CN114965468B - Method for distinguishing 4H-silicon carbide surface - Google Patents
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Abstract
The application relates to a method for distinguishing 4H-silicon carbide surfaces, which 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 wet etching process with KOH as main corrosive agent on the 4H-SiC sample; then hydrochloric acid washing is carried out on the corroded 4H-SiC sample; finally, the AB surface of the 4H-SiC is observed by an optical microscope, and the free energy of the surface is determined according to the isotropy or the anisotropism of the surface, so that the surface with high free energy of the anisotropism of the surface is determined to be the Si surface of the 4H-SiC sample, and the surface with low free energy of the isotropy of the surface is determined to be the C surface of the 4H-SiC sample. The method has low requirements on the detection sample, and has the advantages that no matter whether the sample to be detected is perfect or not, whether the sample to be detected has defects or not, the corrosion temperature and the corrosion time in the corrosion process are shorter, and the result is reliable; and the observation is carried out by adopting an optical microscope, so that the operation is simple and the cost is low.
Description
Technical Field
The present application relates to the field of semiconductors, and in particular, to a method for distinguishing 4H-silicon carbide surfaces.
Background
The wide band gap silicon carbide semiconductor is a new generation of power semiconductor which is newly developed after a silicon semiconductor, and is a necessary material for supporting industries such as 5G communication, intelligent manufacturing, electronic power, military aviation and the like. The third generation semiconductor material represented by silicon carbide (SiC) has a series of advantages of high breakdown field strength, high saturated electron drift rate, high thermal conductivity and the like due to wider forbidden band width, and can be widely applied to extreme conditions such as high temperature, high voltage, high radiation and the like. SiC has 200 homogeneous isoforms or more, 4H-SiC having a high carrier saturation drift rate (electrons 800-1000 cm 2 V -1 s -1 ) And good thermal conductivity (3.7K/W cm) -1 K -1 ) The 4H-SiC material is the only material with complete large-size commercial production line in the silicon carbide homogeneous body. Meanwhile, 4H-SiC has a wide forbidden bandwidth of 3.26 eV and an off-position of 21.8 eVThe material can be combined with the melting point of 2380 and K, so that the material has good radiation resistance and has great application prospect in the fields of aerospace, nuclear energy development, radar and the like. The 4H-SiC single crystal has two polar planes, i.e., a silicon (Si) plane and a carbon (C) plane, and is a polar crystal. The polar faces of the polar crystals are grown at different rates, with the positive polar faces generally growing at a greater rate than the negative polar faces. While the growth situation may further affect its performance. SiC devices are typically grown epitaxially with a silicon face, the bottom surface of the substrate being the carbon polarity face. However, the AB surface of the current 4H-SiC monocrystal 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 rapidly distinguishing the 4H-silicon carbide surface.
The method for distinguishing the 4H-silicon carbide surface 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 wet etching process with KOH as main corrosive agent on the 4H-SiC sample; then hydrochloric acid washing is carried out on the corroded 4H-SiC sample; finally, the AB surface of the 4H-SiC is observed by an optical microscope, and the free energy of the surface is determined according to the isotropy or the anisotropism of the surface, so that the surface with high free energy of the anisotropism of the surface is determined to be the Si surface of the 4H-SiC sample, and the surface with low free energy of the isotropy of the surface is determined to be 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 4H-SiC single crystal substrate to be measured into a sample to be measured, and marking two surfaces of the sample to be measured as an A surface and a B surface respectively, wherein the sample to be measured is a 4H-SiC single crystal substrate, and the two surfaces of the sample to be measured are a Si surface and a C surface respectively;
2) Cleaning a sample to be tested: cleaning the sample to be tested in the step 1) by adopting a modified RCA cleaning process;
3) The sample to be tested after the cleaning step is dried by a nitrogen gun and then is put into a nickel crucible together with corrosive agent,heating to 550-590 ℃ by heating equipment, and preserving heat and corroding for 20-40 min; the corrosive agent is molten KOH and Na 2 O 2 A mixture; wherein Na is 2 O 2 Dissolved oxygen can be provided for the surface of the sample to be tested in the corrosion process, so that the corrosion time is reduced, and the corrosion cost is lowered;
4) Placing the sample to be detected 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) And (3) secondary cleaning: cleaning the cooled sample to be tested by adopting an improved RCA cleaning process again;
6) And observing the A surface and the B surface of the sample to be tested after the secondary cleaning process is completed by using a reflection light source and a transmission light source of the optical microscope respectively.
Further, the improved RCA cleaning process in the method described herein is specifically: SC-1 solution is washed for 20-30 min (NH) 4 OH：H 2 O 2 ：H 2 The volume ratio of O is 1:4:50 Deionized water for 8-15 min, HF for 8-12 min, SC-2 for 20-30 min (HCl: h 2 O 2 ：H 2 The volume ratio of O is 1:1: 6) Washing with deionized water for 8-15 min, washing with HF solution for 8-12 min, and washing with piranha solution for 25-35 min (H) 2 SO 4 ：H 2 O 2 Is 7: 3) The method comprises the steps of washing with deionized water for 8-15 min, washing with HF solution for 8-12 min, and washing with deionized water for 25-35 min.
Further, the method of the present application includes HF and H in HF solution 2 The volume ratio of O is 1:10.
further, KOH and Na in the etchant in step 3) of the method described herein 2 O 2 The mass ratio of (2) is 10-30: 1.
further, the optical microscope of the methods described herein includes a 100x-1000x optical microscope comprising a reflective light source and a transmissive light source of a DIC optic.
Further, the heating device in step 3) of the method described herein is a muffle furnace or a pit furnace.
Further, 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 。
Further, the surface with low surface free energy of isotropic corrosion behavior in the sample to be tested according to the method disclosed in the application is the C surface of the 4H-SiC sample, and the low surface free energy is less than 1000erg/cm 2 . The free energy of the surface of the corrosion surface of the sample to be measured is measured by a liquid cake method or a tab method in a length measurement method. The liquid cake method is to continuously drop liquid drops on the solid surface to form a liquid cake. The height of the cake reaches a maximum as the amount of liquid continues to increase. The surface of the sample to be tested of 4H-SiC is a smooth surface and a rough surface after corrosion, and the rough surface is mostly corrugated. 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. The smooth surface corresponds to the surface with high surface free energy and anisotropic corrosion behavior, and is the Si surface of the 4H-SiC sample; whereas the roughened surface corresponds to a surface with a low surface free energy with isotropic corrosion behaviour, being the C-plane of the 4H-SiC sample.
The beneficial effects of this application include: the method for distinguishing the 4H-silicon carbide surface can effectively and conveniently distinguish the silicon surface and the carbon surface of the 4H-silicon carbide. The difference of corrosiveness of the two surfaces can be clearly seen by observing the flatness of the corroded surface of the sample through an optical microscope, and the free energy of the surface is determined according to isotropic or anisotropic corrosion behaviors, so that the surface A and the surface B of the sample respectively correspond to the surface. The smooth surface corresponds to the surface with high surface free energy and anisotropic corrosion behavior, and is the Si surface of the 4H-SiC sample; the rough surface corresponds to the surface with low free energy of the isotropic corrosion behavior, is the C surface of the 4H-SiC sample, and is mostly corrugated. The method has low requirements on the detection sample, and has the advantages that no matter whether the sample to be detected is perfect or not, whether the sample to be detected has defects or not, the corrosion temperature and the corrosion time in the corrosion process are shorter, and the result is reliable; and the observation is carried out by adopting an optical microscope, so that the operation is simple and the cost is low.
Drawings
FIG. 1 is a schematic flow chart of the method of the present invention;
FIG. 2 is a schematic diagram of a sample to be tested after the secondary cleaning process according to the present invention;
FIG. 3 is a metallographic microscope image of the 4H-SiC of the invention after anisotropic etching of the silicon surface;
FIG. 4 is a metallographic microscope image of the 4H-SiC of the invention after isotropic etching of the carbon face.
Description of the embodiments
In order to make the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions in the embodiments of the present application will be clearly and completely described below. The specific conditions are not specified in the specific embodiments and are carried out according to conventional conditions or conditions suggested 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. 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. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
As shown in fig. 1 to 4, a method for distinguishing 4H-silicon carbide surface described in the present application specifically includes the following steps:
1) Preparing a sample to be tested: firstly, cutting a 4H-SiC single crystal ingot to be measured into a sample with a proper size, and marking two surfaces of the sample as a surface A and a surface B respectively, wherein in the embodiment, the sample to be measured is obtained by cutting a 4H-SiC single crystal ingot, and the size is 5mm multiplied by 5mm;
2) Cleaning a sample to be tested: cleaning the sample to be tested in the step 1) by adopting a modified RCA cleaning process; in this embodiment, the modified RCA cleaning process used is specifically: the cleaning articles are respectively as follows: SC-1 solution was washed for 30min (NH) 4 OH：H 2 O 2 ：H 2 O (O)The volume ratio is 1:4:50 Deionized water for 10min, hf solution for 10min, sc-2 solution for 30min (HCl: h 2 O 2 ：H 2 The volume ratio of O is 1:1: 6) Deionized water for 10min, HF for 10min, piranha for 30min (H 2 SO 4 ：H 2 O 2 Is 7: 3) The cleaning is carried out for 10min by deionized water, 10min by HF solution and 30min by deionized water. HF and H in the HF solution 2 The volume ratio of O is 1:10.
3) Drying a sample to be tested after the cleaning step by using a nitrogen gun, putting the dried sample and an etchant into a nickel crucible together, heating to 550-590 ℃ by using a muffle furnace, and carrying out heat preservation and corrosion for 20-40 min; the corrosive agent is molten KOH and Na 2 O 2 A mixture; and in the present embodiment, the KOH and Na 2 O 2 The mass ratio of (2) is 25:1.
4) Placing 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) And (3) secondary cleaning: cleaning the cooled sample to be tested by adopting the improved RCA cleaning process again;
6) The A-and B-planes of the 4H-SiC sample were observed using the reflective and transmissive light sources of the optical microscope, respectively. The optical microscope comprises a 1000x optical microscope comprising a reflected light source and a transmitted light source of a DIC optic. The difference of the corrosion behaviors of the two surfaces can be clearly seen by observing the flatness of the corroded surface of the sample, and the free energy of the surface is determined according to the isotropic or anisotropic corrosion behaviors of the sample, so that the surface A and the surface B of the sample respectively correspond to the surface. The smooth surface corresponds to the surface with high surface free energy and anisotropic corrosion behavior, and is the Si surface of the 4H-SiC sample; the rough surface corresponds to the surface with low free energy of the isotropic corrosion behavior, is the C surface of the 4H-SiC sample, and is mostly corrugated. In this example, the free energy of the surface of the etched surface of the sample to be measured was measured by the liquid cake method in the length measurement method. The liquid cake method is to continuously drop liquid drops on the solid surface to form a liquid cake. Continue to increaseThe height of the cake reaches a maximum when the amount of liquid is added. The surface of the high surface free energy with anisotropic corrosion behavior in the sample to be tested is the Si surface of a 4H-SiC sample, and the high surface free energy is 1800 erg/cm 2 . The surface of the low surface free energy with isotropic corrosion behavior in the sample to be tested is the C surface of the 4H-SiC sample, and the low surface free energy is 750 erg/cm 2 。
The embodiments described above are some, but not all, of the embodiments of the present application. The detailed description of the embodiments of the present application is not intended to limit the scope of the application, as claimed, but is merely representative of selected embodiments of the application. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present disclosure.
Claims (4)
1. A method for distinguishing 4H-silicon carbide surfaces, characterized in that the method firstly marks two surfaces of a 4H-silicon carbide (4H-SiC) sample to be distinguished as an a-plane and a B-plane respectively; then carrying out wet etching process with KOH as main corrosive agent on the 4H-SiC sample; then hydrochloric acid washing is carried out on the corroded 4H-SiC sample; finally, observing the AB surface of the 4H-SiC by using an optical microscope, determining the free energy of the surface according to isotropic or anisotropic corrosion behavior of the AB surface, and judging that the surface with high free energy of the anisotropic corrosion behavior is the Si surface of the 4H-SiC sample, and the surface with low free energy of the isotropic corrosion behavior is the C surface of the 4H-SiC sample;
the method specifically comprises the following steps:
1) Preparing a sample to be tested: firstly, cutting a 4H-SiC single crystal substrate to be measured into a sample to be measured, and marking two surfaces of the sample to be measured as an A surface and a B surface respectively, wherein the sample to be measured is a 4H-SiC single crystal substrate, and the two surfaces of the sample to be measured are a Si surface and a C surface respectively;
2) Cleaning a sample to be tested: cleaning the sample to be tested in the step 1) by adopting a modified RCA cleaning process; the improved RCA cleaning process specifically comprises the following steps: NH (NH) 4 OH：H 2 O 2 ：H 2 The volume ratio of O is 1:4:50, cleaning with an SC-1 solution for 20-30 min, cleaning with deionized water for 8-15 min, cleaning with an HF solution for 8-12 min, and carrying out HCl: h 2 O 2 ：H 2 The volume ratio of O is 1:1:6 SC-2 solution cleaning for 20-30 min, deionized water cleaning for 8-15 min, HF solution cleaning for 8-12 min, H 2 SO 4 ：H 2 O 2 Is 7:3, cleaning the piranha solution (piranha solution) for 25-35 min, cleaning the piranha solution with deionized water for 8-15 min, cleaning the piranha solution with HF for 8-12 min, and cleaning the piranha solution with deionized water for 25-35 min;
3) Drying a sample to be tested after the cleaning step by using a nitrogen gun, putting the dried sample and corrosive agent into a nickel crucible, heating to 550-590 ℃ by adopting heating equipment, and carrying out heat preservation and corrosion for 20-40 min; the corrosive agent is molten KOH and Na 2 O 2 A mixture; KOH and Na in the corrosive agent 2 O 2 The mass ratio of (2) is 10-30: 1, a step of;
4) Placing the sample to be detected obtained in the step 3) into a hydrochloric acid solution with the mass fraction of 30%, and cooling to room temperature;
5) And (3) secondary cleaning: cleaning the cooled sample to be tested by adopting an improved RCA cleaning process again;
6) The reflection light source and the transmission light source of the optical microscope are respectively used for observing the A surface and the B surface of a sample to be tested which completes the secondary cleaning process, wherein the surface with high surface free energy of anisotropic corrosion behavior is the Si surface of a 4H-SiC sample, and the high surface free energy is more than or equal to 1000erg/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the While the surface with low surface free energy of the isotropic corrosion behavior is the C surface of the 4H-SiC sample, the low surface free energy is less than 1000erg/cm 2 。
2. The method of distinguishing between 4H-silicon carbide surfaces according to claim 1 wherein the HF solution is medium HF and H 2 The volume ratio of O is 1:10.
3. the method of distinguishing 4H-silicon carbide surfaces according to claim 2 wherein the optical microscope is a 100x-1000x optical microscope comprising a reflective light source and a transmissive light source comprising DIC optics.
4. A method of distinguishing between 4H-silicon carbide surfaces according to claim 3 wherein the heating device in step 3) is a muffle furnace or a pit furnace.
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