CN114965468A - Method for distinguishing 4H-silicon carbide surface - Google Patents
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- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B11/00—Measuring arrangements characterised by the use of optical techniques
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Abstract
The application relates to a method for distinguishing a 4H-silicon carbide surface, which comprises the steps of firstly marking two surfaces of a 4H-silicon carbide (4H-SiC) sample to be distinguished as an A surface and a B surface respectively; then carrying out a wet etching process by taking KOH as a main etchant on the 4H-SiC sample; then hydrochloric acid pickling is carried out on the corroded 4H-SiC sample; and finally observing the AB surface of the 4H-SiC by using an optical microscope, and determining the surface free energy according to the isotropic or anisotropic etching behavior, so that the surface with the high surface free energy and the isotropic etching behavior is the Si surface of the 4H-SiC sample, and the surface with the low surface free energy and the isotropic etching behavior is the C surface of the 4H-SiC sample. The method has low requirements on the detection sample, whether the sample to be detected is intact or not and whether the sample to be detected has defects or not, the corrosion temperature and the corrosion time in the corrosion process are both short, and the result is reliable; and the optical microscope is adopted for observation, so that the operation is simple and the cost is low.
Description
Technical Field
The application relates to the field of semiconductors, in particular to a method for distinguishing 4H-silicon carbide surfaces.
Background
The wide bandgap silicon carbide semiconductor is a new generation power semiconductor newly developed after a silicon semiconductor, and is a necessary material for supporting industries such as 5G communication, intelligent manufacturing, electronic power, military industry and aerospace and the like. And third-generation semiconductor materials represented by silicon carbide (SiC) have a series of advantages of high breakdown field strength, high saturated electron drift rate, high thermal conductivity and the like due to wider forbidden bandwidth, and can be widely applied to extreme conditions of high temperature, high pressure, high radiation and the like. SiC has more than 200 types of allotropes, wherein 4H-SiC has higher carrier saturation drift rate (electrons are 800- 2 V -1 s -1 ) And good thermal conductivity (3.7K/W cm) -1 K -1 ) The method has the foundation for preparing high-power devices, so that the 4H-SiC material is the only material with a complete large-size commercial production line in the silicon carbide homogeneous and special-shaped body. Meanwhile, 4H-SiC has a wide energy gap of 3.26eV, an off-potential energy of 21.8eV and a melting point of 2380K, so that the material has good radiation resistance and has a great application prospect in the fields of aerospace, nuclear energy development, radar and the like. The 4H-SiC single crystal has two polar faces, a silicon (Si) face and a carbon (C) face, and is a polar crystal. The growth rates of the polar faces of the polar crystal are different, and the growth rate of the positive face is generally higher than that of the negative face. While growth conditions further affect its performance. SiC devices are typically grown epitaxially using a silicon surface, with the bottom surface of the substrate being a carbon polar surface. However, the AB surface of the 4H-SiC single crystal is difficult to distinguish in a series of tests such as an optical microscope, an atomic force microscope, a photoluminescence spectrum, X-ray diffraction and the like.
Disclosure of Invention
Aiming at the defects of the prior art, the application provides a method for conveniently and quickly distinguishing the surface of 4H-silicon carbide.
The method for distinguishing the surface of the 4H-silicon carbide comprises the steps of firstly, respectively marking two surfaces of a 4H-silicon carbide (4H-SiC) sample to be distinguished as an A surface and a B surface; then carrying out a wet etching process by taking KOH as a main etchant on the 4H-SiC sample; then hydrochloric acid pickling is carried out on the corroded 4H-SiC sample; and finally observing the AB surface of the 4H-SiC by using an optical microscope, and determining the surface free energy according to the isotropic or anisotropic etching behavior, so that the surface with the high surface free energy and the isotropic etching behavior is the Si surface of the 4H-SiC sample, and the surface with the low surface free energy and the isotropic etching behavior is the C surface of the 4H-SiC sample.
Further, the method specifically comprises the following steps:
1) preparing a sample to be tested: firstly, cutting a proper size from 4H-SiC to be detected to be used as a sample to be detected, and marking two surfaces of the sample to be detected as an A surface and a B surface respectively, wherein the sample to be detected is a 4H-SiC single crystal substrate, and the two surfaces are a Si surface and a C surface respectively;
2) cleaning a sample to be tested: cleaning the sample to be detected in the step 1) by adopting an improved RCA cleaning process;
3) drying the sample to be tested after the cleaning step by using a nitrogen gun, putting the sample to be tested and the corrosive agent into a nickel crucible together, then heating the sample to 550-; the corrosive agent is molten KOH and Na 2 O 2 Mixing; wherein Na 2 O 2 Dissolved oxygen can be provided for the surface of a sample to be detected in the corrosion process, so that the corrosion time is reduced, the corrosion is reduced, and the cost is reduced;
4) putting the sample to be tested obtained in the step 3) into a hydrochloric acid solution with the mass fraction of 30%, and cooling to room temperature; the process can also remove alkaline residual substances on the surface of the sample to be detected;
5) secondary cleaning: cleaning the cooled sample to be detected by adopting an improved RCA cleaning process again;
6) and observing the surface A and the surface B of the sample to be measured after the secondary cleaning process is finished by using a reflection light source and a transmission light source of an optical microscope respectively.
Further, the improved RCA cleaning process in the method of the present application specifically includes: the cleaning supplies are respectively: cleaning with SC-1 solution for 20-30 min (NH) 4 OH：H 2 O 2 ：H 2 Volume of O is 1: 4: 50) deionized water cleaning for 8-15 min, HF solution cleaning for 8-12 min, SC-2 solution cleaning for 20-30 min (HCl: h 2 O 2 ：H 2 The volume ratio of O is 1: 1: 6) cleaning with deionized water for 8-15 min, HF solution for 8-12 min, and piranha solution for 25-35 min (H) 2 SO 4 ：H 2 O 2 Is 7: 3) and cleaning with deionized water for 8-15 min, cleaning with HF solution for 8-12 min, and cleaning with deionized water for 25-35 min.
Further, in the method of the present application, HF and H in the HF solution 2 The volume ratio of O is 1: 10.
further, KOH and Na are contained in the etchant in step 3) of the method described in the application 2 O 2 The mass ratio of (A) to (B) is 10-30: 1.
further, the optical microscope of the method described herein is a 100x-1000x optical microscope with a reflective light source (containing DIC optics) and a transmissive light source.
Further, the heating device in step 3) of the method is a muffle furnace or a shaft furnace.
Furthermore, the surface with high surface free energy of anisotropic corrosion behavior in the sample to be tested is the Si surface of the 4H-SiC sample, and the high surface free energy is more than or equal to 1000erg/cm 2 。
Furthermore, the surface with low surface free energy of isotropic corrosion behavior in the sample to be tested by the method is the C surface of the 4H-SiC sample, and the low surface free energy is less than 1000erg/cm 2 . The surface free energy of the corrosion surface of the sample to be measured is measured by a liquid cake method or a flap method in the length measurement method. The liquid cake method is to drop liquid drops continuously on the surface of solid to form a liquid cake. As the amount of liquid continues to increase, the height of the liquid cake reaches a maximum. The corroded surface of the 4H-SiC sample to be tested is represented by a smooth surface and a rough surface, and the rough surface is mostly in a corrugated shape. The surface free energy is determined according to the isotropic or anisotropic corrosion behavior, so that the A surface and the B surface of the sample are respectively corresponding to which surfaces. Smooth surfaces correspond to high surface freedom with anisotropic etching behaviorThe surface of the energy is the Si surface of the 4H-SiC sample; the rough surface corresponds to a surface with low surface free energy and isotropic corrosion behavior, and is the C surface of the 4H-SiC sample.
The beneficial effect of this application includes: the method for distinguishing the surface of the 4H-silicon carbide is provided, and the silicon surface and the carbon surface of the 4H-silicon carbide can be effectively and conveniently distinguished. The flatness of the surface of the sample after corrosion is observed through an optical microscope, the difference of the corrosivity of the two surfaces can be clearly seen, and the size of the free energy of the surface is determined according to the isotropic or anisotropic corrosion behavior, so that the surface A and the surface B of the sample are respectively corresponding to which surface. Wherein the smooth surface corresponds to a surface with high surface free energy and anisotropic corrosion behavior, and is the Si surface of a 4H-SiC sample; the rough surface corresponds to a surface with low surface free energy and isotropic corrosion behavior, is the C surface of a 4H-SiC sample, and is mostly in a corrugated shape. The method has low requirements on the detection sample, whether the sample to be detected is intact or not and whether the sample to be detected has defects or not, the corrosion temperature and the corrosion time in the corrosion process are both short, and the result is reliable; and the optical microscope is adopted for observation, so that the operation is simple and the cost is low.
Drawings
FIG. 1 is a schematic flow diagram of the process of the present invention;
FIG. 2 is a schematic diagram of a sample to be tested after a secondary cleaning process is completed according to the present invention;
FIG. 3 is a metallographic microscopic image of 4H-SiC according to the invention after anisotropic etching of the silicon surface;
FIG. 4 is a metallographic microscopic image of 4H-SiC of the present invention after isotropic etching of the carbon face.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application more apparent, the technical solutions of the embodiments of the present application will be described clearly and completely below. Those whose specific conditions are not specified in the specific embodiment are carried out according to the conventional conditions or conditions recommended by the manufacturer.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
As shown in fig. 1 to 4, the method for distinguishing a 4H-silicon carbide surface according to the present application specifically includes the following steps:
1) preparing a sample to be tested: firstly, cutting a proper size from 4H-SiC to be detected to be used as a sample to be detected, and respectively marking two surfaces of the sample to be detected as an A surface and a B surface, wherein in the embodiment, the sample to be detected is obtained by cutting a 4H-SiC single crystal ingot, and the size of the sample to be detected is 5mm multiplied by 5 mm;
2) cleaning a sample to be tested: cleaning the sample to be detected in the step 1) by adopting an improved RCA cleaning process; in this embodiment, the adopted improved RCA cleaning process specifically includes: the cleaning supplies are respectively: SC-1 solution cleaning for 30min (NH) 4 OH：H 2 O 2 ：H 2 Volume of O is 1: 4: 50) deionized water cleaning for 10min, HF solution cleaning for 10min, SC-2 solution cleaning for 30min (HCl: h 2 O 2 ：H 2 The volume ratio of O is 1: 1: 6) deionized water cleaning for 10min, HF solution cleaning for 10min, piranha solution cleaning for 30min (H) 2 SO 4 ：H 2 O 2 Is 7: 3) and cleaning with deionized water for 10min, cleaning with HF solution for 10min, and cleaning with deionized water for 30 min. HF and H in the HF solution 2 The volume ratio of O is 1: 10.
3) drying the sample to be tested after the cleaning step by using a nitrogen gun, putting the sample to be tested and the corrosive agent into a nickel crucible together, then heating the sample to 550-; the corrosive agent is molten KOH and Na 2 O 2 Mixing; in the present embodiment, KOH and Na are used 2 O 2 The mass ratio of (A) to (B) is 25: 1.
4) putting the sample to be detected obtained in the step 3) into a hydrochloric acid solution with the mass fraction of 30% (AR), and cooling to room temperature;
5) secondary cleaning: cleaning the cooled sample to be tested by adopting the improved RCA cleaning process again;
6) the a-plane and the B-plane of the 4H-SiC sample were observed using a reflection light source and a transmission light source of an optical microscope, respectively. The optical microscope is a 1000x optical microscope with a reflective light source (containing DIC lenses) and a transmissive light source. And observing the flatness of the surface of the sample after corrosion, clearly seeing the difference of the corrosion behaviors of the two surfaces, and determining the size of the surface free energy according to the isotropic or anisotropic corrosion behaviors, thereby judging which surface the A surface and the B surface of the sample respectively correspond to. Wherein the smooth surface corresponds to a surface with high surface free energy and anisotropic corrosion behavior, and is the Si surface of a 4H-SiC sample; the rough surface corresponds to a surface with low surface free energy and isotropic corrosion behavior, is the C surface of the 4H-SiC sample, and is mostly corrugated. In this example, the surface free energy of the etched surface of the sample to be measured was measured by the liquid-cake method among the length measurement methods. The liquid cake method is to drop liquid drops continuously on the solid surface to form a liquid cake. As the amount of liquid continues to increase, the height of the liquid cake reaches a maximum. The surface with high surface free energy of anisotropic corrosion behavior in the sample to be detected is the Si surface of the 4H-SiC sample, and the high surface free energy is 1800erg/cm 2 . The surface with low surface free energy and isotropic corrosion behavior in the sample to be detected is the C surface of the 4H-SiC sample, and the low surface free energy is 750erg/cm 2 。
The embodiments described above are some, but not all embodiments of the present application. The detailed description of the embodiments of the present application is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
Claims (9)
1. A method for distinguishing the surface of 4H-silicon carbide is characterized in that the method firstly marks two surfaces of a 4H-silicon carbide (4H-SiC) sample to be distinguished as an A surface and a B surface respectively; then carrying out a wet etching process by taking KOH as a main etchant on the 4H-SiC sample; then hydrochloric acid pickling is carried out on the corroded 4H-SiC sample; and finally, observing the AB surface of the 4H-SiC by using an optical microscope, determining the surface free energy according to the isotropic or anisotropic corrosion behavior, and judging that the surface with the high surface free energy and the isotropic corrosion behavior is the Si surface of the 4H-SiC sample, and the surface with the low surface free energy and the isotropic corrosion behavior is the C surface of the 4H-SiC sample.
2. Method for distinguishing 4H-silicon carbide surfaces according to claim 1, characterized in that it comprises in particular the following steps:
1) preparing a sample to be tested: firstly, cutting a sample to be detected from 4H-SiC to be a proper size, and marking two surfaces of the sample to be detected as an A surface and a B surface respectively, wherein the sample to be detected is a 4H-SiC single crystal substrate, and the two surfaces of the sample to be detected are a Si surface and a C surface respectively;
2) cleaning a sample to be tested: cleaning the sample to be detected in the step 1) by adopting an improved RCA cleaning process;
3) drying the sample to be tested after the cleaning step by using a nitrogen gun, putting the sample to be tested and the corrosive agent into a nickel crucible together, then heating the sample to 550-; the corrosive agent is molten KOH and Na 2 O 2 Mixing;
4) putting the sample to be tested obtained in the step 3) into a hydrochloric acid solution with the mass fraction of 30%, and cooling to room temperature;
5) secondary cleaning: cleaning the cooled sample to be detected by adopting an improved RCA cleaning process again;
6) and observing the surface A and the surface B of the sample to be measured after the secondary cleaning process by using a reflection light source and a transmission light source of an optical microscope respectively.
3. The method for distinguishing 4H-silicon carbide surfaces according to claim 2, wherein the modified RCA cleaning process is specifically: the cleaning products are respectively: cleaning with SC-1 solution for 20-30 min (NH) 4 OH：H 2 O 2 ：H 2 Volume of O is 1: 4: 50) deionized water cleaning for 8-15 min, HF solution cleaning for 8-12 min, SC-2 solution cleaning for 20-30 min (HCl: h 2 O 2 ：H 2 The volume ratio of O is 1: 1: 6) cleaning with deionized water for 8-15 min, HF solution for 8-12 min, and piranha solution for 25-35 min (H) 2 SO 4 ：H 2 O 2 Is 7: 3) and cleaning with deionized water for 8-15 min, cleaning with HF solution for 8-12 min, and cleaning with deionized water for 25-35 min.
4. The method for distinguishing 4H-silicon carbide surfaces according to claim 3 wherein the HF and H in the HF solution 2 The volume ratio of O is 1: 10.
5. the method for distinguishing 4H-silicon carbide surfaces according to claim 4 wherein KOH and Na in the etchant of step 3) 2 O 2 The mass ratio of (A) to (B) is 10-30: 1.
6. the method of distinguishing 4H-silicon carbide surfaces according to claim 5 wherein the optical microscope is a 100x-1000x optical microscope with a reflective light source (including DIC optics) and a transmissive light source.
7. The method for distinguishing 4H-silicon carbide surfaces according to claim 6, wherein the heating device in step 3) is a muffle furnace or a shaft furnace.
8. The method for distinguishing the surface of 4H-silicon carbide according to claim 7, wherein the surface with high surface free energy of anisotropic corrosion behavior in the sample to be tested is the Si surface of the 4H-SiC sample, and the high surface free energy is not less than 1000erg/cm 2 。
9. The method of claim 8, wherein the surface with low surface free energy having isotropic corrosion behavior in the sample under test is 4H-SiC-likeThe low surface free energy of the C surface of the product is less than 1000erg/cm 2 。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116577340A (en) * | 2023-05-28 | 2023-08-11 | 兰州大学 | Method for distinguishing threading screw dislocation and threading edge dislocation in silicon carbide |
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| CN107991230A (en) * | 2018-01-08 | 2018-05-04 | 中国电子科技集团公司第四十六研究所 | A kind of method for distinguishing silicon carbide wafer carbon silicon face |
| CN113594027A (en) * | 2021-07-27 | 2021-11-02 | 兰州大学 | Method for corroding surface of 4H-silicon carbide |
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| CN103630708A (en) * | 2013-11-26 | 2014-03-12 | 河北同光晶体有限公司 | Method for distinguishing Si surface from C surface of SiC (silicon carbide) wafer |
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Cited By (2)
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|---|---|---|---|---|
| CN116577340A (en) * | 2023-05-28 | 2023-08-11 | 兰州大学 | Method for distinguishing threading screw dislocation and threading edge dislocation in silicon carbide |
| CN116577340B (en) * | 2023-05-28 | 2024-01-05 | 兰州大学 | Method for distinguishing threading screw dislocation and threading edge dislocation in silicon carbide |
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