CN102445373A - Detection method of sapphire monocrystal dislocation density - Google Patents
Detection method of sapphire monocrystal dislocation density Download PDFInfo
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- CN102445373A CN102445373A CN2011103691652A CN201110369165A CN102445373A CN 102445373 A CN102445373 A CN 102445373A CN 2011103691652 A CN2011103691652 A CN 2011103691652A CN 201110369165 A CN201110369165 A CN 201110369165A CN 102445373 A CN102445373 A CN 102445373A
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Abstract
The invention discloses a detection method of sapphire monocrystal dislocation density. The method comprises steps that: sample sheets are cut from a sapphire sample, and a small hole is provided on the edge of each sample sheet; the sample sheets are washed by using ethanol and deionized water, and are dried by blowing by using inert gas; the sheets are suspended by using molybdenum wires through the small holes; a KOH solution is added into a corrosion vessel, a heating furnace is heated, such that the KOH solution is heated; the sample sheets are immersed in the KOH solution; a plurality of detection planes are selected on the upper surfaces of the sample sheets; a dislocation corrosion pit number on each detection plane is counted under a metallurgical microscope; a dislocation corrosion pit density corresponding to each selected detection plane of the sample sheets is calculated; a dislocation corrosion pit average density of each sample sheet cut from a corresponding direction is calculated; and the dislocation corrosion pit average density of the sapphire sample is calculated. With the method provided by the invention, the corrosion is more sufficient, the detection result is more precise, the image is clear, and the dislocation density can be conveniently and accurately calculated.
Description
Technical field
The present invention relates to defects from semiconductor materials corrosion detection technique field, especially disclose a kind of sapphire single-crystal dislocation desity detection method.
Background technology
(development of the semiconductor material of Eg＞2.3V) is called third generation electronic material very rapidly, mainly comprises SiC, adamas, GaN etc. in the broad stopband in recent years.With first and second in generation electronic material compare; It is big that third generation electronic material has energy gap; Characteristics such as the electron drift saturated velocity is high, specific inductive capacity is little, good heat conductivity are highly suitable for making radioresistance, high frequency, high-power and superintegrated electron device.Utilize its distinctive energy gap, can also make the luminescent device and the light-detecting device of blue green light and ultraviolet light.Wherein GaN is the best photoelectron material of a kind of Commercial Prospect, and it has the unrivaled superiority of some other materials.Therefore many major companies, laboratory, institution of higher learning and scientific research all drop into a large amount of manpower and materials and develop this new type light electronics device, but difficulty is all compared in the crystal growth of third generation semiconductor material.The fusing point of GaN is high, is difficult to adopt conventional method direct growth GaN monocrystalline.Therefore, in order to satisfy the needs of making device, various extensions are still the main method that obtains high-quality, large size single crystal sheet.
Preparation extension GaN film, main backing material has at present: sapphire, SiC, silicon etc.Comprehensive many-sided consider that sapphire is the most widely used substrate at present.
The quality of sapphire crystal has very big influence to the performance and the yield rate of follow-up film of growing GaN above that and preparation blue light diode, therefore, must at first be guaranteed as the quality of the Sapphire Substrate on basis.Find after deliberation; Dislocation in the sapphire crystal has reduced the life-span of mobility of charge carrier rate and minority carrier; In the device production process, the dislocation in the crystal also can cause the out-of-flatness of diffusion knot simultaneously, directly influences the quality of epitaxial loayer; Cause phenomenons such as electric leakage, puncture, noise, short circuit, performances such as light-electronics device, sound-electronics device and semiconductor devices thermal conductance are had tangible influence.
In order to produce high-quality sapphire wafer, to satisfy the quality requirements of increasingly stringent, except will improving the sapphire wafer technology of preparing, the detection technique of sapphire wafer quality also is a very important link.The quality determining method of research sapphire wafer; Not only can screen qualified sapphire wafer through quality testing; The more important thing is the deficiency of finding the sapphire wafer fabricating technology through quality testing, promote the development of sapphire wafer growth, process technology and the quality of lifting sapphire wafer.Therefore, demonstrating crystal defect, its formation mechanism for deliberation and control and technology for eliminating exactly is very important to the preparation high quality crystal.
Assessment sapphire single-crystal dislocation desity the most directly method is to utilize transmission electron microscope (TEM); But because TEM method specimen preparation complex process; Cycle is long and expense is high; Unsuitable conventional dislocation detects, and the non-uniform Distribution of less sample and dislocation, also can increase the inaccuracy of measurement result.Measure with respect to TEM, wet chemical etching technique is with low cost, and is simple to operate, and visual result is for the observation and the analysis of dislocation provides more practical more fast method.
Summary of the invention
The objective of the invention is to overcome the deficiency that exists in the prior art, provide a kind of testing result more accurately, once can corrode multi-disc sample, simple to operate, a kind of sapphire single-crystal dislocation desity detection method that cost is low simultaneously.
According to technical scheme provided by the invention, said a kind of sapphire single-crystal dislocation desity detection method comprises the steps:
A, on the sapphire samples under the cutting of a plurality of directions thickness be the sample thin slice of 1～2mm, the upper and lower surfaces of sample thin slice is roughly ground and fine grinding, after the polishing, offer the aperture that is used to hang at the edge part of sample thin slice;
B, the sample thin slice of offering the complete primary school hole use earlier alcohol to clean, and use deionized water to clean then, and deionized water cleans the back and uses inert blowing gas dry-eye disease thin slice, and heat-resisting silk thread is hung the sample thin slice through aperture;
C, be that 80%～100% KOH solution adds in the corrosion container with weight percentage; The corrosion container is put into heating furnace; Heating makes KOH solution be warming up to 300～400 ℃ to heating furnace; The sample thin slice that suspension is got up is immersed in the KOH solution, carries out wet etching, and the wet etching time was controlled at 20～30 minutes;
Sample thin slice behind d, the taking-up wet etching; Use washed with de-ionized water; Dry up with inert gas after the washed with de-ionized water, get a plurality of detection faces at the upper surface of each sample thin slice to be checked then, under metaloscope, count the dislocation etch pit number in each detection faces;
E, according to the dislocation etch pit number in the area of detection faces and each detection faces of counting; Calculate the corresponding dislocation corrosion pit density of each selected detection faces on the sample thin slice; Calculate the dislocation etch pit average density of the every sample thin slice that the counterparty upwards cuts down then, calculate the dislocation etch pit average density of this sapphire samples at last.
Inert gas described in the step b is a nitrogen.
Inert gas described in the steps d is a nitrogen.
The present invention has following advantage:
(1), through stationary installation with sample-sapphire wafer vertical hanging in KOH solution, contact with solution better, corrode more fully, testing result is more accurate, and can realize two-sided corrosion;
(2), once can corrode the multi-disc sample simultaneously, simple to operate, cost is low;
(3), adopt KOH to carry out chemical corrosion, clear picture has shown defective more exactly, can make things convenient for accurately to calculate dislocation desity.
Embodiment
Below in conjunction with specific embodiment the present invention is described further.
Embodiment 1
A kind of sapphire single-crystal dislocation desity detection method comprises the steps:
A, on first sapphire samples, be the sample thin slice of 2mm along epimere, stage casing and next piece thickness of hypomere average level cutting; They are respectively epimere sample thin slice, mid-stream sample thin slice and hypomere sample thin slice; The upper and lower surfaces of three sample thin slices is roughly ground and fine grinding; After the polishing, offering diameter at the edge part of sample thin slice is the aperture that is used to hang about 2mm;
B, the sample thin slice of offering the complete primary school hole use earlier alcohol to clean alcohol concentration: greater than 99%; Use deionized water to clean then, deionized water cleans the back and uses nitrogen to dry up the sample thin slice, and heat-resisting silk thread (present embodiment employing molybdenum filament) is hung the sample thin slice through aperture;
C, be that 80% KOH solution adds in the corrosion container with weight percentage; The corrosion container is put into heating furnace, and heating makes KOH solution be warming up to 300 ℃ to heating furnace, and the sample thin slice that suspension is got up is immersed in the KOH solution; Carry out wet etching, the wet etching time was controlled at 30 minutes;
Sample thin slice behind d, the taking-up wet etching; Use washed with de-ionized water, dry up with nitrogen after the washed with de-ionized water, get 5 detection faces at the upper surface of each sample thin slice to be checked then; Under metaloscope, count the dislocation etch pit number in each detection faces; Enlargement ratio is 100 times, and the viewing area radius is 0.9mm, area: π r
2Be 2.5447mm
2
E, according to the area of detection faces and count the dislocation etch pit number in each detection faces; Calculate the corresponding dislocation corrosion pit density of each selected detection faces on the sample thin slice; Calculate the dislocation etch pit average density of the sample thin slice that gets off along the first sapphire samples epimere horizontal resection then; Calculate the dislocation etch pit average density of the sample thin slice that cuts off along the first sapphire samples middle section water truncation; Calculate the dislocation etch pit average density of the sample thin slice that gets off along the first sapphire samples hypomere horizontal resection, calculate the dislocation etch pit average density of this sapphire samples at last, see table 1.
Table 1
Embodiment 2
A kind of sapphire single-crystal dislocation desity detection method comprises the steps:
A, on second sapphire samples, all cut the sample thin slice that next piece thickness is 1.5mm to the left abreast along epimere, stage casing and hypomere; They are respectively epimere sample thin slice, mid-stream sample thin slice and hypomere sample thin slice; The upper and lower surfaces of three sample thin slices is roughly ground and fine grinding; After the polishing, offering diameter at the edge part of sample thin slice is the aperture that is used to hang about 2mm;
B, the sample thin slice of offering the complete primary school hole use earlier alcohol to clean alcohol concentration: greater than 99%; Use deionized water to clean then, deionized water cleans the back and uses nitrogen to dry up the sample thin slice, and heat-resisting silk thread (present embodiment employing molybdenum filament) is hung the sample thin slice through aperture;
C, be that 90% KOH solution adds in the corrosion container with weight percentage; The corrosion container is put into heating furnace, and heating makes KOH solution be warming up to 350 ℃ to heating furnace, and the sample thin slice that suspension is got up is immersed in the KOH solution; Carry out wet etching, the wet etching time was controlled at 25 minutes;
Sample thin slice behind d, the taking-up wet etching; Use washed with de-ionized water, dry up with nitrogen after the washed with de-ionized water, get 6 detection faces at the upper surface of each sample thin slice to be checked then; Under metaloscope, count the dislocation etch pit number in each detection faces; Enlargement ratio is 100 times, and the viewing area radius is 0.9mm, area π r
2Be 2.5447mm
2
E, according to the area of detection faces and count the dislocation etch pit number in each detection faces; Calculate the corresponding dislocation corrosion pit density of each selected detection faces on the sample thin slice; Calculate the dislocation etch pit average density of the sample thin slice that cuts down to the left along the second sapphire samples epimere then; Calculate the dislocation etch pit average density of the sample thin slice that cuts down to the left along the second sapphire samples stage casing; Calculate the dislocation etch pit average density of the sample thin slice that cuts down to the left along the second sapphire samples hypomere, calculate the dislocation etch pit average density of this sapphire samples at last, see table 2.
Table 2
Embodiment 3
A kind of sapphire single-crystal dislocation desity detection method comprises the steps:
A, on the 3rd sapphire samples, all cut the sample thin slice that next piece thickness is 1mm to the right abreast along epimere, stage casing and hypomere; They are respectively epimere sample thin slice, mid-stream sample thin slice and hypomere sample thin slice; The upper and lower surfaces of three sample thin slices is roughly ground and fine grinding; After the polishing, offering diameter at the edge part of sample thin slice is the aperture that is used to hang about 2mm;
B, the sample thin slice of offering the complete primary school hole use earlier alcohol to clean alcohol concentration: greater than 99%; Use deionized water to clean then, deionized water cleans the back and uses nitrogen to dry up the sample thin slice, and heat-resisting silk thread (present embodiment employing molybdenum filament) is hung the sample thin slice through aperture;
C, pure KOH is added in the corrosion container; The corrosion container is put into heating furnace, and heating makes KOH solution be warming up to 400 ℃ to heating furnace, and the sample thin slice that suspension is got up is immersed in the KOH fused solution; Carry out wet etching, the wet etching time was controlled at 20 minutes;
Sample thin slice behind d, the taking-up wet etching; Use washed with de-ionized water, dry up with nitrogen after the washed with de-ionized water, get 7 detection faces at the upper surface of each sample thin slice to be checked then; Under metaloscope, count the dislocation etch pit number in each detection faces; Enlargement ratio is 100 times, and the viewing area radius is 0.9mm, area π r
2Be 2.5447mm
2
E, according to the area of detection faces and count the dislocation etch pit number in each detection faces; Calculate the corresponding dislocation corrosion pit density of each selected detection faces on the sample thin slice; Calculate the dislocation etch pit average density of the sample thin slice that cuts down to the right along the 3rd sapphire samples epimere then; Calculate the dislocation etch pit average density of the sample thin slice that cuts down to the right along the 3rd sapphire samples stage casing; Calculate the dislocation etch pit average density of the sample thin slice that cuts down to the right along the 3rd sapphire samples hypomere, calculate the dislocation etch pit average density of this sapphire samples at last, see table 3.
Table 3
Claims (3)
1. a sapphire single-crystal dislocation desity detection method is characterized in that this detection method comprises the steps:
A, on the sapphire samples under the cutting of a plurality of directions thickness be the sample thin slice of 1 ~ 2mm, the upper and lower surfaces of sample thin slice is roughly ground and fine grinding, after the polishing, offer the aperture that is used to hang at the edge part of sample thin slice;
B, the sample thin slice of offering the complete primary school hole use earlier alcohol to clean, and use deionized water to clean then, and deionized water cleans the back and uses inert blowing gas dry-eye disease thin slice, and heat-resisting silk thread is hung the sample thin slice through aperture;
C, be that 80% ~ 100% KOH solution adds in the corrosion container with weight percentage; The corrosion container is put into heating furnace; The heating furnace heating makes KOH solution be warming up to 300 ~ 400 ℃; The sample thin slice that suspension is got up is immersed in the KOH solution, carries out wet etching, and the wet etching time was controlled at 20 ~ 30 minutes;
Sample thin slice behind d, the taking-up wet etching; Use washed with de-ionized water; Dry up with inert gas after the washed with de-ionized water, get a plurality of detection faces at the upper surface of each sample thin slice to be checked then, under metaloscope, count the dislocation etch pit number in each detection faces;
E, according to the dislocation etch pit number in the area of detection faces and each detection faces of counting; Calculate the corresponding dislocation corrosion pit density of each selected detection faces on the sample thin slice; Calculate the dislocation etch pit average density of the every sample thin slice that the counterparty upwards cuts down then, calculate the dislocation etch pit average density of this sapphire samples at last.
2. a kind of sapphire single-crystal dislocation desity detection method as claimed in claim 1, it is characterized in that: the inert gas described in the step b is a nitrogen.
3. a kind of sapphire single-crystal dislocation desity detection method as claimed in claim 1, it is characterized in that: the inert gas described in the steps d is a nitrogen.
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Cited By (4)
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|---|---|---|---|---|
| CN103487453A (en) * | 2013-08-20 | 2014-01-01 | 南京信息工程大学 | Measuring method for dislocation density of heteroepitaxially grown gallium nitride |
| CN103698339A (en) * | 2013-12-29 | 2014-04-02 | 云南北方驰宏光电有限公司 | Crystal dislocation corrosion detection method |
| CN112504724A (en) * | 2020-12-10 | 2021-03-16 | 北方民族大学 | Method for detecting c-plane growth dislocation density of sapphire wafer |
| CN116577340A (en) * | 2023-05-28 | 2023-08-11 | 兰州大学 | Method for distinguishing threading screw dislocation and threading edge dislocation in silicon carbide |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103487453A (en) * | 2013-08-20 | 2014-01-01 | 南京信息工程大学 | Measuring method for dislocation density of heteroepitaxially grown gallium nitride |
| CN103698339A (en) * | 2013-12-29 | 2014-04-02 | 云南北方驰宏光电有限公司 | Crystal dislocation corrosion detection method |
| CN103698339B (en) * | 2013-12-29 | 2015-12-09 | 云南北方驰宏光电有限公司 | A kind of crystal dislocation corrosion detection method |
| CN112504724A (en) * | 2020-12-10 | 2021-03-16 | 北方民族大学 | Method for detecting c-plane growth dislocation density of sapphire wafer |
| CN116577340A (en) * | 2023-05-28 | 2023-08-11 | 兰州大学 | Method for distinguishing threading screw dislocation and threading edge dislocation in silicon carbide |
| CN116577340B (en) * | 2023-05-28 | 2024-01-05 | 兰州大学 | Method for distinguishing threading screw dislocation and threading edge dislocation in silicon carbide |
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Application publication date: 20120509 |