CN112444529B - HRXRD test method for distinguishing twin crystal in non (100) plane gallium oxide crystal - Google Patents
HRXRD test method for distinguishing twin crystal in non (100) plane gallium oxide crystal Download PDFInfo
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- 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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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N2223/056—Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
An HRXRD test method for distinguishing the twin crystal of non (100) plane gallium oxide crystal is to place the non (100) plane gallium oxide crystal on the sample stage of the device; setting the width of an incidence slit to be 10mm-13mm; setting 2 θ to 31.738 ° corresponds to a crystal plane of (002); rotating the sample from 0 degree to 90 degrees, setting the rotation step length to be 0.1 degree to 0.3 degree, recording the number of (002) plane diffraction peaks, resetting the sample table, then rotating the sample 180 degrees on an X-Y plane by taking the origin as the center, rotating the sample from 0 degree to 90 degrees by taking the [010] crystal orientation as the axis, setting the rotation step length to be 0.1 degree to 0.3 degree, and recording the number of (002) plane diffraction peaks; if only 1 (002) plane diffraction peak is detected in the process, determining that twin crystals are not in the test region, and if a plurality of (002) plane diffraction peaks are detected, determining that twin crystals are in the test region; the efficiency is improved and the cost is reduced.
Description
Technical Field
The invention relates to an HRXRD (high resolution X-ray diffraction) test method for distinguishing the existence of twin crystals in non (100) plane gallium oxide crystals, which belongs to the technical field of semiconductor single crystal material test and is used for judging whether the twin crystals exist in the non (100) plane gallium oxide crystals.
Background
The forbidden band width of gallium oxide single crystal (gallium oxide) at room temperature is about 4.9 eV, the breakdown field strength is as high as 8MV/cm, the Baliga optimum value (low loss index) is more than 3000 times of that of Si single crystal, and the gallium oxide single crystal is an ideal substrate material of a high-voltage-resistant low-loss power device. The gallium oxide single crystal material can be prepared by a melt method, has high growth rate, high crystal quality and low cost, and has wide application prospect. Gallium oxide single crystal belongs to monoclinic system, a =1.223nm, b =0.304nm and c =0.58nm, the anisotropy is remarkable, wherein (100) plane is most easily obtained, but homoepitaxy cannot be carried out, and the application is severely limited. The crystal planes required by homoepitaxy all form an included angle with the (100) plane, and twin crystals are generated when the gallium oxide crystals with the crystal planes grow. The presence of twins in non- (100) plane gallium oxide wafers affects the quality of the epitaxial layer and therefore it is necessary to identify the presence of twins in the wafer prior to use.
The twin stripes of the non (100) plane gallium oxide crystal are very similar to the growth stripes and are not easy to distinguish, and whether twin crystals exist in the crystal can be determined by observing the crystal with a differential interference microscope after a series of processing technologies such as cutting, grinding and polishing are generally needed, but the method needs too long time, and the accuracy of observing the twin stripes is low, and is closely related to the grinding and polishing quality.
Disclosure of Invention
The invention provides a high-resolution X-ray diffraction test method for distinguishing the twin crystal in the non (100) plane gallium oxide crystal, which well solves the problem that the twin crystal in the non (100) plane gallium oxide crystal cannot be directly distinguished.
The invention adopts the technical scheme that an HRXRD test method for distinguishing the twin crystal existence of non (100) plane gallium oxide crystals comprises the following steps:
a. placing the non- (100) plane gallium oxide crystal on a sample stage of an HRXRD equipment, making the edge of the gallium oxide crystal coincide with the X-axis, and enabling the [010] crystal direction to be parallel to the X-axis direction;
b. setting the width of an incidence slit to be 10mm-13mm, and ensuring that a test area is as large as possible;
c. 2 theta is set to be 31.738 degrees, and the corresponding crystal face is (002), because the peak intensity of the (002) face is obviously larger than that of the (001) face, the detection is easier in the testing process;
d. taking the [010] crystal direction as an axis, rotating the sample from 0 degree to 90 degrees, setting the rotation step length to be 0.1 degree to 0.3 degree, recording the number of (002) surface diffraction peaks, resetting the sample table, then taking the original point as the center, rotating the sample on an X-Y plane by 180 degrees, taking the [010] crystal direction as an axis, rotating the sample from 0 degree to 90 degrees, setting the rotation step length to be 0.1 degree to 0.3 degree, and recording the number of (002) surface diffraction peaks;
e. if only 1 (002) plane diffraction peak is detected in the process, determining that twin crystals are not in the test region, if a plurality of (002) plane diffraction peaks are detected, determining that twin crystals are in the test region, because the growth plane and the twin crystal plane are symmetrical along the (100) plane and form different included angles with the (001) plane, respectively represented by alpha 1 and alpha 2, if twin crystals are in the test region, diffraction peaks can appear when the sample platform rotates to alpha 1 and alpha 2, and if twin crystals are not in the test region, diffraction peaks can appear only when the sample platform rotates to alpha 1;
f. and (3) resetting the sample stage, moving the sample along the y axis by taking the width of the slit as a step length, and repeating d-e until the test area covers the whole crystal, wherein the twin crystal in the gallium oxide crystal penetrates through the test area along the [010] direction, and if the sample is moved along the y axis direction, all the test areas have no twin crystal, the fact that no twin crystal exists in the crystal can be judged.
The beneficial effects of the invention are:
a in the existing method for observing by adopting a differential interference microscope, gallium oxide crystals need to be cut, ground and polished for at least 8 hours, but in the method, gallium oxide crystals with non (100) surfaces can be directly distinguished whether twin crystals exist without processing, the time is short, the testing time of the gallium oxide crystals with 2 inches is only 30min, and the automation degree is high;
b, judging accurately, accurately distinguishing whether twin crystals exist in each test area, and subsequently selecting a twin crystal-free area for processing, so that the efficiency is improved, and the cost is reduced;
the testing method is nondestructive testing and does not cause any damage to the gallium oxide crystal.
Drawings
FIG. 1 is a flow chart of a test method of the present invention;
FIG. 2 is a schematic diagram of twin crystals in a non- (100) plane gallium oxide crystal;
FIG. 3 shows the appearance of the (002) plane diffraction peak when the sample stage is rotated to 22.4 °;
fig. 4 shows the appearance of the (002) plane diffraction peak when the sample stage was rotated to 49.9 °.
Detailed Description
As shown in fig. 1, a high resolution X-ray diffraction test method for discriminating the presence or absence of twin crystals in non (100) plane gallium oxide crystals comprises the following steps:
a. placing a non (100) plane gallium oxide crystal 2 on a sample stage 1 of an HRXRD device so that the edge thereof coincides with the X-axis and the [010] crystal direction is parallel to the X-axis direction;
b. setting the width of an incident slit as a maximum value of 10mm to 13mm, and ensuring that a test area is as large as possible;
c. 2 theta is set to be 31.738 degrees, the corresponding crystal face is (002), and the peak intensity of the (002) face is obviously larger than that of the (001) face, so that the (002) face is easier to detect in the test process;
d. taking the [010] crystal direction as an axis, rotating the sample from 0 degree to 90 degrees, setting the rotation step length to be 0.1 degree to 0.3 degree, recording the number of (002) surface diffraction peaks, resetting the sample table 1, then taking the original point as the center, rotating the sample on an X-Y plane by 180 degrees, taking the [010] crystal direction as an axis, rotating the sample from 0 degree to 90 degrees, setting the rotation step length to be 0.1 degree to 0.3 degree, and recording the number of (002) surface diffraction peaks;
e. if only 1 (002) plane diffraction peak is detected in the process, determining that twin crystals are not present in the test region, and if a plurality of (002) plane diffraction peaks are detected, determining that twin crystals are present in the test region because the growth plane and the twin crystal plane are symmetrical along the (100) plane and form different included angles with the (001) plane, which are respectively represented by alpha 1 and alpha 2, as shown in fig. 2, if twin crystals are present in the test region, diffraction peaks will appear when the sample stage 1 rotates to alpha 1 and alpha 2, and if twin crystals are not present in the test region, diffraction peaks will appear only when the sample stage 1 rotates to alpha 1;
f. and (3) resetting the sample table 1, moving the sample along the y axis by taking the width of the slit as a step length, and repeating d-e until the test area covers the whole crystal, wherein the twin crystal in the gallium oxide crystal penetrates through the test area along the [010] direction, and if the sample is moved along the y axis direction, all the test areas have no twin crystal, the fact that no twin crystal exists in the crystal can be judged.
Examples 1
Low resistance of 10mm by 3mm (
01 Crystal of planar gallium oxide.
a. Placing a 10mm × 10mm × 3mm gallium oxide crystal on a sample stage 1 of an HRXRD apparatus so that the edge thereof coincides with the X-axis and the [010] crystal orientation is parallel to the X-axis direction;
b. setting the width of an incident slit to be 10mm;
c. setting 2 theta to be 31.738 degrees, and corresponding to the crystal plane to be (002);
d. rotating the sample from 0 degree to 90 degrees by taking the [010] crystal direction as an axis, recording the number of (002) plane diffraction peaks, resetting the sample stage 1, rotating the sample on an X-Y plane by 180 degrees by taking the original point as a center, rotating the sample from 0 degree to 90 degrees by taking the [010] crystal direction as an axis, and recording the number of (002) plane diffraction peaks;
e. in the above process, when the sample stage 1 is rotated to 22.4 ° and 49.9 °, respectively, (002) plane diffraction peaks appear, and thus it can be judged that a twin crystal exists in the crystal, as shown in fig. 3 and 4.
EXAMPLES example 2
2 inch high resistance (
01 ) a crystal of planar gallium oxide with a thickness of 3.1mm.
a. 2 inches high resistance (
01 ) plane gallium oxide crystals were placed on the sample stage 1 of the HRXRD equipment so that the edges thereof coincide with the x-axis, and [010] plane gallium oxide crystals were placed on the sample stage]The crystal direction is parallel to the X-axis direction;
b. setting the width of an incident slit to be 13mm;
c. setting 2 theta to be 31.738 degrees, and corresponding to the crystal plane to be (002);
d. taking the [010] crystal direction as an axis, rotating the sample from 0 degree to 90 degrees, setting the rotation step length to be 0.1 degree, recording the number of (002) plane diffraction peaks, resetting the sample stage 1, then taking the origin as the center, rotating the sample on an X-Y plane by 180 degrees, taking the [010] crystal direction as an axis, rotating the sample from 0 degree to 90 degrees, setting the rotation step length to be 0.1 degree, and recording the number of (002) plane diffraction peaks;
e. resetting the sample table 1, moving the sample along the y axis by taking 13mm as a step length, repeating the steps d-e, and covering the whole crystal in a test area after 4 times;
in the above process, the (002) plane diffraction peak appears only when the sample stage 1 is rotated to 22.4 °, and therefore it can be judged that there is no twin crystal in the crystal.
Claims (1)
1. An HRXRD test method for distinguishing the twin crystal existence of non (100) plane gallium oxide crystal is characterized by comprising the following steps:
a. placing a non (100) plane gallium oxide crystal (2) on a sample stage (1) of an HRXRD device so that the edge thereof coincides with the X-axis and the [010] crystal orientation is parallel to the X-axis direction;
b. setting the width of an incidence slit to be 10mm-13mm, and ensuring that a test area is as large as possible;
c. 2 theta is set to be 31.738 degrees, the corresponding crystal face is (002), and the peak intensity of the (002) face is obviously larger than that of the (001) face, so that the (002) face is easier to detect in the test process;
d. taking the [010] crystal direction as an axis, rotating the sample from 0 degree to 90 degrees, setting the rotation step length to be 0.1 degree to 0.3 degree, recording the number of (002) surface diffraction peaks, resetting the sample table 1, then taking the original point as the center, rotating the sample on an X-Y plane by 180 degrees, taking the [010] crystal direction as an axis, rotating the sample from 0 degree to 90 degrees, setting the rotation step length to be 0.1 degree to 0.3 degree, and recording the number of (002) surface diffraction peaks;
e. if only 1 (002) plane diffraction peak is detected in the process, determining that twin crystals are not in the test region, if a plurality of (002) plane diffraction peaks are detected, determining that twin crystals are in the test region, because the growth plane and the twin crystal plane are symmetrical along the (100) plane and form different included angles with the (001), respectively represented by alpha 1 and alpha 2, if twin crystals are in the test region, diffraction peaks can be generated when the sample stage (1) rotates to alpha 1 and alpha 2, and if twin crystals are not in the test region, diffraction peaks can be generated only when the sample stage (1) rotates to alpha 1;
f. and (3) resetting the sample table (1), moving the sample along the y axis by taking the width of the slit as a step length, and repeating d-e until the test area covers the whole crystal, wherein the twin crystal in the gallium oxide crystal penetrates through the gallium oxide crystal along the [010] direction, and if the sample is moved along the y axis direction, all the test areas have no twin crystal, so that the fact that no twin crystal exists in the crystal can be judged.
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