CN104390983A - Corrosion detection method for COP defects in dislocation-free germanium single crystal - Google Patents
Corrosion detection method for COP defects in dislocation-free germanium single crystal Download PDFInfo
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- CN104390983A CN104390983A CN201410740175.6A CN201410740175A CN104390983A CN 104390983 A CN104390983 A CN 104390983A CN 201410740175 A CN201410740175 A CN 201410740175A CN 104390983 A CN104390983 A CN 104390983A
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Abstract
The invention discloses a corrosion detection method for COP defects in a dislocation-free germanium single crystal. The method comprises the following steps: cutting the dislocation-free germanium single crystal to crystal sheets of the thickness of 1-2cm according to the crystal direction, performing rough grinding on one surfaces of the crystal sheets on a carborundum grinding disc, polishing the ground crystal sheets on ground glass until the surfaces of the crystal sheets do not have an obvious scratch; preparing COP corrosive liquid, and cooling to the temperature of 0 DEG C; putting the polished surface of the polished dislocation-free germanium single crystal upwards in the corrosive liquid at the temperature of 0 DEG C, and corroding for 5-8 minutes; and immediately washing and wiping to be dry by using clear water after the corroding operation is ended, and counting the number of the COP defects on the surface of the single crystal under a microscope. With the adoption of the corrosive liquid, a germanium layer on the surface can be corroded, so that a fresh surface is exposed to enable the defects to be exposed, the appearance effect of the COP defects can be guaranteed, the COP morphology can be conveniently observed under the microscope, the number of the COP defects in the dislocation-free germanium single crystal can be accurately detected, and the method is simple and effective.
Description
Technical field
The present invention relates to a kind of single germanium wafer, be specifically related to the detection method of COP defect in a kind of single germanium wafer.
Background technology
In recent years, the p-type germanium single crystal of major diameter (more than 4 inches) heavy doping gallium is because day by day receiving publicity as aerospace field photovoltaic cell substrate material, the advantages such as Ge/GaAs/GaInP tri-junction battery using single germanium wafer as substrate has that transformation efficiency is high, relative weight and little, the excellent anti-cosmic rays radiance of volume, replace traditional silicon battery completely in outer space solar power system.The crystal defects such as the dislocation in such germanium single crystal directly have influence on the critical natures such as gallium arsenide cells fill factor, curve factor (FF), photoelectric transformation efficiency (EFF) and battery life, therefore require that the crystal defects such as such germanium single crystal dislocation are the least possible, external space industry application even requires as dislocation-free.During Grown by CZ Method dislocation-free germanium single crystal, easily form empty type original position point defect in dislocation-free single crystal, i.e. COP defect.Dislocation-free single germanium wafer is used as Ge/GaAs/GaInP tri-junction battery substrate, if there is COP defect in single germanium wafer, will cause battery junction leakage, battery performance is defective, is therefore necessary to detect the COP defect in dislocation-free germanium single crystal.Also there is no the detection method of COP defect in clear and definite dislocation-free single germanium wafer at present.
Summary of the invention
Goal of the invention: the object of the invention is to for the deficiencies in the prior art, provides the corrosion detecting method of COP defect in a kind of dislocation-free single germanium wafer.
Technical scheme: the corrosion detecting method of COP defect in a kind of dislocation-free single germanium wafer, comprises the following steps:
(1) cut out by crystal orientation the wafer that thickness is 1 ~ 2mm from dislocation-free germanium single crystal, the one side of wafer is polished on abrasive disk, on frosted glass, be then polished to wafer surface without obvious cut;
(2) prepare COP corrosive liquid and be cooled to 0 DEG C;
(3) corrosive liquid dislocation-free single germanium wafer polished surface through polishing being put into 0 DEG C upward corrodes, etching time 5 ~ 8 minutes;
(4) rinse well with clear water immediately after etching and dry, count single wafer surface COP defects count under the microscope.
Further, in step COP corrosive liquid described in (2) be nitric acid, the mixed liquor prepared according to volume ratio 4:2:1 of hydrofluorite, copper nitrate, wherein, concentration of nitric acid is 65 ~ 68%, and hydrofluoric acid concentration is 40%, and copper nitrate concentration is 10%.
Beneficial effect: the corrosive liquid that the present invention adopts can corrosion surface one deck germanium, thus expose unsalted surface and expose defect, can ensure that COP defect manifests effect, can easily observe COP pattern under the microscope, can accurately detect COP defects count in dislocation-free single germanium wafer, method is simply effective.
Accompanying drawing explanation
Fig. 1 is the single germanium wafer surface COP defect pattern that the embodiment of the present invention 1 is observed;
Fig. 2 is the single germanium wafer surface COP defect pattern that the embodiment of the present invention 2 is observed;
Fig. 3 is the single germanium wafer surface COP defect pattern that the embodiment of the present invention 3 is observed.
Embodiment
Below technical solution of the present invention is described in detail, but protection scope of the present invention is not limited to described embodiment.
Embodiment 1:
Cut out by certain crystal orientation the wafer that thickness is 1mm from one section of dislocation-free germanium single crystal, the one side of wafer is polished on abrasive disk, on frosted glass, be then polished to wafer surface without obvious cut.Nitric acid (HNO by volume
3): hydrofluorite (HF): copper nitrate (Cu (NO
3)
2)=4:2:1 prepares COP corrosive liquid and is cooled to 0 DEG C, and wherein, concentration of nitric acid is 67%, and hydrofluoric acid concentration is 40%, and copper nitrate concentration is 10%.The corrosive liquid that dislocation-free single germanium wafer polished surface through polishing puts into 0 DEG C is upward corroded, etching time 5 minutes, rinse well with clear water immediately after etching and dry, examine under a microscope single wafer surface COP defect pattern, counting COP defects count is 10.Fig. 1 is the single wafer surface COP defect pattern that the present embodiment is observed.
Embodiment 2:
Cut out by certain crystal orientation the wafer that thickness is 1.5mm from one section of dislocation-free germanium single crystal, the one side of wafer is polished on abrasive disk, on frosted glass, be then polished to wafer surface without obvious cut.Nitric acid (HNO by volume
3): hydrofluorite (HF): copper nitrate (Cu (NO
3)
2)=4:2:1 prepares COP corrosive liquid and is cooled to 0 DEG C, and wherein, concentration of nitric acid is 65%, and hydrofluoric acid concentration is 40%, and copper nitrate concentration is 10%.The corrosive liquid that dislocation-free single germanium wafer polished surface through polishing puts into 0 DEG C is upward corroded, etching time 7 minutes, rinse well with clear water immediately after etching and dry, examine under a microscope single wafer surface COP defect pattern, counting COP defects count is 5.Fig. 2 is the single wafer surface COP defect pattern that the present embodiment is observed.
Embodiment 3:
Cut out by certain crystal orientation the wafer that thickness is 2mm from one section of dislocation-free germanium single crystal, the one side of wafer is polished on abrasive disk, on frosted glass, be then polished to wafer surface without obvious cut.Nitric acid (HNO by volume
3): hydrofluorite (HF): copper nitrate (Cu (NO
3)
2)=4:2:1 prepares COP corrosive liquid and is cooled to 0 DEG C, and wherein, concentration of nitric acid is 68%, and hydrofluoric acid concentration is 40%, and copper nitrate concentration is 10%.The corrosive liquid that dislocation-free single germanium wafer polished surface through polishing puts into 0 DEG C is upward corroded, etching time 8 minutes, rinse well with clear water immediately after etching and dry, examine under a microscope single wafer surface COP defect pattern, counting COP defects count is 12.Fig. 3 is the single wafer surface COP defect pattern that the present embodiment is observed.
Claims (2)
1. the corrosion detecting method of COP defect in dislocation-free single germanium wafer, is characterized in that: comprise the following steps:
(1) cut out by crystal orientation the wafer that thickness is 1 ~ 2mm from dislocation-free germanium single crystal, the one side of wafer is polished on abrasive disk, on frosted glass, be then polished to wafer surface without obvious cut;
(2) prepare COP corrosive liquid and be cooled to 0 DEG C;
(3) corrosive liquid dislocation-free single germanium wafer polished surface through polishing being put into 0 DEG C upward corrodes, etching time 5 ~ 8 minutes;
(4) rinse well with clear water immediately after etching and dry, count single wafer surface COP defects count under the microscope.
2. the corrosion detecting method of COP defect in dislocation-free single germanium wafer according to claim 1, it is characterized in that: in step COP corrosive liquid described in (2) be nitric acid, the mixed liquor prepared according to volume ratio 4:2:1 of hydrofluorite, copper nitrate, wherein, concentration of nitric acid is 65 ~ 68%, hydrofluoric acid concentration is 40%, and copper nitrate concentration is 10%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410740175.6A CN104390983A (en) | 2014-12-09 | 2014-12-09 | Corrosion detection method for COP defects in dislocation-free germanium single crystal |
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| CN201410740175.6A CN104390983A (en) | 2014-12-09 | 2014-12-09 | Corrosion detection method for COP defects in dislocation-free germanium single crystal |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104862702A (en) * | 2015-05-21 | 2015-08-26 | 中国科学院半导体研究所 | Etching solution for dislocation display of monocrystal germanium wafer deflecting to crystal orientation [111] and etching method |
| CN105717137A (en) * | 2016-01-27 | 2016-06-29 | 中国建筑材料科学研究总院 | Silica-glass micro-defect detecting method |
| CN106567079A (en) * | 2016-09-23 | 2017-04-19 | 中锗科技有限公司 | Corrosive liquid for detecting dislocation of monocrystalline germanium slices and corrosion method |
| CN110793986A (en) * | 2019-10-14 | 2020-02-14 | 中国电子科技集团公司第十一研究所 | Method for testing depth of damage layer of InSb wafer |
| CN114088707A (en) * | 2021-10-27 | 2022-02-25 | 安徽光智科技有限公司 | Method for detecting crystal orientation defect of ultra-high pure germanium single crystal <100> |
-
2014
- 2014-12-09 CN CN201410740175.6A patent/CN104390983A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104862702A (en) * | 2015-05-21 | 2015-08-26 | 中国科学院半导体研究所 | Etching solution for dislocation display of monocrystal germanium wafer deflecting to crystal orientation [111] and etching method |
| CN105717137A (en) * | 2016-01-27 | 2016-06-29 | 中国建筑材料科学研究总院 | Silica-glass micro-defect detecting method |
| CN106567079A (en) * | 2016-09-23 | 2017-04-19 | 中锗科技有限公司 | Corrosive liquid for detecting dislocation of monocrystalline germanium slices and corrosion method |
| CN110793986A (en) * | 2019-10-14 | 2020-02-14 | 中国电子科技集团公司第十一研究所 | Method for testing depth of damage layer of InSb wafer |
| CN114088707A (en) * | 2021-10-27 | 2022-02-25 | 安徽光智科技有限公司 | Method for detecting crystal orientation defect of ultra-high pure germanium single crystal <100> |
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Application publication date: 20150304 |
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