CN113231386A - Method for removing gallium nitride surface pollutants and gallium nitride substrate - Google Patents

Method for removing gallium nitride surface pollutants and gallium nitride substrate Download PDF

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CN113231386A
CN113231386A CN202110424840.0A CN202110424840A CN113231386A CN 113231386 A CN113231386 A CN 113231386A CN 202110424840 A CN202110424840 A CN 202110424840A CN 113231386 A CN113231386 A CN 113231386A
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gallium nitride
sample
soaking
solution
surface contaminants
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刘婷
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Nanjing Naco Semiconductor Co ltd
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Nanjing Naco Semiconductor Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/02—Cleaning by the force of jets or sprays
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
    • B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
    • B08B7/0064—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes
    • B08B7/0071—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes by heating
    • B08B7/0085—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes by heating by pyrolysis
    • 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
    • H01L21/02041—Cleaning
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
    • H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
    • H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
    • H01L29/20—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only AIIIBV compounds
    • H01L29/2003—Nitride compounds

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  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • General Physics & Mathematics (AREA)
  • Computer Hardware Design (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
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  • General Chemical & Material Sciences (AREA)
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Abstract

The invention provides a method for removing gallium nitride surface pollutants and a gallium nitride substrate, belonging to the technical field of semiconductors, wherein the method for removing the gallium nitride surface pollutants comprises the following steps: immersing a pre-cleaned gallium nitride sample into cleaning solution for soaking, wherein the cleaning solution is mixed solution of hydrogen peroxide and alkali liquor; taking out, washing and drying the gallium nitride sample after soaking; and carrying out heat treatment on the dried gallium nitride sample in a mixed atmosphere, wherein the mixed atmosphere consists of nitrogen, hydrogen and ammonia. According to the invention, silicon pollutants on the surface of gallium nitride are etched by the mixed solution of hydrogen peroxide and alkali liquor, and a uniform compact oxide film is formed, so that the surface of gallium nitride is prevented from being polluted by silicon impurities in the air again; and then the gallium nitride sample is processed in a mixed atmosphere, so that an oxide film on the surface of the gallium nitride can be decomposed, and an atomic-level clean gallium nitride surface is obtained, thereby facilitating the subsequent secondary epitaxial growth, reducing the leakage current phenomenon and improving the reliability of a gallium nitride device.

Description

Method for removing gallium nitride surface pollutants and gallium nitride substrate
Technical Field
The invention belongs to the technical field of semiconductors, and particularly relates to a method for removing pollutants on the surface of gallium nitride.
Background
Gallium nitride belongs to a III-V group wide bandgap semiconductor material, the forbidden band width of the gallium nitride can reach 3.4eV, and the gallium nitride has high breakdown electric field intensity, high electron saturation velocity, high thermal conductivity, strong corrosion resistance and strong irradiation resistance. Therefore, compared with the traditional silicon-based semiconductor, the gallium nitride material is more suitable for manufacturing high-frequency and high-power devices with high temperature resistance, high voltage resistance and high current resistance, and can be widely applied to the fields of semiconductor illumination, 5G communication, new energy automobiles, satellite communication, optical communication, power electronics, aerospace and the like.
However, many dangling bonds exist on the surface of gallium nitride, when the gallium nitride is exposed in air, impurities such as silicon, oxygen, carbon and the like are inevitably adsorbed, an organic siloxane pollution layer with the thickness of about 1nm is formed, and the application of the gallium nitride material is influenced by the existence of the organic siloxane pollution layer.
In the process of implementing the invention, the inventor finds that the prior art has at least the following defects.
The existing treatment method is to adopt the traditional silicon-based semiconductor cleaning method to remove the pollution layer, although the method can temporarily remove silicon, oxygen and carbon impurities, when the surface of gallium nitride is exposed to the air again, impurities are adsorbed for the second time to form the siloxane pollution layer. When optical and electronic devices are grown on the contaminated gallium nitride material by secondary epitaxy, a silicon contamination layer remained on a secondary epitaxy interface can form a conductive layer, so that electric leakage and breakdown of the device are caused, and the device is failed.
Disclosure of Invention
Based on the background problem, the invention aims to provide a method for removing pollutants on the surface of gallium nitride, which can eliminate a pollution layer on the surface of the gallium nitride, improve the electric leakage condition of a secondary epitaxial interface of a gallium nitride electronic device and improve the reliability of the device; it is another object of the present invention to provide a gallium nitride substrate treated by the above method.
In order to achieve the above object, on one hand, the embodiment of the present invention provides a technical solution:
the method for removing the gallium nitride surface pollutants comprises the following steps:
immersing a pre-cleaned gallium nitride sample into cleaning solution for soaking, wherein the cleaning solution is mixed solution of hydrogen peroxide and alkali liquor;
taking out, washing and drying the gallium nitride sample after soaking;
and carrying out heat treatment on the dried gallium nitride sample in a mixed atmosphere, wherein the mixed atmosphere consists of nitrogen, hydrogen and ammonia.
Further, the gallium nitride sample is sequentially cleaned by adopting acetone, methanol and isopropanol to realize the pre-cleaning of the gallium nitride sample.
Further, the alkali liquor is potassium hydroxide solution or sodium hydroxide solution.
Furthermore, the molar ratio of hydrogen peroxide to alkali liquor in the cleaning solution is 3.26-4.52: 1.
Further, the soaking time is 30-60 min.
Further, ultrasonic water bath heating is simultaneously used in the soaking process, and the heating temperature is 70-95 ℃.
Further, the ultrasonic frequency is 20KHz-40 KHz.
And further, washing with deionized water for 5-10min, and drying with nitrogen after washing.
Further, the heat treatment temperature is 1000-.
According to the invention, the gallium nitride sample is treated by the mixed solution of hydrogen peroxide and alkali liquor, so that not only can silicon pollutants on the surface of gallium nitride be etched, but also a uniform compact oxide film can be formed, and the surface of gallium nitride is prevented from being directly exposed in the air, thereby preventing the surface of gallium nitride from being polluted by silicon impurities in the air again.
According to the invention, a gallium nitride sample is subjected to heat treatment in a mixed atmosphere, wherein the mixed atmosphere consists of nitrogen, hydrogen and ammonia, the ammonia is used for preventing gallium nitride from being thermally decomposed at high temperature, and the hydrogen and the nitrogen are carriers of the ammonia.
The invention controls the mol ratio of hydrogen peroxide to alkali liquor in the cleaning solution to be 3.26-4.52:1, and when the addition amount of hydrogen peroxide is too much and the addition amount of alkali liquor is too little, the oxide on the surface of gallium nitride can be insufficiently dissolved; when the addition amount of hydrogen peroxide is too small and the addition amount of alkali liquor is too large, the surface of gallium nitride is over-etched, and the surface is rough.
The invention controls the heat treatment temperature to be 1000-1100 ℃ and the time to be 5-15min, and can ensure that the oxide film on the surface of the gallium nitride can be completely decomposed within the temperature and time range.
In another aspect, an embodiment of the present invention provides a gallium nitride substrate for secondary epitaxial growth, which is obtained by the above-mentioned method.
The gallium nitride substrate has an atomically clean surface, and can reduce the leakage current and improve the reliability of a gallium nitride device when used for secondary epitaxial growth.
Compared with the prior art, the invention has the following effects:
according to the invention, the gallium nitride sample is treated by the mixed solution of hydrogen peroxide and alkali liquor, so that not only can silicon pollutants on the surface of gallium nitride be etched, but also a uniform compact oxide film can be formed, the surface of gallium nitride is prevented from being directly exposed in the air, and the surface of gallium nitride is prevented from being polluted by silicon impurities in the air again; and then the gallium nitride sample is subjected to heat treatment in a mixed atmosphere, so that an oxide film on the surface of the gallium nitride can be decomposed, pollutants and the oxide film can be evaporated and taken away along with airflow, and an atomic-level clean gallium nitride surface is obtained, so that the subsequent secondary epitaxial growth is facilitated, the leakage current phenomenon can be reduced, and the reliability of a gallium nitride device is improved.
Drawings
FIG. 1 is a TOF-SIMS curve of a gallium nitride wafer treated with a cleaning solution in example 2 of the present invention;
FIG. 2 is a C-V curve of a double epitaxial growth of AlGaN/GaN heterostructure on gallium nitride substrate in example 2 of the present invention and comparative example 1;
FIG. 3 is a TOF-SIMS curve of a gallium nitride-like wafer treated with an organic solvent in comparative example 1.
Detailed Description
In order to solve the problem that the performance of a gallium nitride device is affected by the fact that an organic siloxane pollution layer is easily formed on the surface of the existing gallium nitride, the invention provides a method for removing pollutants on the surface of the gallium nitride, a pre-cleaned gallium nitride sample is immersed into cleaning liquid for soaking, and the cleaning liquid is mixed solution of hydrogen peroxide and alkali liquor; and then carrying out heat treatment on the gallium nitride sample in a mixed atmosphere, wherein the mixed atmosphere consists of nitrogen, hydrogen and ammonia.
According to the invention, silicon pollutants on the surface of gallium nitride are etched by the mixed solution of hydrogen peroxide and alkali liquor, and a uniform compact oxide film is formed, so that the surface of gallium nitride is prevented from being polluted by silicon impurities in the air again; and then the gallium nitride sample is processed in a mixed atmosphere, so that an oxide film on the surface of the gallium nitride can be decomposed, and an atomic-level clean gallium nitride surface is obtained, thereby facilitating the subsequent secondary epitaxial growth, reducing the leakage current phenomenon and improving the reliability of a gallium nitride device.
The invention will be elucidated by means of specific embodiments.
Example 1
The method for removing the gallium nitride surface pollutants comprises the following steps:
(1) cleaning the gallium nitride sample wafer by using acetone, methanol and isopropanol in sequence, and drying by using nitrogen after cleaning; and then soaking the gallium nitride sample wafer in 200mL of cleaning solution, wherein the cleaning solution is prepared by mixing 30% hydrogen peroxide and 3mol/L potassium hydroxide solution according to the volume ratio of 1:1, the soaking time is 30min, ultrasonic water bath heating is used while soaking, the heating temperature is 95 ℃, the ultrasonic frequency is 20KHz, the chemical reaction can be accelerated by the water bath heating, and sufficient time can ensure complete reaction. This step is used to remove the silicon contamination layer on the surface of gallium nitride.
(2) And after soaking, washing the gallium nitride sample wafer for 5min by using deionized water, and blow-drying by using nitrogen gas to form a uniform compact oxide film on the surface of the gallium nitride sample wafer.
(3) And (3) transferring the gallium nitride sample wafer obtained in the step (2) to metal organic chemical vapor deposition equipment, introducing mixed atmosphere formed by nitrogen, hydrogen and ammonia, heating the reaction chamber to 1000 ℃, carrying out heat treatment for 15min, and obtaining a gallium nitride substrate after the treatment is finished.
Example 2
The method for removing the gallium nitride surface pollutants comprises the following steps:
(1) cleaning the gallium nitride sample wafer by using acetone, methanol and isopropanol in sequence, and drying by using nitrogen after cleaning; and then soaking the gallium nitride sample wafer in 200mL of cleaning solution, wherein the cleaning solution is prepared by mixing 35% hydrogen peroxide and 3mol/L sodium hydroxide solution according to the volume ratio of 1:1, the soaking time is 40min, and ultrasonic water bath heating is carried out while soaking, the heating temperature is 80 ℃, and the ultrasonic frequency is 30 KHz. The step is used for removing a silicon pollution layer on the surface of the gallium nitride, and the TOF-SIMS curve of the processed gallium nitride sample wafer is shown in figure 1.
(2) And after soaking, washing the gallium nitride sample wafer for 8min by using deionized water, and blow-drying by using nitrogen for forming a uniform compact oxide film on the surface of the gallium nitride sample wafer.
(3) And (3) transferring the gallium nitride sample wafer obtained in the step (2) to metal organic chemical vapor deposition equipment, introducing mixed atmosphere formed by nitrogen, hydrogen and ammonia, heating the reaction chamber to 1030 ℃, carrying out heat treatment for 10min, and obtaining a gallium nitride substrate after the treatment is finished, wherein the gallium nitride substrate does not need to be taken out of the reaction chamber, and instead can be subjected to in-situ secondary epitaxial growth by the metal organic chemical vapor deposition equipment, specifically, an AlGaN/GaN heterostructure is subjected to secondary epitaxial growth, and the C-V curve of the formed gallium nitride device is shown in figure 2.
Example 3
The method for removing the gallium nitride surface pollutants comprises the following steps:
(1) cleaning the gallium nitride sample wafer by using acetone, methanol and isopropanol in sequence, and drying by using nitrogen after cleaning; and then soaking the gallium nitride sample wafer in 200mL of cleaning solution, wherein the cleaning solution is prepared by mixing 40% hydrogen peroxide and 3mol/L potassium hydroxide according to the volume ratio of 1:1, the soaking time is 60min, and the gallium nitride sample wafer is heated by using an ultrasonic water bath while being soaked, the heating temperature is 70 ℃, and the ultrasonic frequency is 40 KHz. This step is used to remove the silicon contamination layer on the surface of gallium nitride.
(2) And after soaking, washing the gallium nitride sample wafer for 10min by using deionized water, and blow-drying by using nitrogen gas to form a uniform compact oxide film on the surface of the gallium nitride sample wafer.
(3) And (3) transferring the gallium nitride sample wafer obtained in the step (2) to metal organic chemical vapor deposition equipment, introducing mixed atmosphere formed by nitrogen, hydrogen and ammonia, heating the reaction chamber to 1100 ℃, carrying out heat treatment for 5min, and obtaining a gallium nitride substrate after the treatment is finished.
Comparative example
(1) And cleaning the gallium nitride sample wafer by using acetone, methanol and isopropanol in sequence, drying by using nitrogen after cleaning, wherein the TOF-SIMS curve of the treated gallium nitride sample wafer is shown as figure 3.
(2) And (2) growing an AlGaN/GaN heterostructure on the gallium nitride sample wafer treated in the step (1) in a secondary epitaxial mode, wherein a C-V curve of the formed gallium nitride device is shown in figure 2.
Comparing fig. 1 and fig. 3, it can be seen that in comparative example 1, only silicon-containing contaminants exist on the surface of the gallium nitride sample wafer treated by the organic solvent, but no silicon-containing contaminants are detected on the surface of the gallium nitride sample wafer treated by the organic solvent and the cleaning solution in example 2, which indicates that the silicon-containing contaminants on the surface of the gallium nitride sample wafer can be effectively removed by treating the gallium nitride sample wafer with the mixed solution of hydrogen peroxide and alkali solution.
As can be seen from FIG. 2, when gallium nitride was washed only with an organic solvent (comparative example 1), the carrier concentration at the growth interface was as high as 10 through the secondary epitaxial growth18cm-3It was shown that the silicon impurity concentration at the growth interface was high, and that the secondary epitaxial interface had no carrier peak after cleaning with a cleaning solution formed by mixing hydrogen peroxide and an alkali solution (example 2), indicating that no silicon impurity was present at the interfaceThe cleaning solution formed by mixing hydrogen peroxide and alkali liquor can remove silicon pollutants on the surface of gallium nitride.
It should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these changes and modifications belong to the protection scope of the present invention.

Claims (10)

1. The method for removing the gallium nitride surface pollutants is characterized by comprising the following steps of:
immersing a pre-cleaned gallium nitride sample into cleaning solution for soaking, wherein the cleaning solution is mixed solution of hydrogen peroxide and alkali liquor;
taking out, washing and drying the gallium nitride sample after soaking;
and carrying out heat treatment on the dried gallium nitride sample in a mixed atmosphere, wherein the mixed atmosphere consists of nitrogen, hydrogen and ammonia.
2. The method for removing the surface contaminants of the gallium nitride according to claim 1, wherein the gallium nitride sample is sequentially cleaned by acetone, methanol and isopropanol to realize the pre-cleaning of the gallium nitride sample.
3. The method for removing surface contaminants of gallium nitride according to claim 1, wherein the alkaline solution is potassium hydroxide solution or sodium hydroxide solution.
4. The method for removing gallium nitride surface contaminants according to claim 1, wherein the molar ratio of hydrogen peroxide to alkali solution in the cleaning solution is 3.26-4.52: 1.
5. The method for removing surface contaminants of gallium nitride according to claim 1, wherein the soaking time is 30-60 min.
6. The method for removing the surface contaminants of the gallium nitride, according to claim 1, wherein the soaking process is performed while heating with an ultrasonic water bath, and the heating temperature is 70-95 ℃.
7. The method for removing gallium nitride surface contaminants according to claim 6, wherein the ultrasonic frequency is 20KHz-40 KHz.
8. The method for removing surface contaminants on gallium nitride according to claim 1, wherein the rinsing with deionized water is performed for 5-10min, and the rinsing is performed with nitrogen for drying.
9. The method as set forth in claim 1, wherein the heat treatment temperature is 1000-1100 ℃ and the time is 5-15 min.
10. Gallium nitride substrate for secondary epitaxial growth, characterized in that it is obtained by treatment according to any one of claims 1 to 9.
CN202110424840.0A 2021-04-20 2021-04-20 Method for removing gallium nitride surface pollutants and gallium nitride substrate Pending CN113231386A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114664642A (en) * 2022-03-23 2022-06-24 江苏第三代半导体研究院有限公司 HEMT structure based on III-group nitride homoepitaxy, and preparation method and application thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114664642A (en) * 2022-03-23 2022-06-24 江苏第三代半导体研究院有限公司 HEMT structure based on III-group nitride homoepitaxy, and preparation method and application thereof

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Application publication date: 20210810