CN103236406B - A kind of method detecting polycrystalline silicon wafer dislocation density - Google Patents
A kind of method detecting polycrystalline silicon wafer dislocation density Download PDFInfo
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Abstract
The present invention relates to a kind of method detecting polycrystalline silicon wafer dislocation density, comprise the steps: 1. dislocation corrosion; 2. observe Corrosion results, calculate dislocation density, described dislocation corrosion is that the polysilicon chip of removing mechanical damage layer is immersed in K
2cr
2o
7dislocation corrosion is carried out in-HF mixed solution.The present invention is by adding K
2cr
2o
7, make corrosion reaction speed comparatively slow, can corrode the polysilicon chip of thinner thickness, can not there is surface oxidation in polysilicon chip after corrosion, is beneficial to display and the analysis of dislocation.
Description
Technical field
The present invention relates to a kind of method detecting polycrystalline silicon wafer dislocation density, be specifically related to a kind of method of corroding metallographic method detection polycrystalline silicon wafer dislocation density, belong to the dislocation detection field of polysilicon chip.
Background technology
Solar energy power generating utilizes one of form as most potential renewable resource, is achieving development at full speed in recent years, and prepares the developing direction that the cell piece with high light photoelectric transformation efficiency will become future.But in polycrystalline cast ingot process, for various reasons, the internal stress particularly under high temperature in silicon crystal makes to produce slippage between atomic plane, crystal face local produces plastic deformation, in crystal, define lattice defect---dislocation.
The intrinsic becoming metal impurities is assembled center by the dislocation in silicon crystal, becomes the complex centre of hole and electronics, causes the remarkable reduction of minority carrier life time (mean survival time of few son), thus causes the reduction of cell piece photoelectric conversion efficiency.Described few son and minority carrier are the concepts of Semiconductor Physics.
Therefore, the dislocation of silicon chip is shown, be conducive to the analysis of cell piece conversion efficiency, seem particularly important.At present, the display packing of dislocation has x-ray method, electron microscope method, copper decoration IR transmission method and corrosion metallographic method etc., and the most conventional is corrosion metallographic method.
The test philosophy of corrosion metallographic method is: in silicon crystal, the arrangement of its atom of place of dislocation is had to lose systematicness, structure comparison is loose, atom here has higher energy, and is subject to larger tension force, and being therefore easy to be corroded at dislocation line and surperficial intersection forms recessed hole, i.e. so-called etch pit, corrosion metallographic method utilizes this characteristic to show dislocation and fault exactly, is then observed by metallomicroscope, and passes through the density calculation dislocation density of etch pit in visual field.
In corrosion metallographic method, traditional etchant solution is HNO
3-HF mixed acid, i.e. HNO
3-HF mixed acid polysilicon chip dislocation corrosion method, its reaction speed is very fast, is unfavorable for the corrosion compared with thin silicon wafer, and is easily oxidized at silicon chip surface after corrosion, produces the oxide layer of black, is unfavorable for display and the analysis of dislocation.
Therefore, it is comparatively slow that this area needs to develop a kind of corrosion reaction, is convenient to silicon wafer thickness after control corrosion rate, and the corrosion metallographic method that is oxidized also can not occur silicon chip after corrosion.Described method also should reach after corroding polysilicon chip, clearly can see the microstructures such as the crystal grain of silicon chip surface, crystal boundary and twin, be convenient to the requirement of the distributional analysis of dislocation.
Summary of the invention
The invention provides a kind of method detecting polycrystalline silicon wafer dislocation density, fast, wayward in order to solve existing dislocation corrosion speed, oxidizable after corrosion, not easily observe, and be not suitable for the problem of the polysilicon chip of thinner thickness.
The present invention is achieved through the following technical solutions:
Detect a method for polycrystalline silicon wafer dislocation density, comprise the steps: 1. dislocation corrosion; 2. observe Corrosion results, calculate dislocation density; Wherein, described dislocation corrosion is that the polysilicon chip of removing mechanical damage layer is immersed in K
2cr
2o
7dislocation corrosion is carried out in-HF mixed solution.
The present invention adopts K
2cr
2o
7-HF mixed solution carries out dislocation corrosion to polysilicon chip, and reaction speed is comparatively slow, be convenient to corrode the polysilicon chip of thinner thickness, and silicon chip can not be oxidized after corrosion; Meanwhile, after adopting this mixed solution to corrode polysilicon chip, clearly can see the microstructures such as the crystal grain of silicon chip surface, crystal boundary and twin, be convenient to the distributional analysis of dislocation.The present invention adds and has comparatively weak oxide material K
2cr
2o
7, reduce the speed of corrosion reaction, achieve the object can corroded the polysilicon chip of thinner thickness.
K of the present invention
2cr
2o
7in-HF mixed solution, K
2cr
2o
7be 1:1 ~ 1:4.5, such as 1:1.1,1:1.3,1:1.5,1:1.9,1:2.4,1:2.8,1:3.2,1:3.5,1:3.7,1:3.9,1:4.3 etc. with the mass ratio of HF acid.Mass ratio is greater than 1:1, and the addition of HF acid is few, and dislocation corrosion is not thorough, effectively cannot reflect dislocation density; Mass ratio is less than 1:4.5, K
2cr
2o
7addition few, corrosion reaction speed, is unfavorable for corroding thinner polysilicon chip.
As optimal technical scheme, K of the present invention
2cr
2o
7-HF mixed solution is the K of 1:1 ~ 1:4 by volume ratio
2cr
2o
7solution and HF solution mix, and volume ratio can be 1:1.1,1:1.3,1:1.5,1:1.9,1:2.4,1:2.8,1:3.2,1:3.5,1:3.7,1:3.9 etc.;
Described K
2cr
2o
7solution is K
2cr
2o
7the aqueous solution, described K
2cr
2o
7the concentration of solution is 0.1 ~ 0.2mol/L, such as 0.11mol/L, 0.13mol/L, 0.14mol/L, 0.16mol/L, 0.18mol/L, 0.19mol/L etc., preferred 0.15mol/L;
Described HF acid solution is HF aqueous acid, described HF acid solutions is 45 ~ 55wt%, such as 45.2wt%, 45.8wt%, 43wt%, 43.5wt%, 44.1wt%, 44.6wt%, 45.6wt%, 46.3wt%, 48wt%, 49.3wt%, 50.5wt%, 52wt%, 53.6wt%, 54.1wt%, 54.8wt% etc., preferred 49wt%.
Preferably, polysilicon chip of the present invention is at K
2cr
2o
7soak time in-HF mixed solution is 7 ~ 10min, such as 7.1min, 7.6min, 8min, 8.4min, 8.9min, 9.3min, 9.6min etc.
As optimal technical scheme, dislocation corrosion of the present invention comprises the steps:
(1) polysilicon chip is cleaned;
(2) H is immersed in
2crO
4in-HF mixed acid, removing mechanical damage layer;
(3) the remaining acid solution on polysilicon chip surface is removed;
(4) polysilicon chip is immersed in K
2cr
2o
7dislocation corrosion is carried out in-HF mixed solution;
(5) remove the residual solution on polysilicon chip surface, and dry.
The present invention passes through H
2crO
4in-HF mixed acid, the mechanical damage layer of silicon chip surface is removed in reaction, makes the microstructure naked eyes such as the crystal grain of silicon chip surface, crystal boundary and twin high-visible.
Preferably, H of the present invention
2cr
2o
7in-HF mixed acid, H
2cr
2o
7acid is 1:1 ~ 1:4.5, such as 1:1.1,1:1.3,1:1.5,1:1.9,1:2.4,1:2.8,1:3.2,1:3.5,1:3.7,1:3.9,1:4.3 etc. with the mass ratio of HF acid, preferred 1:1.3 ~ 1:4.2.
As optimal technical scheme, H of the present invention
2cr
2o
7-HF mixed acid is the H of 1:1 ~ 3:1 by volume ratio
2cr
2o
7acid solution and HF acid solution mix, and volume ratio can be 1:1,1.1:1,1.3:1,1.9:1,2.2:1,2.5:1,2.8:1 etc.;
Described H
2cr
2o
7acid solution is by CrO
3powder and water formulated, described H
2cr
2o
7the concentration of acid solution is 0.8 ~ 1.2mol/L, such as 0.81mol/L, 0.83mol/L, 0.94mol/L, 0.96mol/L, 1.04mol/L, 1.09mol/L, 1.13mol/L, 1.17mol/L etc., preferred 1mol/L;
Described HF acid solution is HF aqueous acid, described HF acid solutions is 45 ~ 55wt%, such as 45.2wt%, 45.8wt%, 43wt%, 43.5wt%, 44.1wt%, 44.6wt%, 45.6wt%, 46.3wt%, 48wt%, 49.3wt%, 50.5wt%, 52wt%, 53.6wt%, 54.1wt%, 54.8wt% etc., preferred 49wt%.
Preferably, described polysilicon chip is at H
2cr
2o
7soak time in-HF mixed acid is 40-80s, such as 41s, 43s, 47s, 52s, 56s, 62s, 68s, 71s, 79s etc.
As most preferred technical scheme, dislocation corrosion of the present invention comprises the steps:
(1) polysilicon chip of well cutting is cleaned;
(2) polysilicon chip of cleaning is passed through at H
2crO
4in-HF mixed acid, the mechanical damage layer of silicon chip surface is removed in reaction;
Wherein, H
2crO
4acid is by analytically pure CrO
3powder and pure water are mixed with the solution that concentration is 1mol/L, and HF acid concentration is 49%; Two kinds of sour volume ratios are H
2crO
4: HF=1:1 ~ 3:1, reaction time 40 ~ 80s;
(3) will with H
2crO
4the reacted polysilicon chip of-HF mixed acid soaks in deionized water, and the remaining acid solution on polysilicon chip surface is rinsed well;
(4) polysilicon chip after rinsing is soaked into K
2cr
2o
7dislocation corrosion is carried out in-HF mixed solution;
Wherein, K
2cr
2o
7solution is by analytically pure K
2cr
2o
7powder and pure water are mixed with the solution that concentration is 0.15mol/L, and HF concentration is 49%; The volume ratio of two kinds of solution is K
2cr
2o
7: HF=1:1 ~ 1:4, reaction time 7 ~ 10min;
And K (5)
2cr
2o
7the polysilicon chip that-HF mixed solution corrodes soaks in deionized water, the residual solution on polysilicon chip surface is rinsed well, puts into oven for drying subsequently.
The present invention carries out the dislocation observation of metallomicroscope after dislocation corrosion, the calculating of line position of going forward side by side dislocation density, and described dislocation observation and calculating are the ordinary skill in the art, repeat no more herein, and (unit is number/cm to typical but non-limiting dislocation density
2) computing formula be:
N
D=n/s
Wherein, N
dfor dislocation density; N is the number being observed etch pit on face; S is the area being observed face.
Because the defect shape of polysilicon is different, defect of polysilicon comprises dislocation and fault, dislocation is the line defect in crystal, fault is planar defect, therefore, those skilled in the art should understand, detection method of the present invention detects based on the corrosion of the defect to polysilicon dislocation (or fault), corrosion principle is identical, and therefore the detection of dislocation and fault two kinds of defects all can use method provided by the invention.
Compared with prior art, the present invention has following beneficial effect:
(1) the present invention is by the adjustment of silicon slice corrosion acid fluid system material and the optimization of sour ratio, especially adds and has comparatively weak oxide material K
2cr
2o
7make corrosion reaction speed slower, can corrode the silicon chip of thinner thickness, such as the present invention is that the polysilicon chip being greater than 50 μm all can process to thickness, and the polysilicon chip that can be such as 60 μm, 80 μm, 100 μm, 120 μm, 150 μm, 200 μm, 230 μm for thickness processes;
(2) the present invention first processes the mechanical damage layer on polysilicon chip surface, makes the microstructure naked eyes such as the crystal grain of silicon chip surface, crystal boundary and twin high-visible, is convenient to the distribution of dislocation;
(3) the present invention adopts K
2cr
2o
7-HF mixed solution carries out dislocation corrosion, and reaction speed is comparatively slow, be convenient to corrode the polysilicon chip of thinner thickness, and silicon chip surface oxidation can not occur after corrosion, be beneficial to display and the analysis of dislocation.
Accompanying drawing explanation
Fig. 1 is the surface picture of the polysilicon chip removing surperficial mechanical damage layer;
Fig. 2 is the surface picture of the polysilicon chip after dislocation corrosion.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand, described embodiment is only help to understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment 1
Detect a method for polycrystalline silicon wafer dislocation density, comprise step 1. dislocation corrosion; 2. observe Corrosion results, calculate dislocation density; Wherein, dislocation corrosion comprises the steps:
(1) by well cutting, thickness is that the polysilicon chip of 200 μm cleans;
(2) polysilicon chip of cleaning is passed through at H
2crO
4in-HF mixed acid, the mechanical damage layer of silicon chip surface is removed in reaction; Fig. 1 is the surface picture of the polysilicon chip removing surperficial mechanical damage layer;
Wherein, H
2crO
4acid is by analytically pure CrO
3powder and pure water are mixed with the solution that concentration is 1mol/L, and HF acid concentration is 49%; Two kinds of sour volume ratios are H
2crO
4: HF=1:1 ~ 3:1, reaction time 40 ~ 80s;
(3) will with H
2crO
4the completely reacted polysilicon chip of-HF mixed acid soaks in deionized water, and the remaining acid solution on polysilicon chip surface is rinsed well;
(4) polysilicon chip after rinsing is soaked into K
2cr
2o
7dislocation corrosion is carried out in-HF mixed solution;
Wherein, K
2cr
2o
7solution is by analytically pure K
2cr
2o
7powder and pure water are mixed with the solution that concentration is 0.15mol/L, and HF concentration is 49%; The volume ratio of two kinds of solution is K
2cr
2o
7: HF=1:1 ~ 1:4, reaction time 7 ~ 10min;
And K (5)
2cr
2o
7the polysilicon chip that-HF mixed solution corrodes soaks in deionized water, the residual solution on polysilicon chip surface is rinsed well, puts into oven for drying subsequently; Fig. 2 is the surface picture of the polysilicon chip after dislocation corrosion.
As illustrated in fig. 1 and 2, after polysilicon chip is corroded, clearly can see the microstructures such as the crystal grain on polysilicon chip surface, crystal boundary and twin, and dislocation aggregation zone presents black fuse pattern.
Choose the diverse location of the polysilicon chip after dislocation corrosion, by metallography microscope sem observation, and read the dislocation number in visual field, average, divided by visual field area, namely obtain dislocation density;
As calculated, the dislocation density of polysilicon chip that embodiment 1 is chosen is 100cm
-2.
Embodiment 2
Detect a method for polycrystalline silicon wafer dislocation density, comprise step 1. dislocation corrosion; 2. observe Corrosion results, calculate dislocation density; Wherein, dislocation corrosion comprises the steps:
(1) by well cutting, thickness is that the polysilicon chip of 160 μm cleans;
(2) polysilicon chip of cleaning is passed through at H
2crO
4in the mixed acid of-HF, the mechanical damage layer of silicon chip surface is removed in reaction; Wherein, H
2crO
4acid is 1:1 with the mass ratio of HF acid; Reaction time 80s;
(3) will with H
2crO
4the reacted polysilicon chip of-HF mixed acid soaks in deionized water, and the remaining acid solution on polysilicon chip surface is rinsed well;
(4) polysilicon chip after rinsing is soaked into K
2cr
2o
7dislocation corrosion is carried out in-HF mixed solution; Wherein, K in mixed solution
2cr
2o
7be 1:4.5 with the mass ratio of HF acid, reaction time 7min;
And K (5)
2cr
2o
7the polysilicon chip that-HF mixed solution corrodes soaks in deionized water, the residual solution on polysilicon chip surface is rinsed well, puts into oven for drying subsequently;
The distribution of dislocation is identical with embodiment 1 with density calculation.
Embodiment 3
Detect a method for polycrystalline silicon wafer dislocation density, comprise step 1. dislocation corrosion; 2. observe Corrosion results, calculate dislocation density; Wherein, dislocation corrosion comprises the steps:
(1) by well cutting, thickness is that the polysilicon chip of 80 μm cleans;
(2) polysilicon chip of cleaning is passed through at H
2crO
4in the mixed acid of-HF, the mechanical damage layer of silicon chip surface is removed in reaction; Wherein, H
2crO
4acid is 1:4.5 with the mass ratio of HF acid; Reaction time 40s;
(3) will with H
2crO
4the reacted polysilicon chip of-HF mixed acid soaks in deionized water, and the remaining acid solution on polysilicon chip surface is rinsed well;
(4) polysilicon chip after rinsing is soaked into K
2cr
2o
7dislocation corrosion is carried out in-HF mixed solution; Wherein, K in mixed solution
2cr
2o
7be 1:1 with the mass ratio of HF, reaction time 10min;
And K (5)
2cr
2o
7the polysilicon chip that-HF mixed solution corrodes soaks in deionized water, the residual solution on polysilicon chip surface is rinsed well, puts into oven for drying subsequently;
The distribution of dislocation is identical with embodiment 1 with density calculation.
Comparative example
Select HNO
3-HF mixed acid polysilicon chip dislocation corrosion method, carry out dislocation corrosion to the polysilicon chip that thickness is 200 μm, etchant solution is the HNO of volume ratio 1:18
3with HF mixed acid, after 10s, silicon chip central reaction penetrates.
Applicant states, the present invention illustrates DCO flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed testing process, does not namely mean that the present invention must rely on above-mentioned DCO flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of auxiliary element, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (1)
1. detect a method for polycrystalline silicon wafer dislocation density, it is characterized in that, its dislocation corrosion is following steps:
(1) polysilicon chip of well cutting is cleaned;
(2) polysilicon chip of cleaning is passed through at H
2crO
4in-HF mixed acid, the mechanical damage layer of silicon chip surface is removed in reaction;
Wherein, H
2crO
4acid is by analytically pure CrO
3powder and pure water are mixed with the solution that concentration is 1mol/L, and HF acid concentration is 49wt%; Two kinds of sour volume ratios are H
2crO
4: HF=1:1 ~ 3:1, reaction time 40 ~ 80s;
(3) will with H
2crO
4the reacted polysilicon chip of-HF mixed acid soaks in deionized water, and the remaining acid solution on polysilicon chip surface is rinsed well;
(4) polysilicon chip after rinsing is soaked into K
2cr
2o
7dislocation corrosion is carried out in-HF mixed solution;
Wherein, K
2cr
2o
7solution is by analytically pure K
2cr
2o
7powder and pure water are mixed with the solution that concentration is 0.16 ~ 0.2mol/L, and HF concentration is 49wt%; The volume ratio of two kinds of solution is K
2cr
2o
7: HF=1:2.4 ~ 1:4, reaction time 8 ~ 10min;
And K (5)
2cr
2o
7the polysilicon chip that-HF mixed solution corrodes soaks in deionized water, the residual solution on polysilicon chip surface is rinsed well, puts into oven for drying subsequently.
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| CN104900758B (en) * | 2015-05-25 | 2017-03-15 | 连云港市产品质量监督检验中心 | A kind of detection method of quasi-monocrystalline silicon microdefect |
| CN108364888A (en) * | 2018-02-11 | 2018-08-03 | 武汉华星光电半导体显示技术有限公司 | Detection device |
| CN110849875A (en) * | 2019-10-10 | 2020-02-28 | 新余学院 | Method for analyzing microstructure of cast polycrystalline silicon |
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| CN101220477A (en) * | 2008-01-30 | 2008-07-16 | 中国科学院上海技术物理研究所 | Corrosive agent and corrosion method for II-VI family semiconductor material line defect display |
| CN102607916A (en) * | 2012-03-12 | 2012-07-25 | 苏州协鑫工业应用研究院有限公司 | Preparation method of silicon chip metallographic specimen |
| CN102768134A (en) * | 2012-07-20 | 2012-11-07 | 浙江大学 | Method for displaying and detecting void type defects in Czochralski silicon wafer |
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| JP3439332B2 (en) * | 1997-10-24 | 2003-08-25 | Ｎｅｃエレクトロニクス株式会社 | How to measure crystal defects |
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| CN101220477A (en) * | 2008-01-30 | 2008-07-16 | 中国科学院上海技术物理研究所 | Corrosive agent and corrosion method for II-VI family semiconductor material line defect display |
| CN102607916A (en) * | 2012-03-12 | 2012-07-25 | 苏州协鑫工业应用研究院有限公司 | Preparation method of silicon chip metallographic specimen |
| CN102768134A (en) * | 2012-07-20 | 2012-11-07 | 浙江大学 | Method for displaying and detecting void type defects in Czochralski silicon wafer |
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