CN111238910A - Dislocation identification method of silicon carbide crystal - Google Patents
Dislocation identification method of silicon carbide crystal Download PDFInfo
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The invention provides a dislocation identification method of a silicon carbide crystal, which comprises the following steps: (1) corroding the silicon carbide crystal in an alkaline corrosive agent; (2) observing the appearance of the dislocation etch pits after etching is finished, so as to identify edge dislocations, screw dislocations and basal plane dislocations in the silicon carbide crystal; the silicon carbide crystals comprise high-purity silicon carbide and nitrogen-doped silicon carbide, wherein the corrosion time of the high-purity silicon carbide is 5-7 min, and the corrosion time of the nitrogen-doped silicon carbide is 7-9 min. According to the invention, by optimizing the corrosion time of alkaline corrosion and controlling the corrosion time of high-purity silicon carbide and nitrogen-doped silicon carbide to be less than 10min, three dislocations, namely edge dislocation, screw dislocation and basal plane dislocation in the high-purity silicon carbide or the nitrogen-doped silicon carbide, can be accurately distinguished; the etching time is short and three kinds of dislocation in the crystal can be accurately identified.
Description
Technical Field
The invention relates to a dislocation identification method of a silicon carbide crystal, and belongs to the technical field of crystal material testing characterization.
Background
Silicon carbide has been widely used as a novel power device material because of its high electrical resistivity, high strength and good thermal conductivity. However, due to the high requirements of the growth conditions, the defects introduced during the growth process limit the improvement of the performance and the further application and development. Therefore, characterization and statistics of defects are the first prerequisites for improving their defects. Dislocations, which are a type of line defect, are classified into edge dislocations (TED), threading dislocations (TSD), and Basal Plane Dislocations (BPD) according to their formation mechanism and the resulting difference in the half atomic planes. The influence of different dislocations and the density of the dislocations on the subsequent epitaxial growth is different, so that the accurate distinction of various dislocations is very important for determining the quality of the silicon carbide crystal.
Since the presence of dislocations causes microscopic lattice distortion in the silicon carbide dislocation-present region, macroscopically manifested as large surface strain energy, the alkaline etching of silicon carbide is generally used to collapse the surface-stressed region and thus present in the form of etch pits. Molten NaOH or KOH is mostly adopted for dislocation corrosion of silicon carbide, but chemical stability of the silicon carbide after nitrogen doping is more qualitative, so that high-resolution corrosion detection of three kinds of dislocations is difficult to realize by a single alkaline corrosive.
CN108169228A discloses a method for accurately identifying dislocation types of silicon carbide single crystals, which comprises the steps of selectively etching defects of silicon carbide single crystals, observing the appearance of dislocation etch pits after etching is completed, obtaining the sectional view, width and depth information of the etch pits, and further identifying the dislocation types through the sectional view and included angle of the etch pits. The method uses KOH, NaOH or a mixture of KOH and NaOH as a corrosive agent, the corrosion time is 10-35 min, the method can accurately judge the types of mixed dislocation, screw dislocation and edge dislocation in the silicon carbide crystal, but cannot simultaneously identify the edge dislocation, the screw dislocation and the basal plane dislocation, and the corrosion time is long.
Disclosure of Invention
In order to solve the problems, the invention provides a dislocation identification method of a silicon carbide crystal, which provides a corresponding silicon carbide corrosion process to realize good corrosion on the silicon carbide crystal by aiming at the physical characteristics of the high-purity silicon carbide and nitrogen-doped silicon carbide which are widely applied in the current market, so that edge dislocation, screw dislocation and basal plane dislocation in the crystal are accurately distinguished.
The technical scheme adopted by the application is as follows:
in a first aspect, the present invention provides a method of identifying dislocations in a silicon carbide crystal, the method comprising the steps of:
(1) corroding the silicon carbide crystal in an alkaline corrosive agent;
(2) observing the appearance of the dislocation etch pits after etching is finished, so as to identify edge dislocations, screw dislocations and basal plane dislocations in the silicon carbide crystal;
the silicon carbide crystals comprise high-purity silicon carbide and nitrogen-doped silicon carbide, wherein the corrosion time of the high-purity silicon carbide is 5-7 min, and the corrosion time of the nitrogen-doped silicon carbide is 7-9 min.
Preferably, the etching time of the high-purity silicon carbide is 6min, and the etching time of the nitrogen-doped silicon carbide is 8 min.
Preferably, in the step (1), when the high-purity silicon carbide is etched, the alkaline etchant includes KOH, and the etching temperature is 500-600 ℃.
Preferably, when the high-purity silicon carbide is etched, the etching temperature is 520-580 ℃.
More preferably, when the high purity silicon carbide is etched, the temperature of the etching is 550 ℃.
Preferably, in step (1), when the nitrogen-doped silicon carbide is etched, the alkaline etchant includes KOH and Na2O2KOH and Na2O2The mass ratio of the components is 50: 7-9, and the corrosion temperature is 550-650 ℃.
Preferably, KOH and Na2O2In a mass ratio of 50: 8.
Preferably, when the nitrogen-doped silicon carbide is etched, the etching temperature is 580-620 ℃.
More preferably, when the nitrogen-doped silicon carbide is etched, the temperature of the etching is 600 ℃.
For high purity silicon carbide, the dislocation-existing regions are stressed and fusedThe KOH will attack it so that the dislocations are exposed in the form of etch pits; and for the silicon carbide doped with nitrogen, the silicon carbide electronic band is bent upwards to form a p-type inversion region due to the nitrogen element in the substrate, and the chemical stability of the silicon carbide electronic band is enhanced due to the existence of holes in the p-type inversion region, so that the silicon carbide electronic band is difficult to be corroded by a single alkaline corrosive agent. Macroscopically, which is shown by the use of a single molten KOH etch, the hexagonal etch pits tend to be circular, adding difficulty to the differentiation of the different types of dislocations, and the process of the invention therefore uses KOH and Na2O2Etching is carried out, Na2O2When the material is melted at about 600 ℃, atomic oxygen is released, so that many elements in the material lose electrons and are quickly oxidized to the highest valence state; the high valence cation is immediately complexed with oxygen to form a complex; the molten KOH and Na used in the present invention2O2The strong alkalinity generated by the mixed corrosive liquid in a high-temperature molten state is beneficial to the formation and the stability of the high-valence cation complexes, so that the corrosivity to the substance is enhanced, and different degrees of damage to the crystal structure with stress can be realized.
Preferably, in the step (1), before the etching, the surface of the silicon carbide crystal is subjected to lapping, polishing and cleaning treatment.
Preferably, the particles and the grease on the surface of the silicon carbide crystal are cleaned.
Preferably, after the cleaning treatment, the surface of the silicon carbide crystal is subjected to pre-etching using hydrofluoric acid and/or nitric acid.
Preferably, in the step (2), after the etching is completed, the silicon carbide crystal is taken out and cooled to room temperature, and then is alternately cleaned by absolute ethyl alcohol and high-purity water.
Preferably, in step (2), the observation is direct visual observation or observation by means of a microscope. Different types of dislocations are shown in the etch pits with different shapes and sizes through dislocation corrosion, so that the dislocation observation can be carried out through naked eyes or an optical metallographic microscope and the like, the observation is simple, and the cost is low.
Preferably, in the step (2), in the high-purity silicon carbide, the hexagonal etch pits with the equal product circle diameter of 40-50 μm correspond to screw dislocations, the circular etch pits with the equal product circle diameter of 20-30 μm correspond to edge dislocations, and the drop-shaped etch pits with the equal product circle diameter of 20-30 μm correspond to basal plane dislocations.
And/or in the nitrogen-doped silicon carbide, the hexagonal corrosion pits with the equal product circle diameter of 50-60 mu m correspond to screw dislocation, the circular corrosion pits with the equal product circle diameter of 10-20 mu m correspond to edge dislocation, and the water drop-shaped corrosion pits with the equal product circle diameter of 10-20 mu m correspond to basal plane dislocation.
Preferably, in the high-purity silicon carbide and/or the nitrogen-doped silicon carbide, the dislocation line direction is along the crystal axis
And the direction is that the head part of the etch pit is an exposed point of dislocation, and the tail part of the etch pit is a deepened area, so that the substrate plane dislocation is correspondingly formed.
In a second aspect, the invention also provides a silicon carbide crystal dislocation etchant comprising KOH and Na2O2KOH and Na2O2The mass ratio of (A) to (B) is 50: 7-9.
Preferably, among the corrosive agents, KOH and Na2O2In a mass ratio of 50: 8.
Preferably, the silicon carbide crystal is nitrogen-doped silicon carbide.
For different types of dislocations, TED (edge dislocation) is a knife-edge-like semi-atomic plane locally generated by the crystal under the action of shear stress; TSD (threading dislocation) is that an atomic plane is generated locally due to the action of shear stress on a crystal, the crystal plane slides, and the atomic plane rises spirally, so that threading dislocation is generated; BPD (basal plane dislocation) is mostly a crystal defect caused by stress due to temperature gradient difference during the growth of silicon carbide. The TSD bernet vector of dislocations in a silicon carbide crystal is greater than TED, and thus TSD is also greater than TED for etch pit size. Due to the difference of atom arrangement caused by the difference of the three kinds of dislocation formation and the difference of stress generated on the crystal surface, the etching pits with fixed characteristics are shown under the corrosion of the molten corrosive agent, so that the dislocation identification has good identification degree.
The invention has the beneficial effects that:
(1) according to the invention, by optimizing the corrosion time of alkaline corrosion and controlling the corrosion time of high-purity silicon carbide corrosion and nitrogen-doped silicon carbide to be less than 10min, three dislocations, namely edge dislocation, screw dislocation and basal plane dislocation in the high-purity silicon carbide or the nitrogen-doped silicon carbide, can be accurately distinguished; the etching time is short and three kinds of dislocation in the crystal can be accurately identified.
(2) By adopting the method, the edge dislocation, the screw dislocation and the basal plane dislocation in the crystal can clearly appear in the form of the corrosion pit, and the three dislocations can be accurately identified according to the appearance and the size of the corrosion pit and the orientation of dislocation outcrop points, have higher distinguishing degree on the appearance and the size, can be distinguished by naked eyes in the dislocation identification process, and are convenient for the representation and the statistics of the dislocations.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
FIG. 1 is a topographical view of high purity silicon carbide dislocations of the present invention, (A) TSD; (B) TED; (C) BPD;
FIG. 2 is a 3D topographical view of dislocation etch pits of high purity silicon carbide according to the present invention, (A) TSD; (B) TED; (C) BPD;
FIG. 3 is a dislocation profile of etched high purity silicon carbide according to the present invention;
FIG. 4 is a diagram showing dislocation recognition after etching of high purity silicon carbide in accordance with the present invention;
FIG. 5 is a topographical view of nitrogen doped silicon carbide dislocations of the present invention, (A) TSD; (B) TED; (C) BPD;
FIG. 6 is a 3D topographical view of a nitrogen doped silicon carbide dislocation etch pit of the present invention, (A) TSD; (B) TED; (C) BPD;
FIG. 7 is a dislocation distribution map after etching of nitrogen doped silicon carbide in accordance with the present invention;
FIG. 8 is a diagram illustrating dislocation identification after etching of nitrogen doped silicon carbide in accordance with the present invention;
FIG. 9 is an illustration of an identification of basal plane dislocations of the present invention, (A) a head; (B) a tail portion;
FIG. 10 is a schematic illustration of dislocation etch pits for high purity silicon carbide of the present invention at different etch times; (A) the etching time is 4 min; (B) the etching time is 6 min; (C) the etching time is 8 min; (D) the etching time is 10 min;
FIG. 11 is a schematic view of dislocation etch pits of nitrogen-doped silicon carbide of the present invention at different etch recipes; (A) KOH and Na2O2In a mass ratio of 50: 6; (B) KOH and Na2O2In a mass ratio of 50: 8; (C) KOH and Na2O2In a mass ratio of 50: 10;
FIG. 12 is a schematic view of dislocation etch pits for nitrogen-doped silicon carbide of the present invention at various etch times; (A) the corrosion time is 2 min; (B) the etching time is 4 min; (C) the etching time is 6 min; (D) the etching time is 8 min; (E) the etching time was 10 min.
Detailed Description
The present invention is described in detail with reference to specific examples, which are provided to facilitate the understanding of the technical solutions of the present invention by those skilled in the art, and the implementation or use of the present invention is not limited by the description of the present invention.
In the present invention, the raw materials and equipment used are commercially available or commonly used in the art, if not specified.
The methods in the examples are conventional in the art unless otherwise specified.
Example 1: dislocation identification method of high-purity silicon carbide
This embodiment describes a dislocation identification method for high-purity silicon carbide, which includes the following steps:
(1) pretreatment: high-purity silicon carbide is firstly ground and polished according to a normal process, so that the silicon carbide has a flat and smooth surface. Then, ultrapure water is adopted to clean crystal surface particles, dilute sulfuric acid is adopted to clean oil on the crystal surface, hydrofluoric acid (with the mass concentration of 8%) is adopted to pre-corrode the crystal surface, the pre-corrosion temperature is 20 ℃, and the hydrofluoric acid can also eliminate and treat scratches on the crystal surface; and finally, neutralizing and cleaning the pretreatment solution by respectively adopting hydrogen peroxide and sodium bicarbonate. And then, the wafer is cleaned and dried for many times by adopting ultrapure water, so that the pretreatment process is completed. The pretreatment purpose is as follows: firstly, the surface of a wafer is cleaned, so that the surface of the wafer is free from large-particle pollution; secondly, the surface of the steel is pre-etched.
(2) Dislocation etching process: and (3) putting the KOH solid particles into a nickel crucible, and melting in a high-temperature resistance furnace, wherein the melting temperature is stable for 3 hours when reaching 550 ℃, so that the KOH is completely melted, and the physical adsorption water in the KOH is discharged at high temperature. And then, placing the pretreated high-purity silicon carbide wafer in a dry nickel wire corrosion net, and immersing the silicon carbide wafer in molten KOH for corrosion, wherein the corrosion time is 6 min. And after corrosion, taking out the nickel wire corrosion net, cooling to room temperature, alternately cleaning with absolute ethyl alcohol and high-purity water, drying and packaging after multiple times of cleaning, and waiting for subsequent dislocation pit observation.
(3) And (3) dislocation observation: by observing with an optical metallographic microscope, the obtained dislocation morphology of the high-purity silicon carbide is shown in figure 1, the 3D morphology of dislocation etching pits is shown in figure 2, and the dislocation distribution map and the identification map are shown in figures 3 and 4.
As shown in FIGS. 1 to 4, in the high purity silicon carbide, hexagonal etch pits with an equal circle diameter of 40 to 50 μm correspond to TSD dislocations; circular etch pits with the equal circle diameter of 20-30 mu m correspond to TED dislocation; the water drop-shaped etch pits with the equal circle diameters of 20-30 μm correspond to BPD dislocations. The three kinds of dislocation have larger difference in appearance and size, and are easy to distinguish in the dislocation identification process. Dislocation line of BPD along crystal axis in identifying dislocation line of BPD
The direction is that the head of the etch pit is the exposed point of the BPD, and the tail is the deepened area of the etch pit, which can be used as one of the important bases for identifying the BPD dislocation in the silicon carbide crystal. Different types of dislocations are presented in etch pits with different shapes and sizes through dislocation etching, so that the dislocation identification has good identification degree.
Example 2: dislocation identification method of high-purity silicon carbide
This embodiment describes a dislocation identification method for high-purity silicon carbide, which includes the following steps:
(1) pretreatment: high-purity silicon carbide is firstly ground and polished according to a normal process, so that the silicon carbide has a flat and smooth surface. Then, ultrapure water is adopted to clean crystal surface particles, dilute hydrochloric acid is adopted to clean oil on the surface of the crystal, nitric acid (with the mass concentration of 5%) is adopted to pre-corrode the surface of the crystal, the pre-corrosion temperature is 25 ℃, and the nitric acid can also eliminate and treat scratches on the surface of the crystal; and finally, neutralizing and cleaning the pretreatment solution by respectively adopting hydrogen peroxide and sodium bicarbonate. And then, the wafer is cleaned and dried for many times by adopting ultrapure water, so that the pretreatment process is completed.
(2) Dislocation etching process: and (3) putting the KOH solid particles into a nickel crucible, and melting in a high-temperature resistance furnace, wherein the melting temperature is stable for 3.5 hours when reaching 520 ℃, so that the KOH is completely melted, and the physically adsorbed water in the KOH is discharged at high temperature. And then, placing the pretreated high-purity silicon carbide wafer in a dry nickel wire corrosion net, and immersing the silicon carbide wafer in molten KOH for corrosion, wherein the corrosion time is 6 min. And after corrosion, taking out the nickel wire corrosion net, cooling to room temperature, alternately cleaning with absolute ethyl alcohol and high-purity water, drying and packaging after multiple times of cleaning, and waiting for subsequent dislocation pit observation.
(3) And (3) dislocation observation: different types of dislocations are presented in etch pits with different shapes and sizes through dislocation etching, so that the dislocation identification has good identification degree; the edge dislocation, the screw dislocation and the basal plane dislocation in the high-purity silicon carbide can be accurately distinguished by observing through an optical metallographic microscope.
Example 3: dislocation identification method of high-purity silicon carbide
This embodiment describes a dislocation identification method for high-purity silicon carbide, which includes the following steps:
(1) pretreatment: high-purity silicon carbide is firstly ground and polished according to a normal process, so that the silicon carbide has a flat and smooth surface. Then, ultrapure water is adopted to clean crystal surface particles, dilute sulfuric acid is adopted to clean oil on the crystal surface, mixed liquid of hydrofluoric acid and nitric acid with the molar ratio of 6:1 is adopted to pre-corrode the crystal surface, the pre-corrosion temperature is 15 ℃, the mass concentration of the mixed liquid of hydrofluoric acid and nitric acid is 10%, and the mixed liquid of hydrofluoric acid and nitric acid can also eliminate and treat scratches on the crystal surface; and finally, neutralizing and cleaning the pretreatment solution by respectively adopting hydrogen peroxide and sodium bicarbonate. And then, the wafer is cleaned and dried for many times by adopting ultrapure water, so that the pretreatment process is completed.
(2) Dislocation etching process: and (3) putting the KOH solid particles into a nickel crucible, and melting in a high-temperature resistance furnace, wherein the melting temperature is stable for 2.5h when reaching 580 ℃, so that the KOH is completely melted, and the physically adsorbed water in the KOH is discharged at high temperature. And then, placing the pretreated high-purity silicon carbide wafer in a dry nickel wire corrosion net, and immersing the silicon carbide wafer in molten KOH for corrosion, wherein the corrosion time is 6 min. And after corrosion, taking out the nickel wire corrosion net, cooling to room temperature, alternately cleaning with absolute ethyl alcohol and high-purity water, drying and packaging after multiple times of cleaning, and waiting for subsequent dislocation pit observation.
(3) And (3) dislocation observation: different types of dislocations are presented in etch pits with different shapes and sizes through dislocation etching, so that the dislocation identification has good identification degree. The edge dislocation, the screw dislocation and the basal plane dislocation in the high-purity silicon carbide can be accurately distinguished by observing with naked eyes.
Example 4: dislocation identification method of nitrogen-doped silicon carbide
This embodiment describes a dislocation identification method for nitrogen-doped silicon carbide, which includes the following steps:
(1) pretreatment: the nitrogen-doped silicon carbide is firstly ground and polished according to the normal process, so that the silicon carbide has a flat and smooth surface. Then, ultrapure water is adopted to clean crystal surface particles, dilute sulfuric acid is adopted to clean oil on the crystal surface, hydrofluoric acid (with the mass concentration of 10%) is adopted to pre-corrode the crystal surface, the pre-corrosion temperature is 25 ℃, and the hydrofluoric acid can also eliminate and treat scratches on the crystal surface; and finally, neutralizing and cleaning the pretreatment solution by respectively adopting hydrogen peroxide and sodium bicarbonate. And then, the wafer is cleaned and dried for many times by adopting ultrapure water, so that the pretreatment process is completed. The pretreatment aims at cleaning the surface of a wafer to ensure that the surface of the wafer is free from large-particle pollution; and secondly, cleaning the surface scratches and the like of the glass. The pretreatment aims at cleaning the surface of a wafer to ensure that the surface of the wafer is free from large-particle pollution; secondly, the surface of the steel is pre-etched.
(2) Dislocation etching process: mixing KOH and Na2O2Putting the mixture into a nickel crucible according to the mass ratio of 50:8, uniformly stirring, and then melting in a high-temperature resistance furnace, wherein the melting temperature is stable for 3 hours when reaching 600 ℃, and KOH and Na are ensured2O2Completely melting and discharging KOH and Na at high temperature2O2Physically adsorb water. Then, the pretreated wafer is placed in a dry nickel wire corrosion net to put molten KOH and Na2O2And corroding in the mixed solution for 8 min. And after corrosion, taking out the nickel wire corrosion net, cooling to room temperature, alternately cleaning with absolute ethyl alcohol and high-purity water, drying and packaging after multiple times of cleaning, and waiting for subsequent dislocation pit observation.
(3) And (3) dislocation observation: by observation with an optical metallographic microscope, the obtained dislocation morphology of the nitrogen-doped silicon carbide is shown in fig. 5, the 3D morphology of the dislocation etch pits is shown in fig. 6, and the dislocation distribution map and the identification map are shown in fig. 7 and 8.
As shown in FIGS. 5 to 8, in the N-doped silicon carbide, the hexagonal etch pits with an equal circle diameter of 50 to 60 μm correspond to TSD dislocations; circular etch pits with the equal circle diameter of 10-20 mu m correspond to TED dislocation; the water drop-shaped etch pits with the equal circle diameters of 10-20 μm correspond to BPD dislocations. The three kinds of dislocation have larger difference in appearance and size, and are easy to distinguish in the dislocation identification process. In identifying dislocations for BPD, as shown in FIG. 9, the dislocation lines of BPD are along the crystal axis
The direction is that the head of the etch pit is the exposed point of the BPD, the tail is the deepened area of the etch pit, and the characteristic can be used as one of important bases for identifying the BPD in the silicon carbide, and is particularly remarkable in the silicon carbide crystal doped with nitrogen. Making different types of bits by dislocation etchingThe dislocations are shown in the etch pits with different shapes and sizes, so that the identification of the dislocations is provided with good identification degree.
Example 5: dislocation identification method of nitrogen-doped silicon carbide
This embodiment describes a dislocation identification method for nitrogen-doped silicon carbide, which includes the following steps:
(1) pretreatment: the nitrogen-doped silicon carbide is firstly ground and polished according to the normal process, so that the silicon carbide has a flat and smooth surface. Then, ultrapure water is adopted to clean crystal surface particles, dilute hydrochloric acid is adopted to clean oil on the surface of the crystal, nitric acid (with the mass concentration of 1%) is adopted to pre-corrode the surface of the crystal, the pre-corrosion temperature is 15 ℃, and the nitric acid can also eliminate scratches on the surface of the crystal; and finally, neutralizing and cleaning the pretreatment solution by respectively adopting hydrogen peroxide and sodium bicarbonate. And then, the wafer is cleaned and dried for many times by adopting ultrapure water, so that the pretreatment process is completed.
(2) Dislocation etching process: mixing KOH and Na2O2Putting the mixture into a nickel crucible according to the mass ratio of 50:8, uniformly stirring, and then melting in a high-temperature resistance furnace, wherein the melting temperature is stable for 3.5 hours when reaching 580 ℃, and KOH and Na are ensured2O2Completely melting and discharging KOH and Na at high temperature2O2Physically adsorb water. Then, the pretreated wafer is placed in a dry nickel wire corrosion net to put molten KOH and Na2O2And corroding in the mixed solution for 8 min. And after corrosion, taking out the nickel wire corrosion net, cooling to room temperature, alternately cleaning with absolute ethyl alcohol and high-purity water, drying and packaging after multiple times of cleaning, and waiting for subsequent dislocation pit observation.
(3) And (3) dislocation observation: different types of dislocations are presented in etch pits with different shapes and sizes through dislocation etching, so that the dislocation identification has good identification degree; the edge dislocation, the screw dislocation and the basal plane dislocation in the nitrogen-doped silicon carbide can be accurately distinguished by observing through an optical metallographic microscope.
Example 6: dislocation identification method of nitrogen-doped silicon carbide
This embodiment describes a dislocation identification method for nitrogen-doped silicon carbide, which includes the following steps:
(1) pretreatment: the nitrogen-doped silicon carbide is firstly ground and polished according to the normal process, so that the silicon carbide has a flat and smooth surface. Then, ultrapure water is adopted to clean crystal surface particles, dilute sulfuric acid is adopted to clean oil on the crystal surface, mixed liquid of hydrofluoric acid and nitric acid with the molar ratio of 8:1 is adopted to pre-corrode the crystal surface, the pre-corrosion temperature is 15 ℃, the mass concentration of the mixed liquid of hydrofluoric acid and nitric acid is 10%, the mixed liquid of hydrofluoric acid and nitric acid and the mixed liquid of hydrofluoric acid and nitric acid can also eliminate scratches on the crystal surface; and finally, neutralizing and cleaning the pretreatment solution by adopting hydrogen peroxide and sodium bicarbonate respectively. And then, the wafer is cleaned and dried for many times by adopting ultrapure water, so that the pretreatment process is completed.
(2) Dislocation etching process: mixing KOH and Na2O2Putting the mixture into a nickel crucible according to the mass ratio of 50:8, uniformly stirring, and then melting in a high-temperature resistance furnace, wherein the melting temperature is stable for 2.5 hours when reaching 620 ℃, so that KOH and Na are ensured2O2Completely melting and discharging KOH and Na at high temperature2O2Physically adsorb water. Then, the pretreated wafer is placed in a dry nickel wire corrosion net to put molten KOH and Na2O2And corroding in the mixed solution for 8 min. And after corrosion, taking out the nickel wire corrosion net, cooling to room temperature, alternately cleaning with absolute ethyl alcohol and high-purity water, drying and packaging after multiple times of cleaning, and waiting for subsequent dislocation pit observation.
(3) And (3) dislocation observation: different types of dislocations are presented in etch pits with different shapes and sizes through dislocation etching, so that the dislocation identification has good identification degree. The edge dislocation, the screw dislocation and the basal plane dislocation in the high-purity silicon carbide can be accurately distinguished by observing with naked eyes.
Experimental example 1: selection of high purity silicon carbide etch time
The etching process of the high-purity silicon carbide is optimized by a controlled variable method, the etching time of the high-purity silicon carbide is 4, 6, 8 and 10min at 550 ℃, and the obtained comparison graph is shown in figure 10.
As shown in FIG. 10, dislocations gradually appear with the increase of etching time, and when the etching time reaches 6min, the dislocations are basically all shown in the form of etch pits with different morphologies. And with the further extension of the corrosion time, the TED circular corrosion pit is gradually hexagonally formed, the size of the corrosion pit is gradually increased, and when the corrosion time reaches 10min, the size of the TED corrosion pit is close to that of the TSD corrosion pit. Therefore 6min was chosen as the optimum etch time for high purity silicon carbide.
Example 2: optimization of high-purity silicon carbide corrosion conditions
And a corrosion test is carried out by adopting a variable control method to regulate and control the size of the corrosion pit. For the wafers obtained by the same batch growth, KOH and Na with different proportions are adopted under the same etching time (8min)2O2Etching with an etchant of KOH and Na2O2The mass ratios of (a) to (b) are 50:6, 50:8 and 50:10, respectively, and the appearance of dislocation etch pits is shown in fig. 11.
As shown in FIG. 11, when KOH and Na are used2O2When the mass ratio is 50:6, the dislocation corrosion pit is smaller, and part of dislocation is not shown due to shorter corrosion time; when KOH and Na2O2When the mass ratio is 50:8, most dislocations are shown through alkaline corrosion, TSD is a large-size hexagonal corrosion pit, TED is a small-size circular corrosion pit, BPD is a small-size drop-shaped corrosion pit, and the three dislocations have obvious morphological characteristics and larger discrimination; when KOH and Na2O2When the mass ratio is 50:10, the dislocation etch pit size is too large due to too high alkalinity in the etching process, so that the etch pit accumulation and adhesion are shown in a visual field, and the state is not beneficial to the subsequent dislocation identification and the number density statistics.
For the same region on the same wafer, we used KOH and Na selection at 600 deg.C2O2The etchant with the mass ratio of 50:8 performs etching for 2, 4, 6, 8 and 10min, and a comparison diagram of dislocations after etching is shown in fig. 12.
As shown in fig. 12, when the etching time was 2, 4, and 6min, the etch pit size was small and some dislocations were not yet present, and it was difficult to distinguish and count dislocations. When the corrosion time is 8min, the size of the corrosion pits is moderate, and the distribution of the corrosion pits is relatively uniform. Meanwhile, the difference of the etch pits of different dislocations in size and appearance is obvious, which is beneficial to the subsequent automatic identification and quantity statistical calculation of different dislocations. When the etching time is 10min, accumulation and adhesion conditions shown by overlarge etch pits gradually appear due to excessive etching, which is not beneficial to the subsequent dislocation distinguishing and counting, and therefore 8min is selected as the optimal etching time.
The above description is only an example of the present application, and the protection scope of the present application is not limited by these specific examples, but is defined by the claims of the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the technical idea and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. A method for identifying dislocations in a silicon carbide crystal, the method comprising the steps of:
(1) corroding the silicon carbide crystal in an alkaline corrosive agent;
(2) observing the appearance of the dislocation etch pits after etching is finished, so as to identify edge dislocations, screw dislocations and basal plane dislocations in the silicon carbide crystal;
the silicon carbide crystals comprise high-purity silicon carbide and nitrogen-doped silicon carbide, wherein the corrosion time of the high-purity silicon carbide is 5-7 min, and the corrosion time of the nitrogen-doped silicon carbide is 7-9 min.
2. The method for dislocation identification of a silicon carbide crystal according to claim 1, wherein the etching time of the high purity silicon carbide is 6min and the etching time of the nitrogen doped silicon carbide is 8 min.
3. The dislocation identification method of silicon carbide crystals according to claim 1, wherein in the step (1), when the high-purity silicon carbide is etched, the alkaline etchant comprises KOH, and the temperature of the etching is 500-600 ℃;
preferably, when the high-purity silicon carbide is corroded, the corrosion temperature is 520-580 ℃;
more preferably, when the high purity silicon carbide is etched, the temperature of the etching is 550 ℃.
4. The dislocation identification method of silicon carbide crystals as claimed in claim 1, wherein in step (1), when the nitrogen-doped silicon carbide is etched, the alkaline etchant comprises KOH and Na2O2KOH and Na2O2The mass ratio of the components is 50: 7-9, and the corrosion temperature is 550-650 ℃;
preferably, KOH and Na2O2In a mass ratio of 50: 8;
preferably, when the nitrogen-doped silicon carbide is etched, the etching temperature is 580-620 ℃;
more preferably, when the nitrogen-doped silicon carbide is etched, the temperature of the etching is 600 ℃.
5. A dislocation identification method for silicon carbide crystals according to any one of claims 1 to 4, wherein in the step (1), before etching, the surface of the silicon carbide crystal is subjected to polishing and cleaning;
preferably, the particles and grease on the surface of the silicon carbide crystal are cleaned;
preferably, after the cleaning treatment, the surface of the silicon carbide crystal is pre-etched by using hydrofluoric acid and/or nitric acid;
more preferably, the pre-corrosion temperature is 15-25 ℃.
6. A dislocation identification method for silicon carbide crystals according to any one of claims 1 to 4, wherein in step (2), said observation is direct visual observation or observation by means of a microscope.
7. A dislocation identification method for a silicon carbide crystal according to claim 1, wherein in the high purity silicon carbide in the step (2), hexagonal etch pits having an equivalent circle diameter of 40 to 50 μm correspond to threading dislocations, circular etch pits having an equivalent circle diameter of 20 to 30 μm correspond to edge dislocations, and drop-shaped etch pits having an equivalent circle diameter of 20 to 30 μm correspond to basal plane dislocations.
8. A dislocation identification method for a silicon carbide crystal according to claim 1, wherein in the step (2), hexagonal etch pits having an equivalent circle diameter of 50 to 60 μm correspond to threading dislocations, circular etch pits having an equivalent circle diameter of 10 to 20 μm correspond to edge dislocations, and drop-shaped etch pits having an equivalent circle diameter of 10 to 20 μm correspond to basal plane dislocations.
9. The method for identifying dislocations in a silicon carbide crystal according to claim 7 or 8, wherein the dislocation line direction in the high purity silicon carbide and/or the nitrogen doped silicon carbide is along the crystal axis
And the direction is that the head part of the etch pit is an exposed point of dislocation, and the tail part of the etch pit is a deepened area, so that the substrate plane dislocation is correspondingly formed.
10. A dislocation etchant for a silicon carbide crystal, the etchant comprising KOH and Na2O2KOH and Na2O2The mass ratio of (A) to (B) is 50: 7-9;
preferably, KOH and Na2O2In a mass ratio of 50: 8;
preferably, the silicon carbide crystal is nitrogen-doped silicon carbide.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000100680A (en) * | 1998-07-23 | 2000-04-07 | Canon Inc | Semiconductor base material and manufacture thereof |
| JP2008028178A (en) * | 2006-07-21 | 2008-02-07 | Toyota Motor Corp | Evaluation method of single crystal substrate |
| US20080213536A1 (en) * | 2004-08-24 | 2008-09-04 | Bridgestone Corporation | Silicon Carbide Single Crystal Wafer and Method for Manufacturing the Same |
| JP2010219459A (en) * | 2009-03-19 | 2010-09-30 | Toyota Central R&D Labs Inc | Method and device for specifying kind of dislocation present in semiconductor layer |
| JP2013211547A (en) * | 2012-03-02 | 2013-10-10 | Toyota Motor Corp | Inspection method of sic crystal and process of manufacturing sic crystal using the same |
| JP2015059072A (en) * | 2013-09-20 | 2015-03-30 | 新日鉄住金マテリアルズ株式会社 | Silicon carbide single crystal wafer and method of manufacturing silicon carbide single crystal ingot |
| CN104900758A (en) * | 2015-05-25 | 2015-09-09 | 连云港市产品质量监督检验中心 | Method for detecting microdefects of quasi monocrystalline silicon sheets |
| CN106711031A (en) * | 2016-12-15 | 2017-05-24 | 中国电子科技集团公司第五十五研究所 | Method for reducing effect of base plane dislocation on silicon carbide epitaxial layer |
| CN108169228A (en) * | 2017-11-28 | 2018-06-15 | 中国工程物理研究院电子工程研究所 | A kind of method of accurate discrimination single-crystal silicon carbide Types of Dislocations |
| CN110541199A (en) * | 2019-10-11 | 2019-12-06 | 山东大学 | Preparation method of high-quality SiC seed crystal with diameter of 8 inches or more |
-
2020
- 2020-01-15 CN CN202010042808.1A patent/CN111238910A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000100680A (en) * | 1998-07-23 | 2000-04-07 | Canon Inc | Semiconductor base material and manufacture thereof |
| US20080213536A1 (en) * | 2004-08-24 | 2008-09-04 | Bridgestone Corporation | Silicon Carbide Single Crystal Wafer and Method for Manufacturing the Same |
| JP2008028178A (en) * | 2006-07-21 | 2008-02-07 | Toyota Motor Corp | Evaluation method of single crystal substrate |
| JP2010219459A (en) * | 2009-03-19 | 2010-09-30 | Toyota Central R&D Labs Inc | Method and device for specifying kind of dislocation present in semiconductor layer |
| JP2013211547A (en) * | 2012-03-02 | 2013-10-10 | Toyota Motor Corp | Inspection method of sic crystal and process of manufacturing sic crystal using the same |
| JP2015059072A (en) * | 2013-09-20 | 2015-03-30 | 新日鉄住金マテリアルズ株式会社 | Silicon carbide single crystal wafer and method of manufacturing silicon carbide single crystal ingot |
| CN104900758A (en) * | 2015-05-25 | 2015-09-09 | 连云港市产品质量监督检验中心 | Method for detecting microdefects of quasi monocrystalline silicon sheets |
| CN106711031A (en) * | 2016-12-15 | 2017-05-24 | 中国电子科技集团公司第五十五研究所 | Method for reducing effect of base plane dislocation on silicon carbide epitaxial layer |
| CN108169228A (en) * | 2017-11-28 | 2018-06-15 | 中国工程物理研究院电子工程研究所 | A kind of method of accurate discrimination single-crystal silicon carbide Types of Dislocations |
| CN110541199A (en) * | 2019-10-11 | 2019-12-06 | 山东大学 | Preparation method of high-quality SiC seed crystal with diameter of 8 inches or more |
Non-Patent Citations (6)
| Title |
|---|
| X.F. LIU ET AL: "Defect appearance on 4H-SiC homoepitaxial layers via molten KOH etching", 《JOURNAL OF CRYSTAL GROWTH》 * |
| X.F. LIU ET AL: "Defect appearance on 4H-SiC homoepitaxial layers via molten KOH etching", 《JOURNAL OF CRYSTAL GROWTH》, vol. 531, 14 November 2019 (2019-11-14), pages 1 - 2, XP085970663, DOI: 10.1016/j.jcrysgro.2019.125359 * |
| YONG-ZHAO YAO ET AL: ""Molten KOH Etching with Na2O2 Additive for Dislocation Revelation in 4H-SiC Epilayers and Substrates", 《JAPANESE JOURNAL OF APPLIED PHYSICS》 * |
| YONG-ZHAO YAO ET AL: ""Molten KOH Etching with Na2O2 Additive for Dislocation Revelation in 4H-SiC Epilayers and Substrates", 《JAPANESE JOURNAL OF APPLIED PHYSICS》, vol. 50, 20 July 2011 (2011-07-20), pages 1 - 2 * |
| YONG-ZHAO YAO ET AL: "Molten KOH Etching with Na2O2 Additive for Dislocation Revelation in 4H-SiC Epilayers and Substrates", 《JAPANESE JOURNAL OF APPLIED PHYSICS》 * |
| YONG-ZHAO YAO ET AL: "Molten KOH Etching with Na2O2 Additive for Dislocation Revelation in 4H-SiC Epilayers and Substrates", 《JAPANESE JOURNAL OF APPLIED PHYSICS》, vol. 50, 20 July 2011 (2011-07-20), pages 1 - 2 * |
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