CN103590113B - Monocrystalline silicon dislocation corrosive agent and detection method - Google Patents
Monocrystalline silicon dislocation corrosive agent and detection method Download PDFInfo
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- CN103590113B CN103590113B CN201310576502.4A CN201310576502A CN103590113B CN 103590113 B CN103590113 B CN 103590113B CN 201310576502 A CN201310576502 A CN 201310576502A CN 103590113 B CN103590113 B CN 103590113B
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Abstract
The invention discloses a kind of Monocrystalline silicon dislocation corrosive agent, be made up of Fluohydric acid., nitric acid and slow releasing agent, described slow releasing agent is boric acid solution.This Monocrystalline silicon dislocation corrosive agent can be corroded and low-density dislocation, and has no irritating odor, environmental friendliness.Dislocation of monocrystalline silicon detection method of the present invention is to immerse monocrystal silicon to be detected in Monocrystalline silicon dislocation corrosive agent to corrode, and method is simple, and Detection results is good.
Description
Technical field
The invention belongs to monocrystal silicon defect detecting technique field, relate to a kind of Monocrystalline silicon dislocation corrosive agent, also
Relate to dislocation of monocrystalline silicon detection method.
Background technology
Along with the development of World Economics, high efficient energy sources demand is constantly increased by modernization construction.Photovoltaic
Generating, as green energy resource and the one of the main energy sources of human kind sustainable development, is increasingly subject to the world each
The attention of state is also greatly developed.Monocrystalline silicon piece, as the one of the basic material of photovoltaic generation, has
The market demand widely.In silicon single crystal rod growth course, the reason such as thermal shock or thermal stress is drawn in crystal
Enter dislocation.The generation of dislocation not only affects the life-span of minority carrier, mobility etc., has an effect on P-N junction
Performance, so, be directly connected to the electricity conversion of solaode.
Silicon single crystal rod or the detection of silicon chip dislocation, generally use etching pit explicit representation, i.e. first use position
Wrong caustic carries out corrosion treatmentCorrosion Science to sample, then observes the feature such as density of dislocation.Conventional a kind of caustic
For Sirtl corrosive liquid, containing heavy metal chromium ion, the most disabled because polluting environment.Another kind of Dash
Corrosive liquid, it is difficult to corrode and low-density dislocation, it is impossible to adapt to the demand to silicon chip high-quality.It addition,
The acetic acid that this corrosive liquid contains has strong impulse abnormal smells from the patient, also brings inconvenience to practical operation.
Summary of the invention
It is an object of the invention to provide a kind of Monocrystalline silicon dislocation corrosive agent, solve existing caustic not ring
The problem that guarantor or difficulty detect low-dislocation-density.
Second object of the present invention is to provide the side utilizing above-mentioned caustic to carry out dislocation of monocrystalline silicon detection
Method.
The technical scheme is that, Monocrystalline silicon dislocation corrosive agent, by Fluohydric acid., nitric acid and slow releasing agent group
Becoming, slow releasing agent is boric acid solution.
The feature of the present invention also resides in:
By volume mark meter, the ratio of Fluohydric acid., nitric acid and boric acid solution is 1.0:3.0:3.0-10.0, its
In, the mass concentration of Fluohydric acid. is 40-49%, and the mass concentration of nitric acid is 65-68%, boric acid solution
Mass concentration is 10%.
Preferably, the mass concentration of Fluohydric acid. is 40-42%, and the mass concentration of nitric acid is 65%, and boric acid is molten
The mass concentration of liquid is 10%.
Preferably, by volume mark meter, the ratio of Fluohydric acid., nitric acid and slow releasing agent is 1.0:3.0:5.5-6.5.
Second technical scheme of the present invention is to utilize above-mentioned Monocrystalline silicon dislocation corrosive agent to carry out dislocation detection
Method, monocrystal silicon to be detected is immersed in above-mentioned Monocrystalline silicon dislocation corrosive agent and corrodes.
Monocrystal silicon to be detected is silicon single crystal rod, and etching time is 18 minutes to 40 minutes.
Monocrystal silicon to be detected is monocrystalline silicon piece, and etching time is 8 minutes to 20 minutes.
After monocrystal silicon to be detected is corroded, it is carried out, then observes.
Above-mentioned observation is with the naked eye directly to observe or observe by microscope.
There is advantages that
1, dislocation corrosion agent of the present invention is made up of Fluohydric acid., nitric acid and slow releasing agent, has no irritating odor,
Pollution-free, and can corrode and low-density dislocation, the demand to silicon chip high-quality can be met.
2, dislocation detection method of the present invention is simple, and corrosive effect is good.
Accompanying drawing explanation
Fig. 1 is the surface picture after the monocrystalline silicon piece corrosion of first embodiment of the invention；
Fig. 2 is the surface picture after the silicon single crystal rod coupongs corrosion of third embodiment of the invention.
Detailed description of the invention
With multiple embodiments, Monocrystalline silicon dislocation corrosive agent and the dislocation of the present invention are detected below in conjunction with the accompanying drawings
Method and being described in detail.
Embodiment 1, dislocation of monocrystalline silicon detection method, first, it is provided that Monocrystalline silicon dislocation corrosive agent and to be checked
The monocrystal silicon surveyed.
Monocrystalline silicon dislocation corrosive agent is made up of Fluohydric acid., nitric acid and slow releasing agent.Slow releasing agent is boric acid solution.
The mass concentration of Fluohydric acid. is 40-49%, and the mass concentration of nitric acid is 65-68%.In the present embodiment, treat
The monocrystal silicon of detection is monocrystalline silicon piece.Fluohydric acid. and nitric acid are commercially available reagent, and the quality of Fluohydric acid. is dense
Degree is 40-42%, and the mass concentration of nitric acid is 65%.The mass concentration of boric acid solution is 10%, can be by
The mass ratio that boric acid powder and pure water press 1:9 is formulated.The ratio of Fluohydric acid., nitric acid and boric acid solution
For 1.0:3.0:3.1, it is also possible to for 1.0:3.0:3.3,1.0:3.0:3.5,1.0:3.0:3.9,1.0:3.0:4.0,
1.0:3.0:4.3、1.0:3.0:4.7、1.0:3.0:4.8、1.0:3.0:5.1、1.0:3.0:5.3、1.0:3.0:5.6、
1.0:3.0:5.9,1.0:3.0:6.1 or 1.0:3.0:6.4.Preferably, Fluohydric acid., nitric acid and boric acid solution
Ratio is 1.0:3.0:5.5.
Then, will monocrystalline silicon piece immersion Monocrystalline silicon dislocation corrosive agent to be detected be corroded.
Before corrosion, need first to be cleaned removing the spot of the dust on its surface to monocrystalline silicon piece
Deng, then it is carried out chemical polishing to remove the mechanical damage layer on surface.Monocrystalline silicon piece is totally immersed into list
Corroding in crystal silicon dislocation corrosion agent, etching time is 8 minutes to 20 minutes.In the present embodiment,
Etching time is 15 minutes.
Then, monocrystal silicon is cleaned.Clean in monocrystalline silicon piece can be inserted potcher, if desired,
Can repeatedly rinse.
Finally, monocrystal silicon is observed.In the present embodiment, monocrystalline silicon piece is placed under microscope, amplifies 400
Times time, picture as shown in Figure 1 be can be observed, visible significantly etch pit in figure.Through statistics, dislocation
Density is about 400/cm2。
Embodiment 2, dislocation of monocrystalline silicon detection method, its step is essentially identical with first embodiment, its
Difference is, in the Monocrystalline silicon dislocation corrosive agent of use, the ratio of Fluohydric acid., nitric acid and boric acid solution is
1.0:3.0:9.0.Monocrystal silicon to be detected is also monocrystalline silicon piece, and takes from the monocrystal silicon with first embodiment
At the same length of same silicon single crystal rod of sheet.When observing the Corrosion results of monocrystalline silicon piece, obtain similar figure
The picture of 1, the dislocation density of statistics is about 400/cm2。
Embodiment 3, dislocation of monocrystalline silicon detection method, first, it is provided that Monocrystalline silicon dislocation corrosive agent and to be checked
The monocrystal silicon surveyed.Monocrystalline silicon dislocation corrosive agent is made up of Fluohydric acid., nitric acid and boric acid solution, the present embodiment
In, the mass concentration of Fluohydric acid. is 40-42%, and the mass concentration of nitric acid is 65%, the matter of boric acid solution
Amount concentration is 10%.The ratio of Fluohydric acid., nitric acid and boric acid solution is 1.0:3.0:5.8, it is also possible to for
1.0:3.0:6.3、1.0:3.0:6.8、1.0:3.0:6.9、1.0:3.0:7.1、1.0:3.0:7.4、1.0:3.0:7.8、
1.0:3.0:8.1,1.0:3.0:8.3,1.0:3.0:8.7,1.0:3.0:9.2,1.0:3.0:9.3,1.0:3.0:9.5 or
1.0:3.0:9.9.Preferably, the ratio of Fluohydric acid., nitric acid and boric acid solution is 1.0:3.0:6.5.To be detected
Monocrystal silicon be monocrystal rod, in the present embodiment, for monocrystalline silicon round rod.
In the present embodiment, arranging contrast experiment, using by mass concentration is the Fluohydric acid. of 40-42%, matter
Amount concentration be 65% nitric acid and mass concentration to be 99.5% acetic acid form with the volume ratio of 1.0:3.0:9.0
Dash corrosive liquid, carries out corruption by the monocrystal silicon to be detected i.e. monocrystalline silicon round rod described Dash corrosive liquid of immersion
Erosion.After corroding 30 minutes, take out monocrystalline silicon round rod, use direct visual perception, not it is observed that position
Wrong line.
Then, will the monocrystal silicon above-mentioned Monocrystalline silicon dislocation corrosive agent of immersion to be detected be corroded.
Cleaning monocrystalline silicon round rod, is put in the Monocrystalline silicon dislocation corrosive agent that this enforcement provides carrying out corruption
Erosion, etching time is 18 minutes to 40 minutes.In the present embodiment, etching time is 30 minutes.
Then, monocrystal silicon is cleaned.
Finally, monocrystal silicon is observed.In the present embodiment, the most directly observe, can be at monocrystalline silicon round rod table
Dislocation line is seen in face.Visible, use the Monocrystalline silicon dislocation corrosive agent of the technical program embodiment, corrodible
The caustic having can not corrode the dislocation.
For further confirming the dislocation degree of monocrystalline silicon round rod, can terminate at the dislocation line of monocrystalline silicon round rod
Place's coupongs, after cleaning chemical polishing, use aforesaid Monocrystalline silicon dislocation corrosive agent to corrode.Cleaning
After described print is placed under microscope, amplify 400 times of pictures that can be observed as shown in Figure 2, in figure
Visible obvious etch pit.Through statistics, dislocation density is about 3000/cm2。
The invention provides a kind of Monocrystalline silicon dislocation corrosive agent, solve existing Monocrystalline silicon dislocation corrosive agent
Not environmentally or the difficulty problem that detects low-dislocation-density.
Claims (6)
1. Monocrystalline silicon dislocation corrosive agent, it is characterised in that: it is made up of Fluohydric acid., nitric acid and slow releasing agent, institute
Stating slow releasing agent is boric acid solution, by volume mark meter, and the ratio of Fluohydric acid., nitric acid and boric acid solution is
1.0:3.0:5.5-6.5, wherein, the mass concentration of Fluohydric acid. is 40-42%, and the mass concentration of nitric acid is 65%,
The mass concentration of boric acid solution is 10%.
The method that the most according to claim 1, Monocrystalline silicon dislocation corrosive agent carries out dislocation detection, its feature
It is: monocrystal silicon to be detected is immersed in described Monocrystalline silicon dislocation corrosive agent and corrodes.
The method that the most according to claim 2, Monocrystalline silicon dislocation corrosive agent carries out dislocation detection, it is special
Levying and be: monocrystal silicon to be detected is silicon single crystal rod, etching time is 18 minutes to 40 minutes.
The method that the most according to claim 2, Monocrystalline silicon dislocation corrosive agent carries out dislocation detection, it is special
Levying and be: monocrystal silicon to be detected is monocrystalline silicon piece, etching time is 8 minutes to 20 minutes.
5. the side of dislocation detection is carried out according to Monocrystalline silicon dislocation corrosive agent described in any one of claim 2-4
Method, it is characterised in that: after monocrystal silicon to be detected is corroded, it is carried out, then
Observe.
The method that the most according to claim 5, Monocrystalline silicon dislocation corrosive agent carries out dislocation detection, it is special
Levy and be: described observation is with the naked eye directly to observe or observe by microscope.
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| CN108396321B (en) * | 2018-03-07 | 2020-01-21 | 济南大学 | Metallographic corrosive liquid for austenitic stainless steel and preparation corrosion method thereof |
| CN110849875A (en) * | 2019-10-10 | 2020-02-28 | 新余学院 | Method for analyzing microstructure of cast polycrystalline silicon |
| CN111411360B (en) * | 2020-04-03 | 2022-06-10 | 广东韶钢松山股份有限公司 | Metallographic corrosive agent and application thereof |
| CN113845917B (en) * | 2021-09-24 | 2022-09-16 | 上海提牛机电设备有限公司 | Cleaning solution and cleaning method for bent wafer |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102776570A (en) * | 2011-05-11 | 2012-11-14 | 镇江荣德新能源科技有限公司 | Solar-grade mono-crystalline crystal brick surface treatment method |
| CN102931282A (en) * | 2012-11-14 | 2013-02-13 | 东方电气集团(宜兴)迈吉太阳能科技有限公司 | Preparation method of back polished silicon chip |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102776570A (en) * | 2011-05-11 | 2012-11-14 | 镇江荣德新能源科技有限公司 | Solar-grade mono-crystalline crystal brick surface treatment method |
| CN102931282A (en) * | 2012-11-14 | 2013-02-13 | 东方电气集团(宜兴)迈吉太阳能科技有限公司 | Preparation method of back polished silicon chip |
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Address after: 750021 Yinchuan, the Ningxia Hui Autonomous Region (national level) economic and Technological Development Zone Kaiyuan Road, No. 15 Co-patentee after: Longji green energy Polytron Technologies Inc Patentee after: Yinchuan LONGi Silicon Material Co.,Ltd. Co-patentee after: Ningxia LONGi Silicon Material Co.,Ltd. Co-patentee after: Wuxi LONGi Silicon Materials Corp. Address before: 750021 Yinchuan, the Ningxia Hui Autonomous Region (national level) economic and Technological Development Zone Kaiyuan Road, No. 15 Co-patentee before: Xi'an Longji-Silicon Co., LTD. Patentee before: Yinchuan LONGi Silicon Material Co.,Ltd. Co-patentee before: Ningxia LONGi Silicon Material Co.,Ltd. Co-patentee before: Wuxi LONGi Silicon Materials Corp. |
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Effective date of registration: 20211013 Address after: 750021 No.15, Kaiyuan East Road, Yinchuan (National) economic and Technological Development Zone, Ningxia Hui Autonomous Region Patentee after: YINCHUAN LONGI SILICON MATERIALS Co.,Ltd. Address before: 750021 No.15, Kaiyuan East Road, Yinchuan (National) economic and Technological Development Zone, Ningxia Hui Autonomous Region Patentee before: YINCHUAN LONGI SILICON MATERIALS Co.,Ltd. Patentee before: LONGI GREEN ENERGY TECHNOLOGY Co.,Ltd. Patentee before: NINGXIA LONGI SILICON MATERIALS Co.,Ltd. Patentee before: WUXI LONGI SILICON MATERIALS Corp. |