CN104155302B - Method for detecting silicon crystal defects - Google Patents
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- CN104155302B CN104155302B CN201410314199.5A CN201410314199A CN104155302B CN 104155302 B CN104155302 B CN 104155302B CN 201410314199 A CN201410314199 A CN 201410314199A CN 104155302 B CN104155302 B CN 104155302B
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Abstract
The invention discloses a method for detecting silicon crystal defects. The method comprises the following steps: providing a test sample; immersing the test sample in first solution, and removing each layer on a polycrystalline silicon layer; immersing the test sample in second solution and removing the polycrystalline silicon layer, so that a silicon substrate is naked; immersing the test sample in third solution and etching the silicon crystal defects; and checking the silicon crystal defects on the test sample by using an optical microscope, and taking photos of the optical microscope. According to the method, the silicon substrate is naked, and the silicon crystal defects are effectively etched. Moreover, the method is simple and convenient to operate, rapid, high in efficiency, accurate in measurement result and high in repeatability.
Description
Technical field
The present invention relates to technical field of semiconductors, more particularly to a kind of method of detection silicon wafer volume defect.
Background technology
In semiconductor wafer disk manufactures, on substrate, silicon wafer volume defect directly influences the yield of wafer.So one
As failure analysis in chromic acid (WRIGHT) lithographic method be commonly used for the delineation of silicon wafer volume defect and analysis on wafer substrate, and with
The lattice of silicon wafer volume defect, crystalline phase, shapes and sizes are to judge the inducement of silicon wafer volume defect.
But to be succeeded He reproducible delineation result in actual failure analysis is but difficult to.At present, exist
During delamination, the stripping of polysilicon (Poly-Si) is highly difficult, and particularly wide layer polysilicon (Poly-Si), with Fluohydric acid. (HF)
It is difficult to thoroughly remove.
A kind of common traditional method is to be rubbed polysilicon (Poly-Si) with cotton stick while with HF acid solution delamination
Place helps remove, and also has and carrys out sticky removing polysilicon (Poly-Si) using blue mucosa.But these methods not only waste time and energy, Er Qienan
Remove polysilicon (Poly-Si) layer with thorough, and poor repeatability, directly influence the etching success of subsequent silicon wafer volume defect
Whether.
Content of the invention
It is an object of the invention to, a kind of method of detection silicon wafer volume defect is provided, effectively material is carried out to silicon chip
Layer lift-off processing, it is to avoid the illusion of artificial defect, improves accuracy and the repeatability of testing result.
The method of the detection silicon wafer volume defect that the present invention provides, for removing the material layer on wafer and to wafer silicon chip
Silicon wafer volume defect delineated and analyzed, described material layer includes covering many on the polysilicon layer of silicon chip and polysilicon layer
Plant film layer, the method includes：
Cut described wafer to obtain test sample；
Described test sample immersion the first solution is removed each layer on described polysilicon layer；
Described test sample immersion the second solution is removed described polysilicon layer so that silicon chip is naked；
By described test sample immersion the 3rd solution delineation silicon wafer volume defect；
With the silicon wafer volume defect in test sample described in light microscopy, and shoot optical microscope photograph.
Optionally, for the method for described detection silicon wafer volume defect, described first solution is Fluohydric acid., and concentration is
49%.
Optionally, for the method for described detection silicon wafer volume defect, when described test sample is soaked in the first solution
Between be 10min～15min.
Optionally, for the method for described detection silicon wafer volume defect, described second solution is nitric acid and buffer oxide
Etching solution volume ratio is 8:2 mixed liquor, the concentration of described nitric acid is 69.5%, and described buffer oxide etch liquid is volume ratio
For NH4F:HF=7:1 mixed liquor.
Optionally, for the method for described detection silicon wafer volume defect, when described test sample is soaked in the second solution
Between be 3s～10s.
Optionally, for the method for described detection silicon wafer volume defect, the formula of described 3rd solution is：
60 milliliters of concentration is 49% Fluohydric acid.；
30 milliliters of concentration is 69.5% nitric acid；
30 milliliters of concentration are the chromium trioxide solution of 5mol/L；
2 grams of [Cu (NO of copper nitrate containing water of crystallization3)2.3H2O]；
60 milliliters of concentration is 99.7% acetic acid；
60 ml deionized water.
Optionally, for the method for described detection silicon wafer volume defect, when described test sample is soaked in the 3rd solution
Between be 3min～5min.
Optionally, for the method for described detection silicon wafer volume defect, also include：Use scanning electron microscopy measurement silicon wafer
The shapes and sizes of volume defect, to judge the inducement of silicon wafer volume defect.
Optionally, for the method for described detection silicon wafer volume defect, molten in immersion the first solution, the second solution and the 3rd
After the completion of liquid, all utilize deionized water to clean test sample, then dried up with compressor gun.
Optionally, for the method for described detection silicon wafer volume defect, described test sample is silicon substrate wafer or cutting
Silicon substrate wafer afterwards.
Compared with prior art, in the method for detection silicon wafer volume defect that the present invention provides, using multiple solution soaking, go
Except other materials on silicon chip, particularly polysilicon.Compared to existing technology it is ensured that the naked and silicon crystal of silicon chip
Effective delineation of defect.The method of the present invention is easy and simple to handle, and quickly, efficiency high is it is possible to measure the silicon wafer in wide area
Volume defect, and measurement result is accurately and reproducible.Additionally, method of the present invention low cost, only use transmission electron microscope (TEM)
To measure 1/8th of silicon wafer volume defect method, the input of capital and the cost of sample fails analysis greatly reduce.
Brief description
The flow chart that Fig. 1 detects the method for silicon wafer volume defect for the embodiment of the present invention.
Specific embodiment
Method below in conjunction with the detection silicon wafer volume defect to the present invention for the schematic diagram is described in more detail, wherein table
Show the preferred embodiments of the present invention it should be appreciated that those skilled in the art can change invention described herein, and still
Realize the advantageous effects of the present invention.Therefore, description below be appreciated that widely known for those skilled in the art, and
It is not intended as limitation of the present invention.
In order to clear, whole features of practical embodiments are not described.In the following description, it is not described in detail known function
And structure, because they can make the present invention chaotic due to unnecessary details.It will be understood that opening in any practical embodiments
It is necessary to make a large amount of implementation details to realize the specific objective of developer in sending out, such as according to relevant system or relevant business
Limit, another embodiment is changed into by an embodiment.Additionally, it should think that this development is probably complicated and expends
Time, but it is only routine work to those skilled in the art.
Referring to the drawings the present invention more particularly described below by way of example in the following passage.Will according to following explanation and right
Seek book, advantages and features of the invention will become apparent from.It should be noted that, accompanying drawing is all in the form of very simplification and all using non-
Accurately ratio, only in order to purpose that is convenient, lucidly aiding in illustrating the embodiment of the present invention.
By research, inventor finds when applying WRIGHT etching liquid delineation silicon wafer volume defect, in order to obtain repeatability
Good delineation result, committed step is intended to set up the complete sample-pretreating method of set, is particularly using WRIGHT etching liquid
How all material of silicon substrate thoroughly to be peeled off before delineation silicon wafer volume defect, particularly polysilicon (Poly-
Si) it is ensured that silicon chip naked, thus avoiding peeling off clean and artificial defect that cause is false due to wafer upper substrate layer material
As it is ensured that obtaining accurate and reproducible delineation result.
Based on this thought, the method that the present invention provides following detection silicon wafer volume defect, refer to Fig. 1, this method bag
Include：
Step S101：Test sample is provided.Described test sample for model can be<100>、<111>Deng wafer：Bag
Include a silicon chip, described silicon chip is formed with polysilicon layer, described polysilicon layer is coated with multiple film layer.Real in the present invention
Apply in example, described test sample can be certain of a whole silicon substrate wafer or the silicon substrate wafer after being cut
A part.
Step S102：Described test sample immersion the first solution is removed each layer on described polysilicon layer.Preferably,
In the embodiment of the present invention, described first solution is Fluohydric acid. (HF), and concentration is 49%.In order to remove each layer on polysilicon layer,
Described test sample soak time in the first solution is 10min～15min, due to the film layer quantity of different samples and species not
With therefore soak time should flexibly change therewith.
Using the method for this step, can be good at removing each layer on polysilicon layer, thus many for high-quality removal
Crystal silicon layer lays the first stone.In order to obtain more preferable effect, when test sample is immersed in the first solution, need to be completely submerged,
And keep certain movement so that solution is had with test sample sufficiently contacts and chemical reaction, to improve delamination efficiency.
After the completion of this step, horse back deionized water (DI water) cleaning test sample, then in time with compression
Air cannon dries up.
Step S103：First solution soaks after terminating, described test sample immersion the second solution is removed described many
Crystal silicon layer is so that silicon chip is naked.Preferably, described second solution is HB82, specifically nitric acid (HNO3) and buffer oxide
Etching solution (BOE) volume ratio is 8:2 mixed liquor, the concentration of described nitric acid is 69.5%, and described BOE is NH for volume ratio4F:
HF=7:1 mixed liquor.The splitting time of polysilicon layer is 3s～10s, is preferred with 5s～8s, and that is, described test sample is second
In solution, soak time is 3s～10s, preferably 5s～8s, likewise, should also be as thickness regarding polysilicon layer and during to soaking
Between be finely adjusted, with thorough remove polysilicon it is ensured that silicon chip naked.
Likewise, when test sample is immersed in the second solution, needing to be completely submerged, and keep certain movement,
Solution is had with test sample sufficiently contact and chemical reaction, to improve delamination efficiency.
After the completion of this step, horse back deionized water (DI water) cleaning test sample, then in time with compression
Air cannon dries up.
Second solution used by this step is a key point of the present invention, using the second solution of configuration in this step, energy
Enough polysilicon layer is perfectly peeled off it is ensured that silicon chip is naked.Removal process in compared to existing technology, convenient reliability,
And there is good repeatability.
Step S104：By described test sample immersion the 3rd solution delineation silicon wafer volume defect.In the present embodiment, described
The formula of three solution is：
60 milliliters of concentration is 49% Fluohydric acid.；
30 milliliters of concentration is 69.5% nitric acid；
30 milliliters of concentration are the chromium trioxide solution of 5mol/L, contain 1 gram of CrO in 2ml solution3；
2 grams of [Cu (NO of copper nitrate containing water of crystallization3)2.3H2O]；
60 milliliters of concentration is 99.7% acetic acid；
60 ml deionized water (DI water).
The time that described test sample is immersed in the 3rd solution is 3min～5min, to complete to delineate silicon wafer volume defect.
Likewise, when test sample is immersed in the 3rd solution, needing to be completely submerged, and keep certain movement,
Solution is had with test sample sufficiently contact and chemical reaction.After the completion of this step, horse back deionized water (DI
Water) clean test sample, then dried up with compressor gun in time.
In above-mentioned several steps, immersion process is all to need once to complete, that is, be not available for for example by test sample from
Soak one in 3rd solution and take out observation after the meeting, be then immersed in again in the 3rd solution, to avoid the introducing of artificial defect illusion.
Step S105：With the silicon wafer volume defect in test sample described in light microscopy, and shoot optical microscope
Photo.Further, the shapes and sizes of scanning electron microscopy measurement silicon wafer volume defect can also be used again, to judge silicon crystal
The inducement of defect.For example, the inducement " spending " shape structure silicon wafer volume defect is likely due to be increased temperature process by contamination.
By the said method of the present invention, can amplify out：If only for silicon chip, the step that can directly carry out the present invention
S104, delineates silicon wafer volume defect with the 3rd solution.Utilize optical microscope and scanning electron microscopy measurement and analysis silicon afterwards
Crystal defect.
For the Silicon Wafer that do not complete, without polysilicon (Poly-Si) layer, then can skip step S103.
Obviously, those skilled in the art can carry out the various changes and modification essence without deviating from the present invention to the present invention
God and scope.So, if these modifications of the present invention and modification belong to the scope of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to comprise these changes and modification.
Claims (7)
1. a kind of method of detection silicon wafer volume defect, for removing the material layer on wafer and the silicon crystal of wafer silicon chip being lacked
It is trapped into row delineation and analyzes, described material layer includes covering the multiple film layers on the polysilicon layer of silicon chip and polysilicon layer, should
Method includes：
Test sample is provided；
Described test sample immersion the first solution is removed each layer on described polysilicon layer；
Described test sample immersion the second solution is removed described polysilicon layer so that silicon chip is naked；Described second solution is
Nitric acid and buffer oxide etch liquid volume ratio are 8:2 mixed liquor, the concentration of described nitric acid is 69.5%, described buffer oxide
Thing etching solution is NH for volume ratio4F:HF=7:1 mixed liquor, described test sample in the second solution soak time be 3s～
10s；
By described test sample immersion the 3rd solution delineation silicon wafer volume defect；
With the silicon wafer volume defect in test sample described in light microscopy, and shoot optical microscope photograph.
2. as claimed in claim 1 detection silicon wafer volume defect method it is characterised in that described first solution be Fluohydric acid.,
Concentration is 49%.
3. the method for detection silicon wafer volume defect as claimed in claim 2 is it is characterised in that described test sample is in the first solution
Middle soak time is 10min～15min.
4. the method for detection silicon wafer volume defect as claimed in claim 1 is it is characterised in that the formula of described 3rd solution is：
60 milliliters of concentration is 49% Fluohydric acid.；
30 milliliters of concentration is 69.5% nitric acid；
30 milliliters of concentration are the chromium trioxide solution of 5mol/L；
2 grams of Cu (NO of copper nitrate containing water of crystallization3)2·3H2O；
60 milliliters of concentration is 99.7% acetic acid；
60 ml deionized water.
5. the method for detection silicon wafer volume defect as claimed in claim 4 is it is characterised in that described test sample is in the 3rd solution
Middle soak time is 3min～5min.
6. the method for detection silicon wafer volume defect as claimed in claim 1 is it is characterised in that also include：Use scanning electron microscopy
Mirror measures the shapes and sizes of silicon wafer volume defect, to judge the inducement of silicon wafer volume defect.
7. the method for detection silicon wafer volume defect as claimed in claim 1 is it is characterised in that in immersion the first solution, second molten
After the completion of liquid and the 3rd solution, all utilize deionized water to clean test sample, then dried up with compressor gun.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN107316822A (en) * | 2017-06-26 | 2017-11-03 | 张兆民 | Silicon crystal defect inspection method |
| US11282695B2 (en) | 2017-09-26 | 2022-03-22 | Samsung Electronics Co., Ltd. | Systems and methods for wafer map analysis |
| CN109360793A (en) * | 2018-09-13 | 2019-02-19 | 胜科纳米（苏州）有限公司 | The rapid detection method of silicon wafer volume defect on semiconductor crystal wafer substrate |
| CN111220636A (en) * | 2020-01-15 | 2020-06-02 | 胜科纳米（苏州）有限公司 | Method for detecting silicon crystal defects in silicon substrate |
| CN113394126A (en) * | 2021-04-15 | 2021-09-14 | 上海新昇半导体科技有限公司 | Method for detecting defects in semiconductor material |
| CN114778537A (en) * | 2022-04-12 | 2022-07-22 | 胜科纳米(苏州)股份有限公司 | Method for identifying failure mechanism of transistor gate silicon oxide layer |
| CN114460432A (en) * | 2022-04-12 | 2022-05-10 | 胜科纳米(苏州)股份有限公司 | Comprehensive analysis method for failure of silicon oxide layer of grid electrode of transistor manufactured by semiconductor wafer |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101010805A (en) * | 2004-05-25 | 2007-08-01 | 株式会社上睦可 | Method of producing SIMOX substrate and the substrate produced thereby |
| CN101187065A (en) * | 2006-09-25 | 2008-05-28 | 株式会社Siltron | Method of identifying crystal defect region in monocrystalline silicon using metal contamination and heat treatment |
| CN101490314A (en) * | 2006-05-19 | 2009-07-22 | Memc电子材料有限公司 | Controlling agglomerated point defect and oxygen cluster formation induced by the lateral surface of a silicon single crystal during CZ growth |
| CN101996880A (en) * | 2009-08-14 | 2011-03-30 | 中芯国际集成电路制造(上海)有限公司 | Method for exposing semiconductor substrate and invalidation analysis method |
| CN102031557A (en) * | 2009-10-08 | 2011-04-27 | 硅电子股份公司 | Epitaxial wafer and production method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100880436B1 (en) * | 2008-02-05 | 2009-01-29 | 주식회사 실트론 | Test method of method of manufacturing silicon single crystal |
-
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- 2014-07-03 CN CN201410314199.5A patent/CN104155302B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101010805A (en) * | 2004-05-25 | 2007-08-01 | 株式会社上睦可 | Method of producing SIMOX substrate and the substrate produced thereby |
| CN101490314A (en) * | 2006-05-19 | 2009-07-22 | Memc电子材料有限公司 | Controlling agglomerated point defect and oxygen cluster formation induced by the lateral surface of a silicon single crystal during CZ growth |
| CN101187065A (en) * | 2006-09-25 | 2008-05-28 | 株式会社Siltron | Method of identifying crystal defect region in monocrystalline silicon using metal contamination and heat treatment |
| CN101996880A (en) * | 2009-08-14 | 2011-03-30 | 中芯国际集成电路制造(上海)有限公司 | Method for exposing semiconductor substrate and invalidation analysis method |
| CN102031557A (en) * | 2009-10-08 | 2011-04-27 | 硅电子股份公司 | Epitaxial wafer and production method thereof |
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Address after: Room 507, building 09, Northwest District, Suzhou nano City, No. 99, Jinjihu Avenue, Suzhou Industrial Park, China (Jiangsu) pilot Free Trade Zone, Suzhou, Jiangsu 215000 Patentee after: Shengke nano (Suzhou) Co.,Ltd. Address before: Room 507, building 09, northwest Suzhou nano City, 99 Jinjihu Avenue, Suzhou Industrial Park, Jiangsu Province, 215123 Patentee before: SHENGKE NANO (SUZHOU) Co.,Ltd. |