CN118655163B - A non-destructive measurement method for silicon carbide defect density - Google Patents
A non-destructive measurement method for silicon carbide defect density Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 113
- 230000007547 defect Effects 0.000 title claims abstract description 85
- 238000000691 measurement method Methods 0.000 title claims abstract description 17
- 230000001066 destructive effect Effects 0.000 title claims description 5
- 238000001514 detection method Methods 0.000 claims abstract description 37
- 238000004364 calculation method Methods 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000000758 substrate Substances 0.000 claims abstract description 16
- 238000005259 measurement Methods 0.000 claims abstract description 12
- 238000002441 X-ray diffraction Methods 0.000 claims description 37
- 238000000034 method Methods 0.000 claims description 15
- 238000009659 non-destructive testing Methods 0.000 claims 4
- 239000013078 crystal Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001739 density measurement Methods 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005092 sublimation method Methods 0.000 description 1
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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
- 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
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/25—Measuring force or stress, in general using wave or particle radiation, e.g. X-rays, microwaves, neutrons
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L5/00—Apparatus for, or methods of, measuring force, work, mechanical power, or torque, specially adapted for specific purposes
- G01L5/0047—Apparatus for, or methods of, measuring force, work, mechanical power, or torque, specially adapted for specific purposes measuring forces due to residual stresses
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Abstract
A nondestructive measurement method for the defect density of silicon carbide comprises the steps of carrying out XRD detection on a silicon carbide sample to be detected to obtain a rocking curve, further obtaining the half-width of the silicon carbide sample to be detected, carrying out XRD detection on a standard sample to obtain a rocking curve, further obtaining the half-width of the standard sample, and calculating according to a defect density calculation formula to obtain the defect density of the silicon carbide, wherein the defect density calculation formula is dislocation density= (the half-width of the silicon carbide sample to be detected-the half-width of the standard sample) 2/(4.35×b2)×10‑4, and b is a Berth vector of the defect. The invention can be used for nondestructively measuring the defect density of the silicon carbide by measuring the half-width of the rocking curve on the basis of fully researching the defect density of the silicon carbide and the relation between the residual stress and the rocking curve, and further calculating the residual stress by the peak position of the rocking curve, thereby realizing the rapid and accurate measurement of the defect density of the silicon carbide on the basis of not damaging a substrate material, and having high efficiency and low cost.
Description
Technical Field
The invention relates to the technical field of semiconductor defect detection, in particular to a nondestructive measurement method for defect density of silicon carbide.
Background
Silicon carbide is an inorganic substance, the chemical formula is SiC, and the industrial production of silicon carbide substrate materials is mainly carried out by a physical vapor sublimation method, the method needs to sublimate the silicon carbide powder in a high-temperature vacuum environment, and then sublimated components grow on the surface of a seed crystal through the control of a temperature field so as to obtain silicon carbide crystals. Silicon carbide is a semiconductor that exists in nature in the form of the extremely rare mineral morganite. Has been mass produced as powders and crystals since 1893, and used as abrasives and the like. Of the non-oxide high technology refractory materials such as C, N, B, silicon carbide is one of the most widely used and economical materials, and may be referred to as diamond grit or refractory grit.
Silicon carbide is used as a power semiconductor material, the defect density of which directly affects the reliability and yield of silicon carbide power devices, and in order to evaluate the quality of a substrate material, the defect density of the substrate material needs to be measured. In the prior art, defects such as dislocation and the like are exposed mainly through high-temperature alkali corrosion, and then the appearance and the number of the defects are observed under an optical microscope to realize the measurement of the defect density, which is shown in fig. 1-2.
However, the conventional measurement method has irreversible damage to the substrate material, and is widely known to be expensive, such as 4H silicon carbide substrate material, and the like, and the conventional measurement method can damage the substrate material and greatly improve the cost.
Disclosure of Invention
In view of the above, the invention aims to provide a nondestructive measurement method for the defect density of silicon carbide, which can realize rapid and accurate measurement of the defect density of silicon carbide on the basis of not damaging a substrate material, has high efficiency and low cost, and can further calculate residual stress.
The invention provides a nondestructive measurement method of defect density of silicon carbide, which comprises the following steps:
XRD detection is carried out on the silicon carbide sample to be detected, a rocking curve is obtained, and the half-width of the silicon carbide sample to be detected is further obtained;
XRD detection is carried out on the standard sample to obtain a rocking curve, and the half-width of the standard sample is further obtained;
Calculating according to a defect density calculation formula to obtain the defect density of the silicon carbide;
The defect density calculation formula is as follows:
dislocation density= (half-width of silicon carbide sample to be measured-half-width of standard sample) 2/(4.35×b2)×10-4;
Wherein b is the Bosch vector of the defect.
Preferably, the silicon carbide sample to be measured is a hexagonal silicon carbide substrate material.
Preferably, the selected point for XRD detection of the silicon carbide sample to be detected is a center point, and the center point is offset by 10 mm-40 mm from top to bottom, left to right.
Preferably, XRD detection is carried out on different selected points of the silicon carbide sample to be detected to obtain a rocking curve corresponding to the selected points, the half-width of the corresponding selected points is further obtained, and an average value is calculated to obtain the half-width of the silicon carbide sample to be detected.
Preferably, the selected point for XRD detection of the standard sample is a center point, and the center point is shifted by 10 mm-40 mm from top to bottom, left to right.
Preferably, XRD detection is carried out on different selected points of the standard sample to obtain a rocking curve corresponding to the selected points, the half-width of the corresponding selected points is further obtained, and the average value is calculated to obtain the half-width of the standard sample.
Preferably, the error introduced by the self-broadening of the instrument is calibrated by removing the half-width of the silicon carbide sample to be measured from the half-width of the standard sample.
Preferably, the half-width of the silicon carbide sample to be measured-the half-width of the standard sample is more than or equal to 0.3 arc seconds.
Preferably, the value of b for SiC is 10.053 x10 -10.
Preferably, the residual stress of the silicon carbide is calculated according to the rocking curve measurement result.
The invention provides a nondestructive measurement method of defect density of silicon carbide, which comprises the steps of carrying out XRD (X-ray diffraction) detection on a silicon carbide sample to be detected to obtain a rocking curve, further obtaining the half-width of the silicon carbide sample to be detected, carrying out XRD detection on a standard sample to obtain a rocking curve, further obtaining the half-width of the standard sample, and calculating according to a defect density calculation formula to obtain the defect density of the silicon carbide, wherein the defect density calculation formula is dislocation density= (the half-width of the silicon carbide sample to be detected-the half-width of the standard sample) 2/(4.35×b2)×10-4, and b is a Berth vector of the defect. Compared with the prior art, the method has the advantages that the defect density of the silicon carbide can be measured in a nondestructive manner by measuring the half-width of the rocking curve on the basis of fully researching the relationship between the defect density of the silicon carbide and the residual stress and the rocking curve, and the residual stress can be calculated by further passing the peak position of the rocking curve, so that the defect density of the silicon carbide can be measured rapidly and accurately on the basis of not damaging a substrate material, the efficiency is high, the cost is low, and the residual stress can be further calculated.
Drawings
FIG. 1 is a prior art low magnification optical micrograph of a silicon carbide defect density measurement;
FIG. 2 is a high magnification optical microscope photograph of a prior art defect density measurement of silicon carbide;
FIG. 3 is an XRD rocking curve of the Si001 plane in example 1;
Fig. 4 is an XRD rocking curve of the SiC 0004 face, where the silicon carbide surface is subjected to a4 ° chamfering process.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a nondestructive measurement method of defect density of silicon carbide, which comprises the following steps:
XRD detection is carried out on the silicon carbide sample to be detected, a rocking curve is obtained, and the half-width of the silicon carbide sample to be detected is further obtained;
XRD detection is carried out on the standard sample to obtain a rocking curve, and the half-width of the standard sample is further obtained;
Calculating according to a defect density calculation formula to obtain the defect density of the silicon carbide;
The defect density calculation formula is as follows:
dislocation density= (half-width of silicon carbide sample to be measured-half-width of standard sample) 2/(4.35×b2)×10-4;
Wherein b is the Bosch vector of the defect.
According to the invention, XRD detection is performed on the silicon carbide sample to be detected to obtain a rocking curve, and the half-width of the silicon carbide sample to be detected is further obtained.
In the invention, the silicon carbide sample to be measured is preferably a hexagonal silicon carbide substrate material. The source of the hexagonal silicon carbide substrate material is not particularly limited, and commercially available products known to those skilled in the art may be used. At present, defects such as dislocation and the like are mainly exposed through high-temperature alkali corrosion in the prior art aiming at the measurement of the defect density in the silicon carbide substrate material, and then the appearance and the quantity of the defects are observed under an optical microscope, so that the defects are irreversibly damaged and have low efficiency, and meanwhile, the damage is high for the cost due to the high price of the silicon carbide substrate material.
In the invention, the selection point for XRD detection of the silicon carbide sample to be detected is preferably a center point and the positions of the center point, which are shifted by 10 mm-40 mm from top to bottom, left to right. In the preferred embodiment of the invention, the selected point for XRD detection of the silicon carbide sample to be detected is a central point, and the central point is offset by 25mm in the vertical and horizontal directions.
According to the invention, XRD detection is carried out on different selected points of the silicon carbide sample to be detected, so that a rocking curve corresponding to the selected points is obtained, the half-width of the corresponding selected points is further obtained, and the average value is calculated to obtain the half-width of the silicon carbide sample to be detected.
The present invention is not particularly limited to the apparatus and method for XRD detection, and conventional XRD detection may be performed using apparatuses well known to those skilled in the art.
Then, XRD detection is carried out on the standard sample to obtain a rocking curve, and the half-width of the standard sample is further obtained.
In the present invention, the standard sample is preferably a silicon wafer. The source of the silicon wafer is not particularly limited and commercially available products known to those skilled in the art may be used.
In the invention, the selection point for XRD detection of the standard sample is preferably a center point and positions of the center point, which are shifted by 10 mm-40 mm from top to bottom, left to right. In a preferred embodiment of the present invention, the selected point for XRD detection of the standard sample is a center point and the center point is offset by 25mm vertically and horizontally.
According to the invention, XRD detection is carried out on different selected points of the standard sample, so that a rocking curve corresponding to the selected points is obtained, the half-width of the corresponding selected points is further obtained, and the average value is calculated to obtain the half-width of the standard sample.
In the invention, the half-width of the silicon carbide sample to be measured is removed from the half-width of the standard sample, so that the error introduced by the self-broadening of the instrument is calibrated. And the half-width of the silicon carbide sample to be measured and the half-width of the standard sample are preferably more than or equal to 0.3 arc seconds, otherwise, the difference value between the two is too small, so that the defect density calculation formula is not applicable.
The invention fully researches the relation between the defect density of silicon carbide and the rocking curve, improves a general calculation formula based on specific experiments and data, comprises the selection of a constant 4.35 in the formula, and after a plurality of groups of samples to be measured are measured, the data result shows that when the half-width of the samples to be measured deviates from the broadening of an instrument, the defect density is accurately estimated by the rocking curve, and when the half-width of the samples to be measured approaches to the broadening of the instrument, the square term causes larger error and other factors such as measurement and the like need to be eliminated.
On the basis, the defect density calculation formula provided by the invention actually belongs to a corrected defect density calculation formula, and the dislocation density of the calculation result of the corrected defect density calculation formula is preferably more than or equal to 20cm -1, otherwise, the defect density calculation formula is not applicable.
In the invention, the defect density calculation formula is as follows:
dislocation density= (half-width of silicon carbide sample to be measured-half-width of standard sample) 2/(4.35×b2)×10-4;
Wherein b is the Bosch vector of the defect, and the value of b is preferably 10.053 X10 -10 for SiC.
According to the nondestructive measurement method for the defect density of the silicon carbide, provided by the invention, the rocking curve is obtained through XRD detection, and the residual stress of the silicon carbide can be further calculated according to the measurement result of the rocking curve, so that the nondestructive measurement method has the additional technical effect, and the nondestructive measurement method is particularly referred to the technical scheme provided by the Chinese patent CN114858324A, and is not repeated herein.
The invention provides a nondestructive measurement method of defect density of silicon carbide, which comprises the steps of carrying out XRD (X-ray diffraction) detection on a silicon carbide sample to be detected to obtain a rocking curve, further obtaining the half-width of the silicon carbide sample to be detected, carrying out XRD detection on a standard sample to obtain a rocking curve, further obtaining the half-width of the standard sample, and calculating according to a defect density calculation formula to obtain the defect density of the silicon carbide, wherein the defect density calculation formula is dislocation density= (the half-width of the silicon carbide sample to be detected-the half-width of the standard sample) 2/(4.35×b2)×10-4, and b is a Berth vector of the defect. Compared with the prior art, the method has the advantages that the defect density of the silicon carbide can be measured in a nondestructive manner by measuring the half-width of the rocking curve on the basis of fully researching the relationship between the defect density of the silicon carbide and the residual stress and the rocking curve, and the residual stress can be calculated by further passing the peak position of the rocking curve, so that the defect density of the silicon carbide can be measured rapidly and accurately on the basis of not damaging a substrate material, the efficiency is high, the cost is low, and the residual stress can be further calculated.
In order to further illustrate the present invention, the following examples are provided. The silicon wafer used in the following examples of the present invention was supplied by the Ming's chemical, model number was high purity monocrystalline silicon wafer, the SiC used was supplied by Shandong Tianyue, model number was high purity 4H silicon carbide, and model number was Markov panaco X' Pert MRD using XRD tester.
Example 1
A method for non-destructive measurement of silicon carbide defect density, comprising the steps of:
(1) Self-broadening of the measuring instrument:
And a high-quality silicon wafer is used as a standard sample, so that errors introduced by self-broadening of the instrument are calibrated.
The specific operation steps are as follows:
XRD rocking curve of Si001 plane was measured to obtain full width half maximum FWHM_Si (rad), a plurality of points were uniformly taken for each wafer, center point and offset of 25mm in the up-down and left-right directions were taken for 4 inches, and the full width half maximum FWHM_Si (rad) was averaged based on the results of the plurality of points, specifically 15.16 arcsec (see FIG. 3).
(2) XRD rocking curve test of sample to be tested:
the rocking curve of the SiC 0004 surface was measured to obtain full width half maximum FWHM_SiC (rad), a plurality of points were uniformly taken for each wafer, and for 4 inches, the center point and the positions offset by 25mm in the up-down, left-right directions were taken, as shown in FIG. 4, wherein 1 was the center point, 2 was the position 25mm above the center point, 3 was the position 25mm below the center point, 4 was the position 25mm to the left of the center point, and 5 was the position 25mm to the right of the center point.
(3) Defect calculation:
Substituting the test results obtained in the step (1) and the step (2) into a defect density calculation formula, and calculating an average value according to the defect density results of a plurality of points to obtain the defect density of the sample to be tested.
Defect density calculation formula:
Dislocation density/cm -1＝(FWHM_SiC-FWHM_Si)2/(4.35×b2)×10-4;
where b is the Bosch vector of the defect and for SiC, the value is 10.053 X10: 10 -10.
(4) Residual stress calculation:
According to the technical scheme provided by the Chinese patent CN114858324A, the residual stress of the sample to be detected is calculated according to the test result.
The test data are shown in table 1.
TABLE 1
Comparative example 1
The dislocation density detection of the traditional silicon carbide wafer, namely the KOH corrosion detection of the silicon carbide, is adopted.
Detection standard:
1. GB_T30868-2014 chemical etching method for measuring micropipe density of silicon carbide single crystal;
2. T/CASA 013-2021 KOH corrosion combined image recognition method for dislocation density detection method of silicon carbide wafer.
As a result of the test, the average defect density obtained in comparative example 1 was 200.4cm -1, and the defect densities at each point were 294, 149, 294, 150, 115 (cm -1), respectively.
In summary, the technical scheme provided by the invention can be used for nondestructively measuring the defect density of the silicon carbide through the half-width of the rocking curve of the 0004 crystal face on the basis of fully researching the relationship between the defect density of the silicon carbide and the residual stress and the rocking curve, and further calculating the residual stress through the peak position of the rocking curve, so that the rapid measurement method is beneficial to improving the detection efficiency and reducing the production cost.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. A method for non-destructive measurement of silicon carbide defect density, comprising the steps of:
XRD detection is carried out on a silicon carbide sample to be detected to obtain a rocking curve, and the half-width of the silicon carbide sample to be detected is further obtained, wherein the silicon carbide sample to be detected is a hexagonal silicon carbide substrate material;
XRD detection is carried out on the standard sample to obtain a rocking curve, and the half-width of the standard sample is further obtained;
Calculating according to a defect density calculation formula to obtain the defect density of the silicon carbide;
The defect density calculation formula is as follows:
dislocation density= (half-width of silicon carbide sample to be measured-half-width of standard sample) 2/(4.35×b2)×10-4;
Wherein b is the Bosch vector of the defect.
2. The nondestructive measurement method of the defect density of the silicon carbide according to claim 1, wherein the selected point for XRD detection of the silicon carbide sample to be detected is a center point, and the center point is shifted by 10 mm-40 mm in the vertical and horizontal directions respectively.
3. The nondestructive testing method of the defect density of the silicon carbide according to claim 2, wherein the swing curve corresponding to the selected points is obtained by performing XRD (X-ray diffraction) detection on different selected points of the silicon carbide sample to be tested, the half-width of the corresponding selected points is further obtained, and an average value is calculated to obtain the half-width of the silicon carbide sample to be tested.
4. The nondestructive measurement method of silicon carbide defect density according to claim 1, wherein the selected point for XRD detection of the standard sample is a center point and the center point is shifted by 10mm to 40mm in the vertical and horizontal directions.
5. The nondestructive testing method for the defect density of the silicon carbide according to claim 4, wherein XRD detection is carried out on different selected points of the standard sample to obtain a rocking curve corresponding to the selected points, further obtaining the half-width of the corresponding selected points, and calculating an average value to obtain the half-width of the standard sample.
6. The method for non-destructive measurement of defect density of silicon carbide according to claim 1, wherein the error introduced by self-broadening of the instrument is calibrated by removing the full width at half maximum of the standard sample from the full width at half maximum of the silicon carbide sample to be measured.
7. The method for non-destructive testing of defect density of silicon carbide according to claim 6, wherein the half-width of the silicon carbide sample to be tested-the half-width of the standard sample is not less than 0.3 arc seconds.
8. The method for non-destructive measurement of silicon carbide defect density according to claim 1, wherein the value of b for SiC is 10.053 x10 -10.
9. The method for non-destructive testing of silicon carbide defect density according to claim 1, wherein the residual stress of silicon carbide is calculated from rocking curve measurements.
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