CN102866335A - Method for testing oxidation induced fault in czochralski silicon by minority carrier lifetime scanning method - Google Patents
Method for testing oxidation induced fault in czochralski silicon by minority carrier lifetime scanning method Download PDFInfo
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- CN102866335A CN102866335A CN2011101860374A CN201110186037A CN102866335A CN 102866335 A CN102866335 A CN 102866335A CN 2011101860374 A CN2011101860374 A CN 2011101860374A CN 201110186037 A CN201110186037 A CN 201110186037A CN 102866335 A CN102866335 A CN 102866335A
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Abstract
The invention provides a method for testing oxidation induced fault in czochralski silicon by a minority carrier lifetime scanning method. The method includes the steps: firstly, cutting a test sample by a band-sawing machine; secondly, corroding a surface damage layer of the sample with mixed acid solution to make the surface of the sample into a mirror surface; thirdly, cleaning up the sample with cleaning solution; fourthly, placing the sample into a container, adding iodine solution into the container and evenly covering the iodine solution on the surface of the sample; and fifthly, scanning the minority carrier lifetime of the treated sample by a minority carrier lifetime scanning device, and measuring a minority carrier lifetime distribution diagram. The method for testing the oxidation induced fault in the czochralski silicon by the minority carrier lifetime scanning method includes the simple steps, and introduction of equipment and loss of electric quantity are decreased. Sample treatment efficiency is higher, a large amount of time and consumption of auxiliary materials can be saved, and testing cost is reduced.
Description
Technical field
The present invention relates to a kind of method of testing, particularly a kind of minority carrier life time scanning method is tested the method for the oxidation induced fault in the pulling of silicon single crystal, belongs to the detection technique of defective in the monocrystalline silicon.
Background technology
Current sun power has become a kind of novel reproducible clean energy resource progressively to be paid attention to by every country, carrier---the silicon substrate solar battery sheet that therefore utilizes as sun power, just each enterprise product of falling over each other to produce.The monocrystalline silicon of Grown by CZ Method, in the process of making solar battery sheet, easily form oxidation induced stacking fault defects (OSF at the silicon chip that the head of monocrystal rod is cut, Oxidation-Induced Stacking Faults), can reduce greatly the conversion efficiency of the solar battery sheet made from this silicon chip.Therefore, need to there be a kind of method of testing to judge whether monocrystalline silicon piece can form OSF in the process of making cell piece, to guarantee the conversion efficiency of cell piece.
The method whether traditional detection monocrystalline silicon can form OSF is: the oxidizing condition of analog device, and utilize oxidation to come decoration or enlarge defective in the silicon chip, then use preferential etch liquid display defect, and observe with microtechnic.Concrete step is as follows:
1. use inner circle cutting machine, the intercepting crystal bar needs the print of test zone 1～3 millimeters thick.
2. the print edge is polished smooth with chamfering device.
3. (nitric acid: acetic acid: hydrofluorite) surface damage layer with print erodes about 200 microns, and the surface is minute surface with mixed acid solution.
4. open quartz ampoule oxidizing annealing stove, preheat 1000 degrees centigrade.
5. print is put into high-cleanness quartz ampoule oxidizing annealing stove, passed into dried/wet oxygen in (in 10 degrees centigrade of deviations) under 1000 degrees centigrade of steady temperatures, kept 1 hour.Then print is positioned in the clean vent cabinet and is cooled to room temperature.
6. after oxidation is finished, print was soaked in hydrofluorite about 3 minutes, in pure water, clean up.
7. print is positioned over Schimmel (chromium: water: hydrofluorite) corroded about 5～10 minutes in the solution.
8. after pure water cleans up print, with 100 times of optical microscope observation OSF.
The loss ratio of traditional method of testing aspect equipment importing and electric weight is larger, and the efficient aspect the processing of print is also lower, and step is also very loaded down with trivial details, tediously long, and the auxiliary material of consumption are more, just caused testing cost very high.
Summary of the invention
The object of the present invention is to provide a kind of method of testing step terse, reduced the importing of equipment and the loss of electric weight.Efficient is higher, and the minority carrier life time scanning method that can save a large amount of time and auxiliary material and reduction testing cost is tested the method for the oxidation induced fault in the pulling of silicon single crystal.
The method of the oxidation induced fault in the minority carrier life time scanning method test pulling of silicon single crystal of the present invention comprises the steps:
The first step intercepts test sample with band-sawing machine;
Second step corrodes described print surface damage layer with mixed acid solution, makes its surface be minute surface;
In the 3rd step, with cleansing solution described print is cleaned up;
The 4th step, described print is put into container, add again iodine solution, make described iodine solution be covered in uniformly described print surface;
The 5th step, the described print of handling well is scanned described print minority carrier life time with the minority carrier life time scanning device, measure the minority carrier life time distribution pattern.
The thickness of described print is 2 millimeters; Described mixed acid solution is the mixed solution of nitric acid, acetic acid, hydrofluorite, and the volume ratio of nitric acid, acetic acid, hydrofluorite is 5: 3: 2 in the described mixed solution; Described surface damage layer erodes 200 microns; Described container is transparent plastic bag; The described iodine solution that adds is 1 milliliter; The mass percent concentration of described iodine solution is 1%～5%; Described cleansing solution is pure water.
The method step of the oxidation induced fault in the minority carrier life time scanning method test pulling of silicon single crystal of the present invention is terse, has reduced the importing of equipment and the loss of electric weight (the about 35KW of annealing furnace power, the about 2KW of minority carrier life time scanner power).Aspect the print processing, efficient is higher, can save a large amount of time and the use of auxiliary material, has saved testing cost.
Description of drawings
Fig. 1 is the method step block diagram of the oxidation induced fault in the minority carrier life time scanning method test pulling of silicon single crystal of the present invention.
Embodiment
Be described in further detail below in conjunction with the method for accompanying drawing to the oxidation induced fault in the minority carrier life time scanning method test pulling of silicon single crystal of the present invention.
The formation of OSF is owing to be easy to form from the gap silicon atom at the czochralski silicon monocrystal head, and these become circular distribution from the gap silicon atom in silicon single crystal, reacts formation OSF from gap silicon atom and oxygen in follow-up heat treatment process.The minority carrier life time of silicon single crystal can be obviously on the low side at the intensive place of crystal defect, therefore can judge in this monocrystalline silicon whether can form OSF by the minority carrier life time distribution pattern that scans whole silicon chip surface.
As shown in Figure 1, the process of the method for the oxidation induced fault in the minority carrier life time scanning method test pulling of silicon single crystal of the present invention is:
The first step is with the print of about 2 millimeters thick of band-sawing machine intercepting test;
Second step erodes 200 microns with the mixed acid solution of nitric acid, acetic acid and hydrofluorite with the print surface damage layer, makes its surface be minute surface.
In the 3rd step, with pure water print is cleaned up.
The 4th step, print is put into transparent plastic bag, add 1 milliliter of mass percent concentration and be 3% iodine solution, make iodine solution be covered in uniformly the print surface.
In the 5th step, the above-mentioned print of handling well with minority carrier life time scanning device scanning print minority carrier life time, is measured the minority carrier life time distribution pattern.
The silicon chip surface minority carrier life time distributes and low distribution pattern of ring-type life-span obviously to occur, then can judge exist in this monocrystalline silicon ring-type from the gap silicon atom, in follow-up heat treatment process, can form OSF.Following minority carrier life time scanning patter has reflected from the distribution situation of gap silicon atom in silicon single crystal rod, can form OSF in the subsequent process.
Below the preferred embodiment of the invention is specified, but the invention is not limited to described embodiment, those of ordinary skill in the art also can make all modification that is equal to or replacement under the prerequisite of the invention spirit, the modification that these are equal to or replacement all are included in the application's claim limited range.
Claims (8)
1. the method for the oxidation induced fault in the minority carrier life time scanning method test pulling of silicon single crystal is characterized in that, comprises the steps:
The first step intercepts test sample with band-sawing machine;
Second step corrodes described print surface damage layer with mixed acid solution, makes its surface be minute surface;
In the 3rd step, with cleansing solution described print is cleaned up;
The 4th step, described print is put into container, add again iodine solution, make described iodine solution be covered in uniformly described print surface;
The 5th step, the described print of handling well is scanned described print minority carrier life time with the minority carrier life time scanning device, measure the minority carrier life time distribution pattern.
2. the method for the oxidation induced fault in the minority carrier life time scanning method test pulling of silicon single crystal according to claim 1 is characterized in that the thickness of described print is 2 millimeters.
3. minority carrier life time scanning method according to claim 1 is tested the method for the oxidation induced fault in the pulling of silicon single crystal, it is characterized in that, described mixed acid solution is the mixed solution of nitric acid, acetic acid, hydrofluorite, and the volume ratio of nitric acid, acetic acid, hydrofluorite is 5: 3: 2 in the described mixed solution.
4. the method for the oxidation induced fault in the minority carrier life time scanning method test pulling of silicon single crystal according to claim 1 is characterized in that described surface damage layer erodes 200 microns.
5. the method for the oxidation induced fault in the minority carrier life time scanning method test pulling of silicon single crystal according to claim 1 is characterized in that described container is transparent plastic bag.
6. the method for the oxidation induced fault in the minority carrier life time scanning method test pulling of silicon single crystal according to claim 1 is characterized in that the described iodine solution of adding is 1 milliliter.
7. according to claim 1 or the method for the oxidation induced fault in the 6 described minority carrier life time scanning methods test pulling of silicon single crystal, it is characterized in that the mass percent concentration of described iodine solution is 1%～5%.
8. the method for the oxidation induced fault in the minority carrier life time scanning method test pulling of silicon single crystal according to claim 1 is characterized in that described cleansing solution is pure water.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108549003A (en) * | 2018-04-20 | 2018-09-18 | 江苏鑫华半导体材料科技有限公司 | A kind of preprocess method measuring semiconductor grade monocrystalline silicon minority carrier life time suitable for the high frequency method of photoconductivity decay measurement |
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| US5580828A (en) * | 1992-12-16 | 1996-12-03 | Semiconductor Physics Laboratory Rt | Method for chemical surface passivation for in-situ bulk lifetime measurement of silicon semiconductor material |
| CN101162694A (en) * | 2007-11-16 | 2008-04-16 | 中国科学院电工研究所 | Chemical passivation method for measuring minority carrier lifetime of crystalline silicon |
| CN101592469A (en) * | 2009-07-08 | 2009-12-02 | 中电电气（南京）光伏有限公司 | Silicon chip of solar cell damage layer thickness and minority carrier life time measuring method and device |
| CN101655427A (en) * | 2009-09-04 | 2010-02-24 | 中国电子科技集团公司第四十六研究所 | Dislocation corrosion detecting method of single germanium wafer |
| CN102021658A (en) * | 2010-12-10 | 2011-04-20 | 天津中环领先材料技术有限公司 | Heavily doped monocrystalline silicon wafer corrosion technique by alkali corrosion before acid corrosion |
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2011
- 2011-07-05 CN CN2011101860374A patent/CN102866335A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5580828A (en) * | 1992-12-16 | 1996-12-03 | Semiconductor Physics Laboratory Rt | Method for chemical surface passivation for in-situ bulk lifetime measurement of silicon semiconductor material |
| CN101162694A (en) * | 2007-11-16 | 2008-04-16 | 中国科学院电工研究所 | Chemical passivation method for measuring minority carrier lifetime of crystalline silicon |
| CN101592469A (en) * | 2009-07-08 | 2009-12-02 | 中电电气（南京）光伏有限公司 | Silicon chip of solar cell damage layer thickness and minority carrier life time measuring method and device |
| CN101655427A (en) * | 2009-09-04 | 2010-02-24 | 中国电子科技集团公司第四十六研究所 | Dislocation corrosion detecting method of single germanium wafer |
| CN102021658A (en) * | 2010-12-10 | 2011-04-20 | 天津中环领先材料技术有限公司 | Heavily doped monocrystalline silicon wafer corrosion technique by alkali corrosion before acid corrosion |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108549003A (en) * | 2018-04-20 | 2018-09-18 | 江苏鑫华半导体材料科技有限公司 | A kind of preprocess method measuring semiconductor grade monocrystalline silicon minority carrier life time suitable for the high frequency method of photoconductivity decay measurement |
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Application publication date: 20130109 |