substrate 2 doped with Sn ions.
The mixture was sonicated for 5 minutes in sequence using acetone-isopropanol-deionized water, respectively, and then blown dry using nitrogen.
Step two: and growing a gallium oxide drift layer on the front surface of the cleaned gallium oxide substrate by adopting a Hydride Vapor Phase Epitaxy (HVPE) method.
Firstly, HCl reacts with high-purity metal Ga at the temperature of 850 ℃ in a high-temperature reaction zone of an HVPE vertical reactor to generate GaCl and GaCl 3 ；
Then, GaCl and GaCl generated in the high temperature reaction zone are reacted 3 Pushing into low temperature reaction zone, placing gallium oxide substrate 2 with its front side facing upwards in low temperature reaction zone of HVPE vertical reactor, and placing GaCl and GaCl on gallium oxide substrate 2 3 Reacting with oxygen at 600 deg.C to obtain a film with a thickness of 10 μm and a doping concentration of 1 × 10 16 cm -3 And a gallium oxide drift layer 3.
And step three, preparing cathode ohmic metal.
In the atmosphere of inert gas argon, a magnetron sputtering method is adopted, the power is set to be 100W, the sputtering time is set to be 40 minutes, the pressure is set to be 8mtorr, the ambient temperature is set to be 25 ℃, metal Ti/Au is deposited on the back surface of the gallium oxide substrate 2, the thickness of the first layer of metal Ti close to the gallium oxide substrate layer is 20nm, the thickness of the second layer of metal Au is 400nm, and the cathode ohm 1 is formed.
Step four: and annealing the cathode ohmic metal by using an annealing furnace under the nitrogen atmosphere, wherein the annealing temperature is 470 ℃ and the annealing time is 1 minute.
Step five: and depositing a P-type semiconductor layer with gradually changed doping concentration by magnetron sputtering.
Firstly, photoetching a gallium oxide drift layer 3 for the first time by using photoresist to prepare a circular pattern, carrying out magnetron sputtering on the circular pattern for 90 minutes under the process conditions of 150W of power, 33 percent of oxygen to argon, 10mtorr of pressure and 25 ℃ of ambient temperature to form the doping concentration of 1 multiplied by 10 18 cm -3 The central circular NiO material of (4); stripping NiO material deposited on the non-photoetching pattern position on the gallium oxide drift layer 3 by adopting an N-methyl pyrrolidone solution;
then, the photoresist is used for carrying out second photoetching on the gallium oxide drift layer 3 to prepare a circular ring pattern, and the circular ring pattern is subjected to magnetron sputtering for 90 minutes under the process conditions that the power is 150W, the proportion of oxygen to argon is 40%, the pressure is 10mtorr and the ambient temperature is 25 ℃ to form the doping concentration of 5 multiplied by 10 18 cm -3 The first ring of the NiO tube wraps the NiO ring of the central round material; stripping NiO material deposited on the non-photoetching pattern position on the gallium oxide drift layer 3 by adopting an N-methyl pyrrolidone solution;
finally, carrying out third photoetching on the gallium oxide drift layer 3 by using photoresist to prepare a new circular ring pattern, carrying out magnetron sputtering on the circular pattern for 90 minutes under the process conditions of 150W of power, 50 percent of oxygen to argon, 10mtorr of pressure and 25 ℃ of ambient temperature to form the doping concentration of 1 multiplied by 10 19 cm -3 The second ring wraps the NiO ring of the first ring material; and stripping the NiO material deposited on the non-photoetching pattern position on the gallium oxide drift layer 3 by adopting an N-methyl pyrrolidone solution, and forming a P-type semiconductor layer 4 with gradually increased doping concentration from the center to the periphery by using three kinds of NiO materials with different doping concentrations.
Step six: and depositing a p-type semiconductor layer 5 with high doping concentration by magnetron sputtering.
Firstly, preparing a pattern on a P-type semiconductor layer 4 with gradually-changed doping concentration by using a photoresist by utilizing a photoetching technology;
then, a P-type semiconductor 4 with a gradually changing doping concentration was formed with a doping concentration of 10 by magnetron sputtering according to the pattern of photolithography under the conditions of a power of 100W, a ratio of oxygen to argon of 50%, a pressure of 10mtorr, an ambient temperature of 25 ℃ and a processing time of 30 minutes 19 cm -3 The NiO material of (2);
and finally, stripping the NiO material deposited on the P-type semiconductor layer 4 without the photoetching pattern by adopting an N-methyl pyrrolidone solution to form the P-type semiconductor layer 5 with high doping concentration.
Step seven: the anode metal 6 is prepared.
Firstly, an anode pattern is prepared on a p-type semiconductor layer 5 with high doping concentration by using photoresist by utilizing a photoetching technology;
then, in an inert gas argon atmosphere, the power was set at 150W, the evaporation time was 40 minutes, and the degree of vacuum was 10 - 6 TORR, the ambient temperature is the process condition of 25 ℃, adopt the evaporation method of electron beam to deposit metal Ni/Au on the positive pole pattern, and the thickness of the first layer of metal Ni is 45nm, the thickness of the second layer of metal Au is 400 nm;
and finally, washing off the photoresist by adopting an N-methylpyrrolidone solution and stripping to finish the manufacture of the device.
Example two: and manufacturing a gallium oxide pn diode containing a p-type semiconductor layer with gradually-changed doping concentration from the center to the periphery, wherein the p-type semiconductor layer is formed by four copper oxide materials with different doping concentrations.
Step 1: and cleaning the gallium oxide substrate.
The thickness is 450 μm, and the effective doping carrier concentration is 10 18 cm -3 And the gallium oxide substrate with the doping ion species of Sn ions is subjected to ultrasonic treatment for 5 minutes by using acetone-isopropanol-deionized water respectively, and then is dried by using nitrogen.
And 2, step: and growing a gallium oxide drift layer on the front surface of the cleaned gallium oxide substrate by adopting a Hydride Vapor Phase Epitaxy (HVPE) method.
2.1) in HIn the high-temperature reaction zone of the VPE vertical reactor, HCl and high-purity metal Ga react at the temperature of 850 ℃ to generate GaCl and GaCl 3 ；
2.2) GaCl and GaCl formed in the high temperature reaction zone 3 Pushing into low temperature reaction zone, placing gallium oxide substrate 2 with its front side facing upwards in low temperature reaction zone of HVPE vertical reactor, and placing GaCl and GaCl on gallium oxide substrate 2 3 Reacting with oxygen at 600 deg.C to obtain a product with thickness of 4 μm and doping concentration of 2 × 10 16 cm -3 And a gallium oxide drift layer 3.
And 3, preparing cathode ohmic metal.
In the atmosphere of inert gas argon, a magnetron sputtering method is adopted, the sputtering power is set to be 100W, the time is set to be 30 minutes, the pressure is set to be 6mtorr, the ambient temperature is set to be 25 ℃, metal Ti/Au is deposited on the back surface of the gallium oxide substrate 2, the thickness of the first layer of metal Ti close to the gallium oxide substrate layer is 20nm, the thickness of the second layer of metal Au is 300nm, and the cathode ohm 1 is formed.
And 4, step 4: the cathode ohmic metal was annealed at 470 deg.c for 1 minute using an annealing furnace under a nitrogen atmosphere.
And 5: and depositing a P-type semiconductor layer 4 with the gradient doping concentration by magnetron sputtering.
5.1) carrying out first photoetching on the gallium oxide drift layer 3 by using photoresist to prepare a circular pattern; setting the technological conditions of 150W of power, 33 percent of oxygen to argon, 10mtorr of pressure and 25 ℃ of ambient temperature, carrying out magnetron sputtering on the circular pattern for 80 minutes to form the doping concentration of 1 multiplied by 10 18 cm -3 The central circular copper oxide material of (2); stripping the copper oxide material deposited on the non-photoetching pattern position on the gallium oxide drift layer 3 by adopting an acetone organic solution;
5.2) carrying out second photoetching on the gallium oxide drift layer 3 by using the photoresist to prepare a first circular ring pattern, carrying out magnetron sputtering on the circular pattern for 80 minutes under the process conditions that the power is 150W, the proportion of oxygen to argon is 40%, the pressure is 10mtorr and the ambient temperature is 25 ℃ to form the doping concentration of 5 multiplied by 10 18 cm -3 The first circle of wrapping centerA copper oxide ring of circular material; stripping the copper oxide material deposited on the gallium oxide drift layer 3 without photoetching patterns by using an acetone organic solution;
5.3) carrying out third photoetching on the gallium oxide drift layer 3 by using the photoresist to prepare a second circular ring pattern, carrying out magnetron sputtering on the second circular ring pattern for 80 minutes under the process conditions that the power is 150W, the oxygen-argon ratio is 45 percent, the pressure is 10mtorr and the ambient temperature is 25 ℃ to form the doping concentration of 8 multiplied by 10 18 cm -3 The second ring of copper oxide rings wraps the first ring of copper oxide rings; stripping the copper oxide material deposited on the gallium oxide drift layer 3 without photoetching patterns by using an acetone organic solution;
5.4) carrying out fourth photoetching on the gallium oxide drift layer 3 by using the photoresist to prepare a third circular ring pattern, setting the process conditions of 150W of power, 50 percent of oxygen to argon, 10mtorr of pressure and 25 ℃ of ambient temperature, carrying out magnetron sputtering on the third circular ring for 80 minutes to form the doping concentration of 1 multiplied by 10 19 cm -3 The third ring of the copper oxide ring wraps the second ring of the ring material; and stripping the copper oxide material deposited on the gallium oxide drift layer 3 without the photoetching pattern by adopting an acetone organic solution to obtain a P-type semiconductor layer 4 with gradually increased doping concentration from the center to the periphery, wherein the four copper oxide materials with different doping concentrations form the P-type semiconductor layer.
Step 6: and depositing a p-type semiconductor layer 5 with high doping concentration by magnetron sputtering.
6.1) preparing a pattern on the P-type semiconductor layer 4 with the gradually-changed doping concentration by using a photoetching technology;
6.2) forming a doping concentration of 5X 10 on the P-type semiconductor 4 with a graded doping concentration by magnetron sputtering according to a photoetching pattern under the conditions of a power of 100W, a ratio of oxygen to argon of 60%, a pressure of 10mtorr, an ambient temperature of 25 ℃ and a processing time of 30 minutes 19 cm -3 Copper oxide material of (a); and stripping the copper oxide material deposited on the non-photoetching pattern part on the P-type semiconductor 4 by adopting an N-methyl pyrrolidone solution.
And 7: the anode metal 6 is prepared.
7.1) preparing an anode pattern on the p-type semiconductor layer 5 with high doping concentration by using photoresist by utilizing a photoetching technology;
7.2) setting the power at 150W, the evaporation time at 20 minutes and the vacuum degree at 3X 10 in an inert gas argon atmosphere -6 TORR, the process condition that the ambient temperature is 25 ℃, adopting an electron beam evaporation method to sequentially deposit metal Ni with the thickness of 45nm and metal Au with the thickness of 200nm on the anode pattern;
and 7.3) washing off the photoresist by adopting an N-methyl pyrrolidone solution and stripping off the metal on the anode pattern which is not formed, thereby completing the preparation of the device.
Example three: and manufacturing a gallium oxide pn diode containing a p-type semiconductor layer which is composed of five NiO materials with different doping concentrations and has the doping concentration gradually changed from the center to the periphery.
Step A, cleaning a gallium oxide substrate:
A1) the thickness of the selected gallium oxide substrate is 300 mu m, and the effective doping carrier concentration is 10 19 cm -3 The doping ion species is Sn ions;
A2) the mixture was sonicated in sequence using acetone-isopropanol-deionized water for 5 minutes in sonication, and then blown dry using nitrogen.
B, growing a gallium oxide drift layer on the front surface of the cleaned gallium oxide substrate by adopting a hydride vapor phase epitaxy technology HVPE method:
B1) reacting HCl with high purity metal Ga at 850 ℃ in a high temperature reaction zone of an HVPE vertical reactor to produce GaCl and GaCl 3 ；
B2) Reacting GaCl and GaCl generated in the high-temperature reaction zone 3 Pushing into low temperature reaction zone, placing gallium oxide substrate 2 with its front side facing upwards in low temperature reaction zone of HVPE vertical reactor, and placing GaCl and GaCl on gallium oxide substrate 2 3 Reacting with oxygen at 650 deg.C to obtain a doped carrier with a thickness of 6 μm and a concentration of 10 17 m -3 And a gallium oxide drift layer 3.
And step C, preparing cathode ohmic metal.
In an inert gas argon atmosphere, setting the process conditions of 100W of power, 35 minutes of sputtering time, 10mtorr of pressure and 25 ℃ of ambient temperature, and adopting a magnetron sputtering method to sequentially deposit Ti with the thickness of 20nm and Au with the thickness of 350nm on the back surface of the gallium oxide substrate 2 to form a cathode ohm 1.
And D, annealing the cathode ohmic metal for 1 minute at the temperature of 500 ℃ in the nitrogen atmosphere by using an annealing furnace.
Step E, depositing a P-type semiconductor layer 4 with gradient doping concentration by magnetron sputtering:
E1) performing first photoetching on the gallium oxide drift layer 3 by using photoresist to prepare a circular pattern, and performing magnetron sputtering on the circular pattern for 60 minutes under the process conditions of 150W of power, 10 percent of oxygen to argon, 10mtorr of pressure and 25 ℃ of ambient temperature to form the doping concentration of 1 multiplied by 10 17 cm -3 The central circular NiO material of (1); stripping NiO material deposited on the non-photoetching pattern position on the gallium oxide drift layer 3 by adopting an N-methyl pyrrolidone solution;
E2) performing second photoetching on the gallium oxide drift layer 3 by using photoresist to prepare a first circular ring pattern, setting the process conditions of 150W of power, 33 percent of oxygen to argon, 10mtorr of pressure and 25 ℃ of ambient temperature, performing magnetron sputtering on the first circular ring pattern for 60 minutes to form the gallium oxide drift layer with the doping concentration of 1 multiplied by 10 18 cm -3 The first ring of the NiO tube wraps the NiO ring of the central round material; stripping NiO material deposited on the non-photoetching pattern position on the gallium oxide drift layer 3 by adopting an N-methyl pyrrolidone solution;
E3) carrying out third photoetching on the gallium oxide drift layer 3 by using photoresist to prepare a second circular ring pattern, setting the power to be 150W, the proportion of oxygen to argon to be 40 percent, the pressure to be 10mtorr and the ambient temperature to be 25 ℃, carrying out magnetron sputtering on the second circular ring pattern for 60 minutes to form the doping concentration of 5 multiplied by 10 18 cm -3 The second ring wraps the NiO ring of the first ring material; stripping NiO material deposited on the non-photoetching pattern position on the gallium oxide drift layer 3 by adopting an N-methyl pyrrolidone solution;
E4) performing a fourth photolithography on the gallium oxide drift layer 3 by using the photoresist to prepare a secondSetting the power of the three circular ring patterns to be 150W, the oxygen to argon ratio to be 45 percent, the pressure to be 10mtorr and the ambient temperature to be 25 ℃, carrying out magnetron sputtering on the third circular ring pattern for 80 minutes to form the doping concentration of 8 multiplied by 10 18 cm -3 The third circle of the NiO ring wraps the second circle of the ring material; stripping off NiO material deposited on the non-photoetching pattern position on the gallium oxide drift layer 3 by adopting an N-methyl pyrrolidone solution;
E5) performing fifth photoetching on the gallium oxide drift layer 3 by using photoresist to prepare a fourth circular ring pattern, setting the power to be 150W, the proportion of oxygen to argon to be 50 percent, the pressure to be 10mtorr and the ambient temperature to be 25 ℃, performing magnetron sputtering on the fourth circular ring pattern for 60 minutes to form the doping concentration to be 1 multiplied by 10 19 cm -3 The fourth circle of the NiO-shaped ring wraps the NiO ring of the third circle of ring material; and stripping the NiO material deposited on the non-photoetching pattern position on the gallium oxide drift layer 3 by adopting an N-methyl pyrrolidone solution to obtain a P-type semiconductor layer 4 with gradually increased doping concentration from the center to the periphery, wherein the NiO material is formed by five kinds of NiO materials with different doping concentrations.
Step F: and (3) magnetron sputtering deposition of the p-type semiconductor layer 5 with high doping concentration:
F1) preparing a pattern on the P-type semiconductor 4 with the gradually-changed doping concentration by using a photoresist by utilizing a photoetching technology;
F2) forming a doping concentration of 1 × 10 on the P-type semiconductor 4 with a gradient doping concentration by magnetron sputtering according to a photolithographic pattern under the conditions of a power of 100W, a proportion of oxygen to argon of 70%, a pressure of 10mtorr, an ambient temperature of 25 ℃ and a processing time of 30 minutes 20 cm -3 The NiO material of (1);
F3) and stripping the NiO material deposited on the P-type semiconductor layer 4 without the photoetching pattern by adopting an acetone organic solution to form a P-type semiconductor layer 5 with high doping concentration.
Step G, preparing anode metal:
G1) preparing an anode pattern on the high-doping-concentration p-type semiconductor layer 5 by using a photoresist by using a photolithography technique;
G2) in the atmosphere of inert gas argon gas,setting power 200W, time 30 minutes and vacuum degree 5X 10 - 6 TORR, the ambient temperature is the process condition of 25 ℃, adopting electron beam evaporation to deposit anode metal Ni/Au on the anode pattern, and the thickness of the first layer of metal Ni is 45nm, and the thickness of the second layer of metal Au is 300 nm;
G3) and (5) washing off the photoresist by adopting an N-methyl pyrrolidone solution and stripping to finish the preparation of the device.
The foregoing description is only three specific examples of the present invention and is not intended to limit the present invention in any way, and it will be apparent to those skilled in the art that various modifications and variations in form and detail can be made without departing from the principles and structure of the present invention, for example, the number of rings of P-type semiconductor with graded doping concentration is not limited to the number of rings in the three examples of the present invention, and more rings can be deposited; the P-type semiconductor with the gradually-changed doping concentration can be not only in a ring shape, but also in a square ring shape; the preparation method of the p-type semiconductor is not limited to magnetron sputtering, and any one of chemical vapor deposition process methods of metal organic compounds can be used; the preparation method of the anode metal is not limited to electron beam evaporation, and any one of methods such as magnetron sputtering, thermal evaporation and the like can be used; the cathode ohmic metal preparation method is not limited to magnetron sputtering, and any one of electron beam evaporation or thermal evaporation can be used, but such modifications and changes based on the idea of the present invention are still within the protection scope of the claims of the present invention.

Claims (10)

1. A gallium oxide pn diode based on P-type doping concentration gradually changed from the center to the periphery comprises the following components from bottom to top: the solar cell comprises cathode ohmic metal (1), a gallium oxide substrate (2), a gallium oxide drift layer (3), a P-type semiconductor layer (4), a high-doping-concentration P-type semiconductor layer (5) and anode metal (6). The gallium oxide-based semiconductor device is characterized in that the P-type semiconductor layer (4) is a gradient doped P-type semiconductor layer formed by depositing multiple circles of semiconductor materials with different doping concentrations in a gradient manner from the center to the periphery in sequence from low to high, so that the reverse breakdown voltage of the device is improved, the on-resistance of the device is reduced, and the Bari plus optimum value of the gallium oxide device is improved.
2. The diode of claim 1, wherein said graded doped P-type semiconductor layer has a thickness of 5-30nm and a graded doping concentration ranging from 1 x 10 16 cm -3 Gradation to 1 × 10 19 cm -3 。
3. The diode of claim 1, wherein:
the cathode ohmic metal (1) is Ti/Au metal, the thickness of the first layer of Ti close to the gallium oxide substrate layer is 20-50nm, and the thickness of the second layer of Au metal is 100-400 nm;
the thickness of the gallium oxide substrate (2) is 300-650 mu m, and the effective doping carrier concentration is 10 18 -10 20 cm -3 The doping ion species is Si ions or Sn ions.
The gallium oxide drift layer (3) has a thickness of 3-15 μm and a doped carrier concentration of 10 16 -10 18 cm -3 。
4. The diode of claim 1, wherein the optional P-type semiconductor material of the graded doped P-type semiconductor layer (4) and the heavily doped P-type semiconductor layer (5) comprises nickel oxide, copper oxide and tin oxide, the heavily doped P-type semiconductor layer (5) has a thickness of 3-20nm and a dopant carrier concentration of 10 19 -10 20 cm -3 。
5. The diode according to claim 1, wherein the anode metal (6) is Ni/Au metal, and the thickness of the first layer of Ni metal is 45-60nm, and the thickness of the second layer of Au metal is 200-400 nm.
6. A manufacturing method of a gallium oxide pn diode based on P-type doping concentration gradually changed from the center to the periphery is characterized by comprising the following steps:
1) sequentially cleaning the gallium oxide substrate (2) by acetone-isopropanol-deionized water;
2) epitaxially forming a gallium oxide drift layer (3) on the front surface of the cleaned gallium oxide substrate (2) by adopting a hydride vapor phase epitaxy technology (HVPE) method, depositing ohmic cathode metal (1) on the back surface by adopting magnetron sputtering in an argon atmosphere, and carrying out ohmic annealing on the ohmic cathode metal (1);
3) depositing a graded doping concentration P-type semiconductor layer (4) on the gallium oxide drift layer (3):
3a) performing primary photoetching on the front surface of the gallium oxide drift layer (3) to form a circular pattern;
3b) setting the magnetron sputtering process conditions of 100-150W of power, 5-50 percent of oxygen to argon, 10-90 minutes of processing time, 4-10mtorr of pressure and 25 ℃ of ambient temperature;
3c) forming a circular P-type material with lower doping concentration by adopting magnetron sputtering deposition according to the circular pattern subjected to primary photoetching, and stripping off the P-type material deposited on the gallium oxide drift layer (3) at the position without the photoetching pattern;
3d) carrying out secondary photoetching on the front surface of the gallium oxide drift layer (3) to form a circular ring pattern, improving the proportion of oxygen to argon in a magnetron sputtering process, depositing a circular ring wrapping a circular P-type material deposited at the previous time by adopting magnetron sputtering according to the circular ring pattern subjected to secondary photoetching, wherein the P-type doping concentration of the circular ring is higher than that of the circular ring deposited at the previous time, and stripping off the P-type material deposited at the position without the photoetching pattern on the gallium oxide drift layer (3);
3e) carrying out n times of photoetching on the front surface of the gallium oxide drift layer (3) to form a ring pattern, improving the proportion of oxygen to argon in a magnetron sputtering process, depositing a ring wrapping a ring P-type material deposited by the previous n-1 by adopting magnetron sputtering according to the ring pattern subjected to n times of photoetching, wherein the P-type doping concentration of the ring is higher than that of the previous n-1, and stripping off the P-type material deposited on the gallium oxide drift layer (3) at a position without the photoetching pattern; repeating the steps until the total width of the P-type material formed by deposition according to the photoetching pattern is equal to the width of the anode metal (6), forming a P-type semiconductor layer (4) with doping concentration from the center to the periphery from low to high, wherein n is an integer larger than 2;
4) depositing a high-doping-concentration P-type semiconductor layer (5) on the front surface of the P-type semiconductor layer (4) with the doping concentration from the center to the periphery from low to high:
4a) forming a pattern on the front surface of the P-type semiconductor layer (4) by adopting a photoetching process;
4b) setting magnetron sputtering process conditions: the power is 100-150W, the proportion of oxygen to argon is 50-80%, the processing time is 10-90 minutes, the pressure is 4-10mtorr, and the ambient temperature is 25 ℃;
4c) depositing a high-doping-concentration P-type semiconductor layer (5) on the P-type semiconductor layer (4) by magnetron sputtering according to the set process conditions of 4b) according to the photoetching pattern;
5) and forming an anode pattern on the front surface of the high-doping-concentration P-type semiconductor layer (5) by adopting a photoetching process, and depositing anode metal (6) by adopting electron beam evaporation according to the anode pattern to finish the manufacture of the device.
7. The method according to claim 6, characterized in that, in the step 2), a Hydride Vapor Phase Epitaxy (HVPE) method is adopted to epitaxially and lightly dope gallium oxide on the front surface of the cleaned gallium oxide substrate (2) to form the gallium oxide drift layer (3), and the following is realized:
in the atmosphere of ammonia gas, HCl and high-purity metal Ga are reacted at the temperature of 800-900 ℃ in a high-temperature reaction zone of an HVPE vertical reactor to generate GaCl and GaCl 3 ；
Reacting GaCl and GaCl generated in the high-temperature reaction zone 3 Pushing the substrate into a low-temperature reaction area, placing the cleaned gallium oxide substrate (2) in the HVPE vertical reactor with the front surface facing upwards in the low-temperature reaction area, and placing GaCl and GaCl on the gallium oxide substrate (2) 3 Reacting with oxygen at 650 deg.C, by changing GaCl and GaCl 3 The volume ratio of the carrier to oxygen is controlled to 10 16 -10 18 cm -3 And epitaxially forming a lightly doped gallium oxide drift layer (3).
8. The method as claimed in claim 6, wherein the ohmic cathode metal (1) is deposited on the back surface of the gallium oxide substrate (2) in step 2) by magnetron sputtering, the gallium oxide substrate (2) is placed in a magnetron sputtering apparatus with the back surface facing upwards, the power is set at 300W, the sputtering time is 30-90 minutes, the pressure is 6-12mtorr, and the ambient temperature is 25 ℃ under the process conditions of inert gas argon atmosphere, and the ohmic cathode metal (1) is deposited on the back surface of the gallium oxide substrate (2).
9. The method as claimed in claim 6, wherein the annealing of the ohmic cathode metal (1) in step 2) is performed under a nitrogen atmosphere at an annealing temperature of 400-500 ℃ for an annealing time of 1-3 minutes.
10. The method according to claim 6, characterized in that the electron beam evaporation in step 5) deposits the anodic metal (6) as follows:
the high-doping concentration P-type semiconductor layer (5) is arranged in an electron beam evaporation instrument with the right side facing upwards, the power is 150-350W in the inert gas argon atmosphere, the evaporation time is 40-100 minutes, and the vacuum degree is 10 -6 -10 -7 And TORR, under the process condition that the ambient temperature is 25 ℃, depositing anode metal (6) on the front surface of the high-doping-concentration P-type semiconductor layer (5) by adopting electron beam evaporation.
CN202210864505.7A 2022-07-21 2022-07-21 Gallium oxide pn diode based on P-type doping concentration gradually changed from center to periphery and preparation method Pending CN115084234A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117219677A (en) * 2023-10-11 2023-12-12 杭州致善微电子科技有限公司 Limiting diode with anode concentration gradient linear distribution and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117219677A (en) * 2023-10-11 2023-12-12 杭州致善微电子科技有限公司 Limiting diode with anode concentration gradient linear distribution and preparation method thereof
CN117219677B (en) * 2023-10-11 2024-02-23 杭州致善微电子科技有限公司 Limiting diode with anode concentration gradient linear distribution and preparation method thereof

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