CN103590113A - Monocrystalline silicon dislocation corrosive agent and detection method - Google Patents
Monocrystalline silicon dislocation corrosive agent and detection method Download PDFInfo
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- CN103590113A CN103590113A CN201310576502.4A CN201310576502A CN103590113A CN 103590113 A CN103590113 A CN 103590113A CN 201310576502 A CN201310576502 A CN 201310576502A CN 103590113 A CN103590113 A CN 103590113A
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Abstract
The invention discloses a monocrystalline silicon dislocation corrosive agent which comprises hydrofluoric acid, nitric acid and a slow-release agent, wherein the slow-release agent is a boric acid solution. The monocrystalline silicon dislocation corrosive agent can corrode low density dislocation, and is free from pungent smell and environment-friendly. A monocrystalline silicon dislocation detection method comprises the step of immersing monocrystalline silicon to be detected in the monocrystalline silicon dislocation corrosive agent for corrosion, and is simple and good in detection effect.
Description
Technical field
The invention belongs to silicon single crystal defect detecting technique field, relate to a kind of dislocation of monocrystalline silicon etching reagent, also relate to dislocation of monocrystalline silicon detection method.
Background technology
Along with the development of world economy, modernization construction constantly increases high efficient energy sources demand.Photovoltaic generation is a kind of as the main energy sources of green energy resource and human kind sustainable development, is day by day subject to the attention of countries in the world and is greatly developed.Monocrystalline silicon piece is a kind of as the base mateiral of photovoltaic generation, has the market requirement widely.In silicon single crystal rod process of growth, the reasons such as thermal shocking or thermal stresses are introduced dislocation in crystal.The generation of dislocation not only affects the life-span, mobility of minority carrier etc., also affects the performance of P-N knot, so, is directly connected to the electricity conversion of solar cell.
The detection of silicon single crystal rod or silicon chip dislocation, is used etching pit explicit representation conventionally, that is, first use dislocation corrosion agent to carry out corrosion treatment to sample, then observe the features such as density of dislocation.Conventional a kind of etching reagent is Sirtl corrosive fluid, contains heavy metal chromium ion, because of contaminate environment disabled gradually.Another kind of Dash corrosive fluid, is difficult to erode away low-density dislocation, can not adapt to the demand high-quality to silicon chip.In addition, the acetic acid that this corrosive fluid contains has strong impulse smell, also to actually operating, brings inconvenience.
Summary of the invention
The object of the present invention is to provide a kind of dislocation of monocrystalline silicon etching reagent, solve the not environmental protection of existing etching reagent or the difficult problem that detects low-dislocation-density.
Second object of the present invention is to provide the method for utilizing above-mentioned etching reagent to carry out dislocation of monocrystalline silicon detection.
Technical scheme of the present invention is, dislocation of monocrystalline silicon etching reagent, is comprised of hydrofluoric acid, nitric acid and sustained release dosage, and sustained release dosage is boric acid solution.
Feature of the present invention is also:
Mark meter by volume, the ratio of hydrofluoric acid, nitric acid and boric acid solution is 1.0:3.0:3.0-10.0, and wherein, the mass concentration of hydrofluoric acid is 40-49%, and the mass concentration of nitric acid is 65-68%, and the mass concentration of boric acid solution is 10%.
Preferably, the mass concentration of hydrofluoric acid is 40-42%, and the mass concentration of nitric acid is 65%, and the mass concentration of boric acid solution is 10%.
Preferably, mark meter by volume, the ratio of hydrofluoric acid, nitric acid and sustained release dosage is 1.0:3.0:5.5-6.5.
Second technical scheme of the present invention be, utilizes above-mentioned dislocation of monocrystalline silicon etching reagent to carry out the method for dislocation detection, and silicon single crystal to be detected is immersed in above-mentioned dislocation of monocrystalline silicon etching reagent and corroded.
Silicon single crystal to be detected is silicon single crystal rod, and etching time is 18 minutes to 40 minutes.
Silicon single crystal to be detected is monocrystalline silicon piece, and etching time is 8 minutes to 20 minutes.
After silicon single crystal to be detected is corroded, it is cleaned, then observe.
Above-mentioned observation is with the naked eye directly to observe or by microscopic examination.
The present invention has following beneficial effect:
1, dislocation corrosion agent of the present invention is comprised of hydrofluoric acid, nitric acid and sustained release dosage, has no irritating odor, pollution-free, and can erode away low-density dislocation, can meet the demand high-quality to silicon chip.
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 of first embodiment of the invention corrodes;
Fig. 2 is the surface picture after the silicon single crystal rod coupongs of third embodiment of the invention corrode.
Embodiment
Below in conjunction with accompanying drawing and a plurality of embodiment to dislocation of monocrystalline silicon etching reagent of the present invention and dislocation detection method and be elaborated.
Embodiment 1, and first dislocation of monocrystalline silicon detection method, provides dislocation of monocrystalline silicon etching reagent and silicon single crystal to be detected.
Dislocation of monocrystalline silicon etching reagent is comprised of hydrofluoric acid, nitric acid and sustained release dosage.Sustained release dosage is boric acid solution.The mass concentration of hydrofluoric acid is 40-49%, and the mass concentration of nitric acid is 65-68%.In the present embodiment, silicon single crystal to be detected is monocrystalline silicon piece.Hydrofluoric acid and nitric acid are commercially available reagent, and the mass concentration of hydrofluoric acid is 40-42%, and the mass concentration of nitric acid is 65%.The mass concentration of boric acid solution is 10%, and the mass ratio that boric acid powder and pure water can be pressed to 1:9 is formulated.The ratio of hydrofluoric acid, nitric acid and boric acid solution is 1.0:3.0:3.1, can be also 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, the ratio of hydrofluoric acid, nitric acid and boric acid solution is 1.0:3.0:5.5.
Then, monocrystalline silicon piece to be detected is immersed in dislocation of monocrystalline silicon etching reagent and corroded.
Before corrosion, need to first clean to remove to monocrystalline silicon piece the spot etc. of its surperficial dust, then it is carried out to chemical rightenning to remove surperficial mechanical damage layer.Monocrystalline silicon piece is all immersed in dislocation of monocrystalline silicon etching reagent and corroded, and etching time is 8 minutes to 20 minutes.In the present embodiment, etching time is 15 minutes.
Then, silicon single crystal is cleaned.Monocrystalline silicon piece can be inserted in rinse tank and cleaned, if desired, can carry out repeatedly rinsing.
Finally, observe silicon single crystal.In the present embodiment, monocrystalline silicon piece is placed under microscope, while amplifying 400 times, can be observed picture as shown in Figure 1, visible significantly corrosion pit in figure.By statistics, dislocation desity is about 400/cm
2.
Embodiment 2, dislocation of monocrystalline silicon detection method, and its step and the first embodiment's is basic identical, and its difference is, and in the dislocation of monocrystalline silicon etching reagent of use, the ratio of hydrofluoric acid, nitric acid and boric acid solution is 1.0:3.0:9.0.Silicon single crystal to be detected is also monocrystalline silicon piece, and takes from the same length place with the same silicon single crystal rod of monocrystalline silicon piece of the first embodiment.While observing the Corrosion results of monocrystalline silicon piece, obtain the picture of similar Fig. 1, the dislocation desity of statistics is about 400/cm
2.
Embodiment 3, and first dislocation of monocrystalline silicon detection method, provides dislocation of monocrystalline silicon etching reagent and silicon single crystal to be detected.Dislocation of monocrystalline silicon etching reagent is comprised of hydrofluoric acid, nitric acid and boric acid solution, and in the present embodiment, the mass concentration of hydrofluoric acid is 40-42%, and the mass concentration of nitric acid is 65%, and the mass concentration of boric acid solution is 10%.The ratio of hydrofluoric acid, nitric acid and boric acid solution is 1.0:3.0:5.8, can be also 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 hydrofluoric acid, nitric acid and boric acid solution is 1.0:3.0:6.5.Silicon single crystal to be detected is single crystal rod, in the present embodiment, is monocrystalline silicon round rod.
In the present embodiment, contrast experiment is set, the nitric acid that the hydrofluoric acid that use is 40-42% by mass concentration, mass concentration are 65% and the mass concentration Dash corrosive fluid that to be 99.5% acetic acid form with the volume ratio of 1.0:3.0:9.0 is that monocrystalline silicon round rod immerses described Dash corrosive fluid and corrodes by silicon single crystal to be detected.Corrode after 30 minutes, take out monocrystalline silicon round rod, adopt naked eyes directly to observe, fail to observe dislocation line.
Then, silicon single crystal to be detected is immersed in above-mentioned dislocation of monocrystalline silicon etching reagent and corroded.
Clean monocrystalline silicon round rod, is inserted in the dislocation of monocrystalline silicon etching reagent that this enforcement provides and is corroded, and etching time is 18 minutes to 40 minutes.In the present embodiment, etching time is 30 minutes.
Then, silicon single crystal is cleaned.
Finally, observe silicon single crystal.In the present embodiment, with the naked eye directly observe, can see dislocation line on monocrystalline silicon round rod surface.Visible, the dislocation of monocrystalline silicon etching reagent of use the technical program embodiment, the dislocation that the corrodible etching reagent having can not erode away.
For further confirming the dislocation degree of monocrystalline silicon round rod, can, at the dislocation line termination coupongs of monocrystalline silicon round rod, after clean also chemical rightenning, adopt aforesaid dislocation of monocrystalline silicon etching reagent corrosion.After clean, described print is placed under microscope, amplifies 400 times of pictures that can be observed as shown in Figure 2, visible significantly corrosion pit in figure.By statistics, dislocation desity is about 3000/cm
2.
The invention provides a kind of dislocation of monocrystalline silicon etching reagent, solved not environmental protection or the difficult problem that detects low-dislocation-density of existing dislocation of monocrystalline silicon etching reagent.
Claims (9)
1. dislocation of monocrystalline silicon etching reagent, is characterized in that: hydrofluoric acid, nitric acid and sustained release dosage, consist of, described sustained release dosage is boric acid solution.
2. dislocation of monocrystalline silicon etching reagent according to claim 1, it is characterized in that: mark meter by volume, the ratio of hydrofluoric acid, nitric acid and boric acid solution is 1.0:3.0:3.0-10.0, wherein, the mass concentration of hydrofluoric acid is 40-49%, the mass concentration of nitric acid is 65-68%, and the mass concentration of boric acid solution is 10%.
3. dislocation of monocrystalline silicon etching reagent according to claim 2, is characterized in that: the mass concentration of hydrofluoric acid is 40-42%, and the mass concentration of nitric acid is 65%, and the mass concentration of boric acid solution is 10%.
4. according to the dislocation of monocrystalline silicon etching reagent described in claim 2 or 3, it is characterized in that: mark meter by volume, the ratio of hydrofluoric acid, nitric acid and sustained release dosage is 1.0:3.0:5.5-6.5.
5. the method that misplaces and detect according to dislocation of monocrystalline silicon etching reagent described in claim 1-4 any one, is characterized in that: silicon single crystal to be detected is immersed in described dislocation of monocrystalline silicon etching reagent and corroded.
6. the method that dislocation of monocrystalline silicon etching reagent misplaces and detects according to claim 5, is characterized in that: silicon single crystal to be detected is silicon single crystal rod, etching time is 18 minutes to 40 minutes.
7. the method that dislocation of monocrystalline silicon etching reagent misplaces and detects according to claim 5, is characterized in that: silicon single crystal to be detected is monocrystalline silicon piece, etching time is 8 minutes to 20 minutes.
8. the method that misplaces and detect according to dislocation of monocrystalline silicon etching reagent described in claim 5-7 any one, is characterized in that: after silicon single crystal to be detected is corroded, it is cleaned, then observe.
9. the method that dislocation of monocrystalline silicon etching reagent misplaces and detects according to claim 8, is characterized in that: described observation is with the naked eye directly to observe or by microscopic examination.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108396321A (en) * | 2018-03-07 | 2018-08-14 | 济南大学 | A kind of metallographic etchant for austenitic stainless steel and its prepare caustic solution |
| CN110849875A (en) * | 2019-10-10 | 2020-02-28 | 新余学院 | Method for analyzing microstructure of cast polycrystalline silicon |
| CN111411360A (en) * | 2020-04-03 | 2020-07-14 | 广东韶钢松山股份有限公司 | Metallographic corrosive agent and application thereof |
| CN113845917A (en) * | 2021-09-24 | 2021-12-28 | 上海提牛机电设备有限公司 | Cleaning solution and cleaning method for bent wafer |
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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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Patent Citations (2)
| 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 |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108396321A (en) * | 2018-03-07 | 2018-08-14 | 济南大学 | A kind of metallographic etchant for austenitic stainless steel and its prepare caustic solution |
| 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 |
| CN111411360A (en) * | 2020-04-03 | 2020-07-14 | 广东韶钢松山股份有限公司 | Metallographic corrosive agent and application thereof |
| 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 |
| CN113845917A (en) * | 2021-09-24 | 2021-12-28 | 上海提牛机电设备有限公司 | Cleaning solution and cleaning method for bent wafer |
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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. |
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