CN117110337A - Method for testing orientation of main reference surface of silicon carbide crystal - Google Patents

Method for testing orientation of main reference surface of silicon carbide crystal Download PDF

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CN117110337A
CN117110337A CN202311069490.6A CN202311069490A CN117110337A CN 117110337 A CN117110337 A CN 117110337A CN 202311069490 A CN202311069490 A CN 202311069490A CN 117110337 A CN117110337 A CN 117110337A
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silicon carbide
ray
crystal
carbide crystal
orientation
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吴殿瑞
彭红宇
刘旭
付健行
李宝盛
李祥皓
杨方慧
宋生
梁庆瑞
刘家朋
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Shandong Tianyue Advanced Technology Co Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions

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  • Crystallography & Structural Chemistry (AREA)
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Abstract

The application discloses a method for testing the orientation of a main reference surface of a silicon carbide crystal, which comprises the following steps: 1) Selecting a (11-28) crystal face as a reference face, and calculating a Bragg diffraction angle theta of the crystal face; 2) Adjusting an X-ray orientation system, and selecting a normal line to enable an intersection point of an incident ray emitted by the orientation system and a reflection line to be focused on a central point of the top surface of the silicon carbide crystal; the included angle between the incident ray and the (11-28) crystal face and the included angle between the reflecting ray and the (11-28) crystal face are theta, the plane where the incident ray and the reflecting ray are positioned is parallel to the (1-100) crystal face of the silicon carbide crystal, and the X-ray orientation system displays a first signal intensity value; 3) And then rotating the test bench, wherein when the signal intensity value displayed by the X-ray orientation system is maximum relative to the first signal intensity value, the rotation angle of the test bench is the deviation value of the orientation of the main reference surface of the silicon carbide crystal. The method is applicable to silicon carbide crystals with different thicknesses, fills the blank that the silicon carbide substrate cannot be tested, and widens the detection range.

Description

Method for testing orientation of main reference surface of silicon carbide crystal
Technical Field
The application relates to a method for testing the orientation of a main reference surface of a silicon carbide crystal, and belongs to the technical field of semiconductor crystal performance testing.
Background
The test of the deviation value of the orientation of the main reference plane of the silicon carbide substrate, particularly the deviation value of the orientation of the NOTCH edge, is an important control point in the processing of the silicon carbide substrate, and the parameter is related to the problem of positioning the silicon carbide crystal, and if the deviation is excessive, the problems of deviation of the position of the silicon carbide crystal, deviation of the crystal orientation of the surface, overlarge deviation of the orthogonal orientation and the like can be caused, so that the deviation value of the orientation of the main reference plane is a test which is necessary to be performed in the processing of the silicon carbide substrate.
The current test of the deviation value of the orientation of the main reference surface is generally focused on the crystal bar stage of silicon carbide processing, and an X-ray orientation instrument is used for directly detecting the side surface of the crystal bar, namely the position of the main reference surface, or detecting the opposite surface of a NOTCH edge or the direction of 90 degrees. The limitation of the detection method is that the method is only suitable for testing the silicon carbide crystal bar with a certain length, but the silicon carbide substrate test belongs to a blank area, because the thickness of the silicon carbide substrate (corresponding to the length of the silicon carbide crystal bar) is thinner, and the detection can not be performed on the side face of the silicon carbide substrate.
The X-ray test needs to be focused on a certain surface, the main reference surface is vertical to the upper surface and the lower surface of the crystal bar, namely the side surface of the crystal bar, the test can be directly performed only from the side surface, and for a thinner substrate, the side surface is very thin and only has the thickness of 350-500 mu m, so that the test cannot be performed. And for NOTCH edge testing, the NOTCH edge or the 90-degree side surface needs to be used for measurement, and only the NOTCH edge of the silicon carbide crystal bar can be tested. In addition, in the conventional method, referring to fig. 1, since the measurement is performed by using a side surface, the accuracy is difficult to ensure, two values must be tested for the test of the main reference surface to determine the deviation value of the orientation of the main reference surface, and particularly for the measurement of the NOTCH edge, only the opposite or 90-degree arc surface is used for the test, so that the inaccuracy is further increased and the efficiency is low. The common X-ray direction finder has no test adaptation platform for testing, is inconvenient to operate, needs to hold or customize tools in addition, is incompatible with normal surface orientation test, needs to switch the tools back and forth, is poor in equipment compatibility degree, causes time increase and efficiency reduction.
In addition, a laboratory uses a method for testing the fault angle to test the orientation of the main reference surface of the silicon carbide crystal, but the testing mode is only suitable for testing the orientation of the silicon carbide crystal rod, and is not fully applicable to the silicon carbide substrate, because the thickness of the silicon carbide substrate is thinner, faults are not necessarily generated, and the problem that the fault exists and the test cannot be complemented is solved.
Disclosure of Invention
In order to solve at least one of the problems, a method for testing the orientation of a main reference surface of a silicon carbide crystal is provided, and the testing method does not need to select the side surface of the silicon carbide crystal as a testing surface, so that the method can be suitable for silicon carbide crystals with different thicknesses, and particularly fills the blank that a sheet silicon carbide substrate cannot be tested, and greatly widens the detection range; because the test surface is a plane instead of the side surface with an arc-shaped curved surface, the test point is easy to be positioned, thereby greatly improving the test accuracy and saving the test time; the test method does not need special tools, greatly simplifies operation, does not need special change to a common test instrument, increases detection efficiency and universality, can be carried out on silicon carbide crystals, and is suitable for industrial test of the silicon carbide crystals.
The technical scheme provided by the application is as follows:
a method of testing the orientation of a principal reference plane of a silicon carbide crystal, comprising the steps of:
1) Horizontally placing a silicon carbide crystal to be detected on a test bench, selecting a (11-28) crystal face of the silicon carbide crystal as a reference face, and calculating a Bragg diffraction angle theta of the (11-28) crystal face;
2) Adjusting an X-ray orientation system, and selecting a straight line passing through the central point of the top surface of the silicon carbide crystal and perpendicular to the (11-28) crystal face as a normal line, so that the intersection point of the incident ray emitted by the X-ray orientation system and the reflection line is focused on the central point of the top surface of the silicon carbide crystal;
the included angle between the incident ray and the (11-28) crystal face and the included angle between the reflecting ray and the (11-28) crystal face are theta, the plane where the incident ray and the reflecting ray are located is parallel to the (1-100) crystal face of the silicon carbide crystal, and the X-ray orientation system displays a first signal intensity value at the moment;
3) And then horizontally rotating the test bench in a clockwise and/or anticlockwise direction, wherein when the signal intensity value displayed by the X-ray orientation system is maximum relative to the first signal intensity value, the rotation angle of the test bench is the deviation value of the orientation of the main reference surface of the silicon carbide crystal.
Optionally, in step 1), the method for calculating the bragg diffraction angle θ of the (11-28) crystal plane is as follows:
2dsin(θ)＝nλ
wherein lambda is the wavelength of X rays, the materials of X rays emitted by the X ray orientation system are copper target structures, and the materials are fixed values;
n is a positive natural number; d is the distance value between the (11-28) crystal faces,
calculated, the Bragg diffraction angle θ of the (11-28) crystal plane is equal to 52.5++0.5°.
Optionally, in step 2), the angle of the incident line to the test bench is 9 ° ± 1 °;
the angle between the reflection line and the test bench is 96 degrees plus or minus 1 degree.
Optionally, the X-ray orientation system comprises an X-ray emitting unit for emitting an incident ray, an X-ray receiving unit for receiving a reflected ray, and a signal intensity monitoring unit;
step 2) further comprises a first arcuate scan: and taking the center point of the top surface of the silicon carbide crystal as a circle center, taking the distance from the X-ray emission unit to the center point as a radius, and taking the top surface of the silicon carbide crystal as a 0-degree reference surface, so that the X-ray emission unit performs first arc scanning on a plane where the incident ray and the reflection line are located, wherein the first arc scanning range is 9+/-1 degrees, and in the first arc scanning process, when the signal intensity monitoring unit displays the highest signal peak, the X-ray emission unit is adjusted to be at the position.
Optionally, step 2) further comprises a second arc scan: and taking the center point of the top surface of the silicon carbide crystal as a circle center, taking the distance from the X-ray receiving unit to the center point as a radius, and taking the top surface of the silicon carbide crystal as a 0-degree reference surface, so that the X-ray receiving unit performs a second arc scanning on the plane where the incident ray and the reflection line are located, wherein the second arc scanning range is 96 degrees+/-1 degrees, and when the signal intensity monitoring unit displays the highest signal peak, the X-ray receiving unit is adjusted to be at the position.
Optionally, in step 2), the angle of the incident line to the test bench is 96 ° ± 1 °;
the angle between the reflection line and the test bench is 9 degrees plus or minus 1 degree.
Optionally, the X-ray orientation system comprises an X-ray emitting unit for emitting an incident ray, an X-ray receiving unit for receiving a reflected ray, and a signal intensity monitoring unit;
step 2) further comprises a first arcuate scan: and taking the center point of the top surface of the silicon carbide crystal as a circle center, taking the distance from the X-ray emission unit to the center point as a radius, and taking the top surface of the silicon carbide crystal as a 0-degree reference surface, so that the X-ray emission unit performs first arc scanning on a plane where the incident ray and the reflection line are located, wherein the first arc scanning range is 96+/-1 degrees, and in the first arc scanning process, when the signal intensity monitoring unit displays the highest signal peak, the X-ray emission unit is adjusted to be at the position.
Optionally, step 2) further comprises a second arc scan: and taking the center point of the top surface of the silicon carbide crystal as a circle center, taking the distance from the X-ray receiving unit to the center point as a radius, and taking the top surface of the silicon carbide crystal as a 0-degree reference surface, so that the X-ray receiving unit performs a second arc scanning on the plane where the incident ray and the reflection line are located, wherein the second arc scanning range is 9+/-1 degrees, and when the signal intensity monitoring unit displays the highest signal peak, the X-ray receiving unit is adjusted to be at the position.
Optionally, adjusting the height of the test bench, and fixing the test bench at the height when the first signal intensity value is displayed to be maximum;
and then horizontally rotating the test bench along the clockwise and/or anticlockwise direction, wherein the rotating angle range is +/-3 degrees, and the rotating angle of the test bench is the deviation value of the main reference plane orientation of the silicon carbide crystal when the signal intensity value displayed by the X-ray orientation system is maximum relative to the first signal intensity value in the angle range.
Optionally, repeating the first arc scan, the second arc scan, adjusting the height of the test bench, and horizontally rotating the test bench in the clockwise and/or counterclockwise directions for a plurality of times, wherein the angle of rotation of the test bench for the last time is the deviation value of the orientation value of the main reference surface of the final silicon carbide crystal.
Optionally, the silicon carbide crystal itself has an inclination angle of 0 ° to 4 °;
the included angle between the (11-28) crystal face and the (0001) crystal face of the silicon carbide crystal is 39.5 degrees plus or minus 0.5 degrees.
Optionally, the silicon carbide crystal is a silicon carbide substrate, a silicon carbide crystal rod, a silicon carbide grinding sheet or a silicon carbide polishing sheet.
Optionally, the X-ray orientation system is an X-ray diffractometer or an X-ray orientation instrument.
The beneficial effects of the application include, but are not limited to:
according to the method for testing the orientation of the main reference surface of the silicon carbide crystal, the (11-28) crystal face is selected as the reference surface, the Bragg diffraction angle theta of the crystal face is calculated, and the top surface of the silicon carbide crystal is selected as the test surface, so that the method can be suitable for silicon carbide crystals with different thicknesses, and particularly fills the blank that a sheet silicon carbide substrate cannot be tested, and greatly widens the detection range.
Because the test surface is a plane instead of the side surface with an arc-shaped curved surface, the test point is easy to be positioned, thereby greatly improving the test accuracy and saving the test time.
The test method does not need special tools, greatly simplifies operation, does not need special change to a common test instrument, increases detection efficiency and universality, can be carried out on silicon carbide crystals, and is suitable for industrial test of the silicon carbide crystals.
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 specification, illustrate embodiments of the application and together with the description serve to explain the application and do not constitute a limitation on the application. In the drawings:
FIG. 1 is a schematic diagram of a conventional method for testing the orientation of a principal reference plane of a silicon carbide crystal in accordance with the background of the application.
FIG. 2 is a schematic illustration of a test silicon carbide crystal primary reference plane orientation in accordance with an embodiment of the present application.
FIG. 3 is a schematic view of the test angles involved in FIG. 2 for testing the orientation of the principal reference planes of silicon carbide crystals.
FIG. 4 is a schematic view of another test angle for testing the orientation of the principal reference plane of a silicon carbide crystal according to an embodiment of the present application.
11. A main reference plane (silicon carbide crystal side), 12. Silicon carbide crystal top, 13. X-ray emitting unit, 14. X-ray receiving unit, 15. Incident ray, 16. Reflected ray,
21. (0001) Crystal plane, 22 (11-20) crystal plane, 23 (1-100) crystal plane, 24 (11-28) crystal plane, 25 [1-100] crystal orientation, 26 [11-20] crystal orientation,
31. silicon carbide crystal, 32. Normal, 33. Silicon carbide substrate itself tilt angle, 34 angle between (11-28) crystal plane and (0001) crystal plane.
Detailed Description
The present application is described in detail below with reference to examples, but the present application is not limited to these examples.
The embodiment provides a method for testing the orientation of a main reference surface of a silicon carbide crystal, which comprises the following steps:
1) Placing the silicon carbide crystal to be inspected horizontally on a test bench such that the main reference surface 11 of the silicon carbide crystal is perpendicular to the test bench, where the main reference surface 11 of the silicon carbide crystal is the side of the silicon carbide crystal; selecting a (11-28) crystal face 24 of the silicon carbide crystal as a reference plane, and calculating a Bragg diffraction angle theta of the (11-28) crystal face 24;
the Bragg diffraction angle theta of the (11-28) crystal face of the silicon carbide crystal is calculated as follows:
2dsin(θ)＝nλ
wherein lambda is the wavelength value of an X-ray copper target, and the materials of the X-ray directional system for emitting X-rays are copper target structures, which are constant values of 1.54056 angstroms;
n is a positive natural number 1; d has a value of the (11-28) interplanar spacing of about 0.97 angstroms,
calculated, the Bragg diffraction angle theta of the (11-28) crystal plane is equal to 52.5 DEG + -0.5 DEG, namely 2 theta is equal to 105 DEG + -1 DEG, and a range value is fixed because the calculated 2 theta is not an integer; preferably, 2 theta is about 104 DEG to 105 deg.
2) Adjusting an X-ray orientation system, referring to fig. 2 and 3, selecting a straight line passing through the center point of the top surface of the silicon carbide crystal and perpendicular to the (11-28) crystal face 24 as a normal line 32, so that the intersection point of an incident ray 15 emitted by the X-ray orientation system and a reflection line 16 is focused on the center point of the top surface of the silicon carbide crystal;
the included angle between the incident ray 15 and the (11-28) crystal face 24 and the included angle between the reflection ray 16 and the (11-28) crystal face 24 are both theta angles, the plane where the incident ray 15 and the reflection ray 16 are located is parallel to the (1-100) crystal face 23 of the silicon carbide crystal, and the X-ray orientation system displays a first signal intensity value at the moment;
3) And then horizontally rotating the test bench in a clockwise and/or anticlockwise direction, wherein when the signal intensity value displayed by the X-ray orientation system is maximum relative to the first signal intensity value, the rotation angle of the test bench is the deviation value of the orientation of the main reference surface of the silicon carbide crystal.
If the main reference surface of the silicon carbide crystal is not inclined during processing, a plane formed by an incident ray 15 emitted by the X-ray orientation system and a received reflection ray 16 is perpendicular to a (11-28) crystal face 24, and the signal intensity value is the largest at the moment, namely, the rotation angle of the test bench is 0 DEG, and the signal intensity value is a first signal intensity value at the moment;
if the main reference plane of the silicon carbide crystal is deflected during processing, the (11-28) crystal plane 24 is deflected, the test signal intensity is not maximum, the test bench is horizontally rotated clockwise and/or anticlockwise, the strongest signal intensity is found, the plane formed by the incident ray 15 emitted by the X-ray orientation system and the received reflection line 16 is perpendicular to the (11-28) crystal plane 24, namely, the angle of deflection of the (11-28) crystal plane by rotating the test bench, namely, the deflection angle of the (11-28) crystal plane and the (1-100) crystal plane is perpendicular, namely, the deflection angle of the main reference plane 11 of the silicon carbide crystal and the (1-100) crystal plane 23, namely, the deflection value of the orientation of the main reference plane 11 of the silicon carbide crystal.
The included angle 34 between the (11-28) crystal face 24 of the silicon carbide crystal and the (0001) crystal face 21 of the silicon carbide crystal is 39.5 degrees + -0.5 degrees, and in the method for testing the orientation of the principal reference plane of the silicon carbide crystal, in actual operation, it is not easy to precisely find the reference plane (11-28) crystal face 24, and a certain operation error may exist.
Thus, in one embodiment, the reference plane (11-28) crystal plane 24 is converted to a horizontal plane as the reference plane. The method comprises the following steps:
in step 2), the angle of the incident line 15 to the test bench is 9°±1°;
the angle of the reflection line 16 to the test bench is 96 deg. + -1 deg., the test bench is parallel to the horizontal plane, and the (0001) crystal plane is also parallel to the horizontal plane.
Referring to fig. 3, an included angle between an incident line and a test bench is defined as +.1, and +.1 is also an included angle between the incident line and a (0001) crystal plane, an included angle between a reflected line and the test bench is defined as +.2, and +.2 is also an included angle between the reflected line and the (0001) crystal plane, and the calculation modes of +.1 and +.2 are as follows:
∠1＝∠θ-(39.5°±0.5°)-4°＝9°±1°
∠2＝∠θ+(39.5°±0.5°)+4°＝96°±1°
where 4 is the tilt angle 33 of the silicon carbide crystal itself, typically the tilt angle 33 of the silicon carbide crystal itself is 0-4, calculated here by way of example as 4.
The reference plane (11-28) crystal plane 25 is converted into a horizontal plane to be used as a reference plane, and the test method is as follows:
in one embodiment, referring to fig. 2 and 3:
the X-ray orientation system comprises an X-ray emitting unit 13 for emitting an incident ray, an X-ray receiving unit 14 for receiving a reflected ray, and a signal intensity monitoring unit (not shown in the figure);
after horizontally placing the silicon carbide crystal to be inspected on a test bench, the following steps (1) - (4) are performed:
step (1): adjusting the X-ray emitting unit 13 to perform a first arc scan: the center point of the top surface of the silicon carbide crystal 31 is used as the center point, the distance from the X-ray emission unit 13 to the center point is used as the radius, the top surface of the silicon carbide crystal is used as a 0-degree reference surface (the top surface of the silicon carbide crystal is parallel to the test table and is a horizontal plane), so that the X-ray emission unit 13 performs a first arc scanning on the plane where the incident ray 15 and the reflected ray 16 are located, the first arc scanning range is 9+/-1 degrees, and the X-ray emission unit 13 is adjusted at the position when the signal intensity monitoring unit displays the highest signal peak in the first arc scanning process.
Step (2): adjusting the X-ray receiving unit 14 to perform a second arc scan: the center point of the top surface of the silicon carbide crystal 31 is used as the center point, the distance from the X-ray receiving unit to the center point is used as the radius, the top surface of the silicon carbide crystal is used as a 0-degree reference surface (the top surface of the silicon carbide crystal is parallel to the test table and is a horizontal surface), so that the X-ray receiving unit 14 performs a second arc scanning on the plane where the incident line 15 and the reflection line 16 are located, the second arc scanning range is 96 DEG + -1 DEG, and when the signal intensity monitoring unit displays the highest peak of the signal, the X-ray receiving unit 14 is adjusted at the position.
Step (3): adjusting the height of the test bench, and fixing the test bench at the height when the first signal intensity value is displayed to be maximum;
step (4): and then horizontally rotating the test bench in the clockwise and/or anticlockwise directions, wherein the rotating angle range is +/-3 degrees, and the rotating angle of the test bench is the deviation value of the orientation of the main reference surface 11 of the silicon carbide crystal when the signal intensity value displayed by the X-ray orientation system is maximum relative to the first signal intensity value.
During rotation of the test table, when the maximum value of the signal intensity value displayed by the X-ray orientation system is the first signal intensity value, the main reference surface 11 of the silicon carbide crystal is not inclined during processing, and the deviation value of the orientation of the main reference surface 11 of the silicon carbide crystal is 0 degrees.
Repeating the steps (1) - (4) again, adjusting each parameter again, and obtaining a deviation value again more accurately, if a higher-precision test is needed, repeating the steps (1) - (4) only for several times, and adjusting the parameter range each time to obtain a more accurate deviation value.
In another embodiment, the X-ray emitting unit 13 and the X-ray receiving unit 14 in fig. 2 and 3 are exchanged, and referring to fig. 4, a test of the orientation of the silicon carbide crystal main reference surface 11 can be achieved as well, specifically as follows:
in the step 2), the angle between the incident line 15 and the test bench is 96 degrees plus or minus 1 degree;
the angle of the reflection line 16 to the test bench is 9 deg. + -1 deg..
The included angle between the incident ray and the test bench is defined as < 1 >, the included angle between the reflected ray and the test bench is defined as < 2 >, and the calculation modes of < 1 and < 2 are as follows:
∠1＝∠θ+(39.5°±0.5°)+4°＝96°±1°
∠2＝∠θ-(39.5°±0.5°)-4°＝9°±1°
where 4 is the tilt angle 33 of the silicon carbide crystal itself, typically the tilt angle 33 of the silicon carbide crystal itself is 0-4, calculated here by way of example as 4.
The reference plane (11-28) crystal plane 24 is converted into a horizontal plane to be used as a reference plane, and the test method is as follows:
after horizontally placing the silicon carbide crystal to be inspected on a test bench, the following steps (1) - (4) are performed:
step (1): adjusting the X-ray emitting unit 13 to perform a first arc scan: the center point of the top surface of the silicon carbide crystal 31 is used as the center point, the distance from the X-ray emission unit 13 to the center point is used as the radius, the top surface of the silicon carbide crystal is used as a 0-degree reference surface (the top surface of the silicon carbide crystal is parallel to the test table and is a horizontal plane), so that the X-ray emission unit 13 performs a first arc scanning on the plane where the incident ray 15 and the reflected ray 16 are located, the first arc scanning range is 96 DEG+/-1 DEG, and the X-ray emission unit 13 is adjusted at the position when the signal intensity monitoring unit displays the highest signal peak in the first arc scanning process.
Step (2): adjusting the X-ray receiving unit 14 to perform a second arc scan: the center point of the top surface of the silicon carbide crystal 31 is used as a center, the distance from the X-ray receiving unit 14 to the center point is used as a radius, and the top surface of the silicon carbide crystal 31 is used as a 0-degree reference surface (the top surface of the silicon carbide crystal is parallel to the test table and is a horizontal plane), so that the X-ray receiving unit 14 performs a second arc scanning on the plane where the incident ray 15 and the reflected ray 16 are located, the second arc scanning range is 9 DEG + -1 DEG, and when the signal intensity monitoring unit displays the highest peak of the signal, the X-ray receiving unit 14 is adjusted at the position.
Step (3): adjusting the height of the test bench, and fixing the test bench at the height when the first signal intensity value is displayed to be maximum;
step (4): and then horizontally rotating the test bench in the clockwise and/or anticlockwise directions, wherein the rotating angle range is +/-3 degrees, and the rotating angle of the test bench is the deviation value of the orientation of the main reference surface of the silicon carbide crystal when the signal intensity value displayed by the X-ray orientation system is maximum relative to the first signal intensity value.
During rotation of the test table, when the maximum value of the signal intensity value displayed by the X-ray orientation system is the first signal intensity value, the main reference surface 11 of the silicon carbide crystal is not inclined during processing, and the deviation value of the orientation of the main reference surface 11 of the silicon carbide crystal is 0 degrees.
Repeating the steps (1) - (4) again, adjusting each parameter again, and obtaining a deviation value again more accurately, if a higher-precision test is needed, repeating the steps (1) - (4) only for several times, and adjusting the parameter range each time to obtain a more accurate deviation value.
The X-ray orientation system may be an X-ray diffractometer or an X-ray director, where the X-ray diffractometer and the X-ray director are both existing devices, and are not described herein, and the X-ray transmitting unit is a transmitter of the X-ray transmitting unit, and the X-ray receiving unit is a receiver of the X-ray transmitting unit.
The silicon carbide crystal of the application can be silicon carbide crystals with different thicknesses such as silicon carbide substrates, silicon carbide crystal bars, silicon carbide grinding sheets or silicon carbide polishing sheets.
According to the application, the (11-28) crystal face 24 is selected as a reference plane or the (11-28) crystal face 24 is converted into a horizontal reference plane, the horizontal reference plane is like a test bench and the (0001) crystal face 21 of the silicon carbide crystal, the Bragg diffraction angle theta of the (11-28) crystal face 24 is calculated, the top surface of the silicon carbide crystal 31 is selected as a test plane, the side surface 11 of the silicon carbide crystal is selected as the test plane instead of the side surface 11 of the silicon carbide crystal in the prior art, the blank that the sheet-shaped silicon carbide substrate cannot be tested is filled, and the detection range is greatly widened.
Because the test surface is a plane instead of the side surface with an arc-shaped curved surface, the test point is easy to be positioned, thereby greatly improving the test accuracy and saving the test time.
The testing method does not need special tools, greatly simplifies operation, does not need special change to a common testing instrument, increases detection efficiency and universality, can be suitable for XRD, an X-ray orientation instrument and the like, and has higher testing accuracy; can be used for silicon carbide crystals, and is suitable for industrial testing of the silicon carbide crystals.
The above description is only an example of the present application, and the scope of the present application is not limited to the specific examples, but is defined by the claims of the present application. Various modifications and variations of the present application will be apparent 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 (12)

1. A method of testing the orientation of a principal reference plane of a silicon carbide crystal, comprising the steps of:
1) Horizontally placing a silicon carbide crystal to be detected on a test bench, selecting a (11-28) crystal face of the silicon carbide crystal as a reference face, and calculating a Bragg diffraction angle theta of the (11-28) crystal face;
2) Adjusting an X-ray orientation system, and selecting a straight line passing through the central point of the top surface of the silicon carbide crystal and perpendicular to the (11-28) crystal face as a normal line, so that the intersection point of the incident ray emitted by the X-ray orientation system and the reflection line is focused on the central point of the top surface of the silicon carbide crystal;
the included angle between the incident ray and the (11-28) crystal face and the included angle between the reflecting ray and the (11-28) crystal face are theta, the plane where the incident ray and the reflecting ray are located is parallel to the (1-100) crystal face of the silicon carbide crystal, and the X-ray orientation system displays a first signal intensity value at the moment;
3) And then horizontally rotating the test bench in a clockwise and/or anticlockwise direction, wherein when the signal intensity value displayed by the X-ray orientation system is maximum relative to the first signal intensity value, the rotation angle of the test bench is the deviation value of the orientation of the main reference surface of the silicon carbide crystal.
2. The method for testing the orientation of a principal reference plane of a silicon carbide crystal according to claim 1, wherein in step 1), the bragg diffraction angle θ of the (11-28) crystal plane is calculated as follows:
2dsin(θ)＝nλ
wherein lambda is the wavelength of X rays, the materials of X rays emitted by the X ray orientation system are copper target structures, and the materials are fixed values;
n is a positive natural number; d is the distance value between the (11-28) crystal faces,
calculated, the Bragg diffraction angle θ of the (11-28) crystal plane is equal to 52.5++0.5°.
3. The method of testing the orientation of a principal reference plane of a silicon carbide crystal according to claim 1, wherein in step 2) the incident line is at an angle of 9 ° ± 1 ° with respect to the test bench;
the angle between the reflection line and the test bench is 96 degrees plus or minus 1 degree.
4. A method of testing the orientation of a principal reference plane of a silicon carbide crystal according to claim 3, wherein the X-ray orientation system comprises an X-ray emitting unit for emitting an incident ray, an X-ray receiving unit for receiving a reflected ray, and a signal intensity monitoring unit;
step 2) further comprises a first arcuate scan: and taking the center point of the top surface of the silicon carbide crystal as a circle center, taking the distance from the X-ray emission unit to the center point as a radius, and taking the top surface of the silicon carbide crystal as a 0-degree reference surface, so that the X-ray emission unit performs first arc scanning on a plane where the incident ray and the reflection line are located, wherein the first arc scanning range is 9+/-1 degrees, and in the first arc scanning process, when the signal intensity monitoring unit displays the highest signal peak, the X-ray emission unit is adjusted to be at the position.
5. A method of testing the orientation of a principal reference plane of a silicon carbide crystal as claimed in claim 4,
step 2) further comprises a second arcuate scan: and taking the center point of the top surface of the silicon carbide crystal as a circle center, taking the distance from the X-ray receiving unit to the center point as a radius, and taking the top surface of the silicon carbide crystal as a 0-degree reference surface, so that the X-ray receiving unit performs a second arc scanning on the plane where the incident ray and the reflection line are located, wherein the second arc scanning range is 96 degrees+/-1 degrees, and when the signal intensity monitoring unit displays the highest signal peak, the X-ray receiving unit is adjusted to be at the position.
6. The method of testing the orientation of a principal reference plane of a silicon carbide crystal according to claim 1, wherein in step 2) the incident line is at an angle of 96 ° ± 1 ° with respect to the test bench;
the angle between the reflection line and the test bench is 9 degrees plus or minus 1 degree.
7. The method of testing the orientation of a principal reference plane of a silicon carbide crystal according to claim 6, wherein the X-ray orientation system comprises an X-ray emitting unit for emitting an incident ray, an X-ray receiving unit for receiving a reflected ray, and a signal intensity monitoring unit;
step 2) further comprises a first arcuate scan: and taking the center point of the top surface of the silicon carbide crystal as a circle center, taking the distance from the X-ray emission unit to the center point as a radius, and taking the top surface of the silicon carbide crystal as a 0-degree reference surface, so that the X-ray emission unit performs first arc scanning on a plane where the incident ray and the reflection line are located, wherein the first arc scanning range is 96+/-1 degrees, and in the first arc scanning process, when the signal intensity monitoring unit displays the highest signal peak, the X-ray emission unit is adjusted to be at the position.
8. A method of testing the orientation of a principal reference plane of a silicon carbide crystal as claimed in claim 7,
step 2) further comprises a second arcuate scan: and taking the center point of the top surface of the silicon carbide crystal as a circle center, taking the distance from the X-ray receiving unit to the center point as a radius, and taking the top surface of the silicon carbide crystal as a 0-degree reference surface, so that the X-ray receiving unit performs a second arc scanning on the plane where the incident ray and the reflection line are located, wherein the second arc scanning range is 9+/-1 degrees, and when the signal intensity monitoring unit displays the highest signal peak, the X-ray receiving unit is adjusted to be at the position.
9. A method for testing the orientation of a principal reference plane of a silicon carbide crystal as claimed in claim 5 or 8,
adjusting the height of the test bench, and fixing the test bench at the height when the first signal intensity value is displayed to be maximum;
and then horizontally rotating the test bench along the clockwise and/or anticlockwise direction, wherein the rotating angle range is +/-3 degrees, and the rotating angle of the test bench is the deviation value of the main reference plane orientation of the silicon carbide crystal when the signal intensity value displayed by the X-ray orientation system is maximum relative to the first signal intensity value in the angle range.
10. The method of claim 9, wherein the first arcuate scan, the second arcuate scan, the height adjustment of the test stand, and the horizontal rotation of the test stand in a clockwise and/or counterclockwise direction are repeated a plurality of times, the last test stand rotation being at an angle offset from the final silicon carbide crystal main reference plane orientation value.
11. A method of testing the orientation of a principal reference plane of a silicon carbide crystal according to claim 1, wherein said silicon carbide crystal itself has an inclination angle of 0 ° to 4 °;
the included angle between the (11-28) crystal face and the (0001) crystal face of the silicon carbide crystal is 39.5 degrees plus or minus 0.5 degrees.
12. The method of testing the orientation of a principal reference plane of a silicon carbide crystal according to claim 1, wherein the silicon carbide crystal is a silicon carbide substrate, a silicon carbide boule, a silicon carbide abrasive sheet, or a silicon carbide polished sheet.
CN202311069490.6A 2023-08-23 2023-08-23 Method for testing orientation of main reference surface of silicon carbide crystal Pending CN117110337A (en)

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