CN109781654A - The detection method that silicon chip surface stains - Google Patents
The detection method that silicon chip surface stains Download PDFInfo
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- CN109781654A CN109781654A CN201910183016.3A CN201910183016A CN109781654A CN 109781654 A CN109781654 A CN 109781654A CN 201910183016 A CN201910183016 A CN 201910183016A CN 109781654 A CN109781654 A CN 109781654A
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Abstract
The present invention relates to the detection methods that a kind of silicon chip surface stains comprising following steps: carrying out constituent analysis to the contaminated area and is formed with the element of pollutant in the determination contaminated area；The infrared spectroscopy of the contaminated area is compared the infrared spectroscopy for acquiring the contaminated area with the infrared spectroscopy in standard sample library.Which kind of substance is the detection method that above-mentioned silicon chip surface stains can be specially with the pollutant of comprehensive descision silicon chip surface contaminated area, compared in conjunction with the element composition of pollutant and the infrared spectroscopy of Polluted area of silicon chip surface contaminated area with standard diagram, the two comprehensive dimensions can qualitatively judge the exact ingredient of the pollutant of silicon chip surface contaminated area, and then have great significance for judgement contamination source, investigation contamination cause.
Description
Technical field
The present invention relates to silicon wafers to stain detection field, the detection method stain more particularly to a kind of silicon chip surface.
Background technique
As the technology of photovoltaic industry constantly upgrades, the processing procedure standard of crystal silicon solar batteries is proposed tightened up
It is required that.The superiority and inferiority of main body of the silicon wafer as crystal silicon solar batteries, quality has vital influence to photovoltaic module.
Silicon chip surface contamination is most common one of bad in silicon wafer production process, is usually denier since silicon wafer stains
, and form of poluttants is different, complicated component, is difficult to be which kind of substance by the pollutant of micro-judgment silicon chip surface.It passes
The component analyzing method of the silicon chip surface pollutant of system mainly has Secondary Ion Mass Spectrometry, inductively coupled plasma mass spectrometry and complete
Reflection X-ray fluorescence method, but the above method can only analyze the element composition information of pollutant on silicon chip surface, still cannot
Determine which kind of substance pollutant is, i.e., the pollutant of silicon chip surface can not be carried out qualitative.
Summary of the invention
Based on this, it is necessary to aiming at the problem which kind of substance the pollutant that can not determine silicon chip surface contaminated area be, mention
The pollutant that silicon chip surface contaminated area can be determined for one kind is the detection method of the silicon chip surface contamination of which kind of substance.
A kind of detection method that silicon chip surface stains, which comprises the steps of:
Constituent analysis is carried out to the contaminated area to form with the element of pollutant in the determination contaminated area；
The infrared spectroscopy for acquiring the contaminated area, by the infrared light of the infrared spectroscopy of the contaminated area and standard sample
Spectrum is compared.
The detection method that above-mentioned silicon chip surface stains can be specially with the pollutant of comprehensive descision silicon chip surface contaminated area
Which kind of substance, the i.e. element in conjunction with the pollutant of silicon chip surface contaminated area form and the infrared spectroscopy and standard of Polluted area
The comparison of map, the two comprehensive dimensions can qualitatively judge the exact ingredient of the pollutant of silicon chip surface contaminated area, in turn
Source is stain for judgement, investigation contamination cause has great significance.In addition, the detection method stain of above-mentioned silicon chip surface without
Complicated pretreatment procedure need to be carried out to silicon chip surface, and will not damage silicon wafer.
Constituent analysis is being carried out to the contaminated area with dirty in the determination contaminated area in one of the embodiments,
It further include scanning the contaminated area of silicon chip surface to obtain the microcosmic of the contaminated area before the step of contaminating the element composition of object
The step of pattern.
The microcosmic shape of the contaminated area is obtained in the contaminated area of scanning silicon chip surface in one of the embodiments,
It is the contaminated area using scanning of scanning electron microscope silicon chip surface in the step of looks.
Amplification factor is 500 when contaminated area described in the scanning of scanning electron microscope in one of the embodiments,
- 2000 times again.
Beam voltage when contaminated area described in the scanning of scanning electron microscope in one of the embodiments,
For 0.1kV-20kV.
Constituent analysis is being carried out to the contaminated area with dirty in the determination contaminated area in one of the embodiments,
It further include the contaminated area using infrared detection silicon chip surface to determine silicon chip surface before the step of contaminating the element composition of object
The step of.
It in one of the embodiments, in the step of acquiring the infrared spectroscopy of the contaminated area, is stained with described in acquisition
The micro ft-ir spectroscopy in dirty region.
In one of the embodiments, in the step of acquiring the micro ft-ir spectroscopy of the contaminated area, acquisition is differentiated
Rate is 1cm-1-4cm-1。
In one of the embodiments, in the step of acquiring the micro ft-ir spectroscopy of the contaminated area, spectrogram scanning
Number is 16 times -256 times.
In one of the embodiments, in the step of acquiring the micro ft-ir spectroscopy of the contaminated area, diaphragm is acquired
Region is 100 μm -500 of 100 μ m, 500 μm of μ m.
Detailed description of the invention
Fig. 1 is the microscopic appearance figure of the scanning of scanning electron microscope of the contaminated area of monocrystalline silicon sheet surface；
Fig. 2 is the X-ray energy spectrogram of the contaminated area of monocrystalline silicon sheet surface；
Fig. 3 is that the pollutant of monocrystalline silicon sheet surface contaminated area is the micro ft-ir spectroscopy of silicone oil and the silicone oil of master sample
The comparison chart of infrared spectroscopy；
Fig. 4 is that the pollutant of monocrystalline silicon sheet surface contaminated area is the micro ft-ir spectroscopy and standard sample of one-component glue
The bright pink external spectrum of single-component glue comparison chart.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing to the present invention
Specific embodiment be described in detail.Many details are explained in the following description in order to fully understand this hair
It is bright.But the invention can be embodied in many other ways as described herein, those skilled in the art can be not
Similar improvement is done in the case where violating intension of the present invention, therefore the present invention is not limited by the specific embodiments disclosed below.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term " and or " used herein includes one or more phases
Any and all combinations of the listed item of pass.
One embodiment of the invention provides a kind of detection method that silicon chip surface stains comprising following steps:
S1, the contaminated area of silicon chip surface is scanned to obtain the microscopic appearance of silicon chip surface contaminated area.
Silicon wafer type does not do excessive restriction in the present invention, can be monocrystalline silicon piece, polysilicon chip or quasi-monocrystalline silicon.
The thickness for the silicon slice under test sample selected in one of the embodiments, is no more than 0.2mm, silicon slice under test sample
Thickness, which is no more than 0.2mm, can reduce absorption of the silicon wafer substrate to infrared light, reduce interference of the silicon wafer substrate to detection is stain.
Scan the concrete operation step of the contaminated area of silicon chip surface are as follows: take surface contamination to have the silicon wafer of pollutant, later
The enlarged drawing for obtaining the microscopic appearance of silicon chip surface contaminated area is scanned to it, operator's preliminary observation contaminated area
Microscopic appearance can tentatively judge the substantially type of pollutant, such as: tentatively judge that pollutant is organic matter or inorganic matter, is solid
Body particle or the drop of ambiguity etc..
The contaminated area for scanning silicon chip surface in one of the embodiments, is using scanning of scanning electron microscope silicon wafer
The contaminated area on surface.Scanning electron microscope is scanned on sample using focused high-energy electron beam, to inspire
Various physical messages are imaged by the receiving of these information, amplification and display, obtain test sample micromorphology.Electronics
Micro- scarnning mirror has many advantages, such as that amplification factor height, the depth of field, the visual field is big, imaging volume sense is strong, sample pre-treatment is simple.
It can use scanning electron microscope in one of the embodiments, and determine on silicon chip surface that naked eyes can not distinguish
Contaminated area specifically carries out array scanning to entire silicon chip surface using scanning electron microscope and obtains silicon chip surface difference
The microscopic appearance picture in region judges silicon chip surface with the presence or absence of contaminated area by microcosmic pattern picture.
The contaminated area of scanning of scanning electron microscope silicon chip surface is aobvious in scanning electron in one of the embodiments,
It is carried out in the sample bin of micro mirror, vacuumize process is carried out to the sample bin of scanning electron microscope, foreign gas is discharged, control is swept
The vacuum degree for retouching the sample bin of electron microscope is 5.0 × 10-5Mbar controls the main of vacuum degree hereinafter, discharge foreign gas
Reason has following two aspects:
(1) if there are gases in the electron gun of scanning electron microscope, it is gentle that electric discharge can be generated when electron gun adds high pressure
Volume ionization keeps the electronic beam current of transmitting unstable, can adversely affect to the microscopic appearance for obtaining contaminated area.
(2) such as remaining oxygen and steam, it can be chemically reacted with the tungsten cathode for being heated to incandescent lamp state, make tungsten wire
Occur to corrode and burn.Furthermore as made silicon chip surface cause secondary dirt in residual impurity gas content to silicon slice under test surface
Dye.
The amplification factor during the scanning of scanning electron microscope is 500 times -2000 in one of the embodiments,
Times.Within the scope of this amplification factor, the microscopic appearance image of the contaminated area for the silicon chip surface being more clear can get.
The beam voltage during the scanning of scanning electron microscope is set as in one of the embodiments,
0.1kV-20kV.Further, the beam voltage during the scanning of scanning electron microscope is set as 0.1kV-
10kV。
It further include using infrared detection silicon chip surface to obtain silicon in one of the embodiments, before step S1
The contaminated area on piece surface.Specifically, infrared ray is carried out to silicon chip surface to be detected using the sorter with infrared ray instrument
Scanning, infrared ray instrument have infrared ray transmitting terminal and infrared receiver end, when silicon chip surface is there are when pollutant, infrared receiver
The signal receiving strength at end dies down, so that it may judge that there are pollutants in the region, it can determine the contaminated area of silicon chip surface.
Further, the detection frequency of the infrared ray is 400cm-1-4000cm-1。
It is appreciated that the detection method that silicon chip surface of the invention stains can not execute step S1, i.e., do not execute scanning
The step of microscopic appearance of the contaminated area of silicon chip surface to obtain silicon chip surface contaminated area, only with following steps S2 and step
Rapid S3.
S2, contaminated area progress constituent analysis is formed with the element of pollutant in the determination contaminated area.
The mistake that constituent analysis is formed with the element of pollutant in the determination contaminated area is being carried out to the contaminated area
The method of Cheng Zhong, constituent analysis are unlimited, i.e. selection those skilled in the art are regarded to determine pollutant in the contaminated area
Element composition analysis method, such as: X-ray energy spectrum analytic approach, total reflection X ray fluorescence method, inductive coupling etc. from
Daughter mass spectrography etc..
The present invention selects the scanning electron microscope for being furnished with X-ray energy spectrum analyzer in one of the embodiments, in this way
Observation and the Microanalysis of contaminated area microscopic appearance can be carried out simultaneously, and then determine pollutant in the contaminated area
Element composition.
It further include using infrared detection silicon chip surface to obtain silicon in one of the embodiments, before step S2
The contaminated area on piece surface.Specifically, infrared ray is carried out to silicon chip surface to be detected using the sorter with infrared ray instrument
Scanning, infrared ray instrument have infrared ray transmitting terminal and infrared receiver end, when silicon chip surface is there are when pollutant, infrared receiver
The signal receiving strength at end dies down, so that it may judge that there are pollutants in the region, it can determine the contaminated area of silicon chip surface.
Further, the detection frequency of the infrared ray is 400cm-1-4000cm-1。
S3, the acquisition contaminated area infrared spectroscopy, by the red of the infrared spectroscopy of the contaminated area and standard sample
External spectrum is compared.
Infrared spectrum technology belongs to molecular spectrum field, and infrared spectrum technology can determine molecular composition and structure.According to
The intensity, location and shape of absorption peak in unknown material infrared spectroscopy, so that it may determine in the unknown material molecule include which base
Group, to infer the structure of the unknown material.The advantages of Infrared Spectrum Technology is that high sensitivity, wave number are accurate, reproducible.
It in one of the embodiments, in the step of acquiring the infrared spectroscopy of the contaminated area, is stained with described in acquisition
The micro ft-ir spectroscopy in dirty region, specifically, acquiring the infrared microscopy light of the contaminated area using micro ft-ir spectroscopy instrument
Spectrum.Infrared microscopy technology is to combine infrared spectrum technology with microscopy, integrating microscope technology and infrared light
The advantage of spectral technology focuses on light beam accurately in the small area of sample, to realize that measurement microsize sample is red
The purpose of external spectrum.For common infrared spectroscopy, infrared microscopy technology sensitivity, resolution ratio and measurement accuracy
It is significantly increased, is more advantageous to and judges in unknown material molecule comprising which group.
The detection method that silicon chip surface of the invention stains in one of the embodiments, is by scanning electron microscope skill
Art utilizes the scanning of scanning electron microscope silicon chip surface with X-ray energy spectrometer in conjunction with infrared microscopy technology
Contaminated area is formed with the microscopic appearance and element that obtain the contaminated area, and the micro ft-ir spectroscopy for acquiring contaminated area determines
Pollutant component information, the two be combined with each other, and complete the pollutant qualitative work of silicon chip surface contaminated area, and judgement is stain
Source, investigation contamination cause have great significance.Such as: silicon chip surface contaminated area is that the mixing that silicon powder and glue form is dirty
Contaminate object.Because of the interference of substrate silicon wafer, it may determine that with infrared microscopy technology and contain glue in mixed pollutants, but be difficult
Silicon powder is qualitatively judged, the microscopic appearance the at this moment scanning of scanning electron microscope with X-ray energy spectrometer being combined to obtain
And element composition, it can judge that another substance is silicon powder in mixed pollutants.And then Instructing manufacture personnel are being readily incorporated
It is strictly managed in the process of both pollutants, avoids introducing silicon powder and glue.The pollution of silicon chip surface contaminated area for another example
Object is carbonate, and sodium carbonate, the micro ft-ir spectroscopy structure of calcium carbonate are similar, it is also difficult to carry out it is qualitative, at this moment combine contaminated area
Which kind of carbonate microscopic appearance and the element composition in domain can also be determined as.
It is acquired in the micro ft-ir spectroscopy step of the contaminated area in one of the embodiments, micro ft-ir spectroscopy
Acquisition resolution be 1cm-1-4cm-1.Under acquisition resolution within the scope of this this, silicon chip surface contaminated area it is micro- red
The peak shape of the absorption peak of external spectrum is more preferable.
It is acquired in the micro ft-ir spectroscopy step of the contaminated area in one of the embodiments, micro ft-ir spectroscopy
Map scanning times be 16 times -256 times.Within the scope of this under spectrogram scanning times, noise is excellent and testing efficiency is high, further
Ground, the spectrogram scanning times of the micro ft-ir spectroscopy are 64 times -128 times.
It is acquired in the micro ft-ir spectroscopy step of the contaminated area in one of the embodiments, micro ft-ir spectroscopy
Acquisition diaphragm region be 100 μm -500 of 100 μ m, 500 μm of μ m.Benefit is the microcosmic object of both available high-resolutions
Matter distribution can guarantee that sample has enough signal strengths again, it is ensured that the accuracy of test.Further, micro ft-ir spectroscopy
Acquisition diaphragm region is 250 μm -350 of 250 μ m, 350 μm of μ m.
It is acquired in the micro ft-ir spectroscopy step of the contaminated area in one of the embodiments, the infrared microscopy
The acquisition mode of spectrum is transmission mode.Transmission mode can obtain the stronger absorption signal in silicon chip surface contaminated area, improve
Test accuracy.Of course it is to be understood that the acquisition mode of the micro ft-ir spectroscopy is not limited only to projection mode, it can also be anti-
Emission mode or ATR mode.
It is appreciated that the microscopic appearance that the detection method that silicon chip surface of the invention stains can not execute step S1 obtains
It takes, only with step S2 and step S3.It is also to be understood that step S1, S2 of the detection method that silicon chip surface of the present invention stains and
S3 is not that the sequencing for the detection method stain to silicon chip surface is defined, and is intended merely to the one kind for facilitating discussion to provide
Example.That is, step S1, S2 and S3 sequence for the detection method that silicon chip surface of the invention stains can be interchanged, such as
The step of detection method that silicon chip surface of the invention stains, is successively are as follows: S2, carries out constituent analysis to the contaminated area with true
The element composition of pollutant in the fixed contaminated area.S1, the contaminated area of silicon chip surface is scanned to obtain the contaminated area
Microscopic appearance.S3, the infrared spectroscopy for acquiring the contaminated area, by the infrared spectroscopy of the contaminated area and standard sample library
Infrared spectroscopy be compared.
The detection method that above-mentioned silicon chip surface stains can be specially with the pollutant of comprehensive descision silicon chip surface contaminated area
Which kind of substance, the i.e. element in conjunction with the pollutant of silicon chip surface contaminated area form and the infrared spectroscopy and standard of Polluted area
The comparison of map, the two comprehensive dimensions can qualitatively judge the exact ingredient of the pollutant of silicon chip surface contaminated area, in turn
Source is stain for judgement, investigation contamination cause has great significance.In addition, the detection method stain of above-mentioned silicon chip surface without
Complicated pretreatment procedure need to be carried out to silicon chip surface, and will not damage silicon wafer.
In order to which objects and advantages of the present invention are more clearly understood, the present invention is carried out with reference to embodiments further
It is described in detail.It should be appreciated that described herein, specific examples are only used to explain the present invention, is not intended to limit the present invention.
Embodiment 1
A kind of detection method of polysilicon chip surface contamination comprising following steps:
1, polysilicon chip sample is adhered on sample stage, polysilicon chip sample is put into together with sample stage together then and is swept
It retouches in the sample bin of electron microscope, is evacuated to 2.0 × 10-5Then mbar adjusts beam voltage to 5kV, amplification
Multiple is 1250 times, scans polysilicon chip specimen surface contaminated area, the microscopic appearance image of contaminated area is obtained, referring to Fig. 1.
2, beam voltage is adjusted to 20kV, X-ray energy spectrum analyzer collects the X-ray energy spectrum letter of contaminated area
Number, determine that tri- kinds of elements of C, O and Si are contained in contaminated area, referring to fig. 2.
3, polysilicon chip sample is transferred on micro ft-ir spectroscopy instrument objective table, acquires the infrared microscopy light of contaminated area
Spectrum, wherein use micro ft-ir spectroscopy test condition are as follows: projecting pattern detection, spectra collection resolution ratio 4cm-1, spectrogram scanning time
Number 64 times, the acquisition diaphragm region of micro ft-ir spectroscopy is 300 μm of 300 μ m.Then by the infrared spectroscopy and mark of contaminated area
Infrared spectroscopy in quasi- sample library is compared, referring to Fig. 3.
In conjunction with the microscopic appearance image of contaminated area, the element of contaminated area forms and the comparison chart of pollutant infrared spectroscopy
Comprehensive descision, it is known that the pollutant of the contaminated area is silicone oil.
Embodiment 2
A kind of detection method that monocrystalline silicon sheet surface stains comprising following steps:
1, monocrystalline silicon piece sample is adhered on sample stage, monocrystalline silicon piece sample is put into together with sample stage together then and is swept
It retouches in the sample bin of electron microscope, is evacuated to 2.0 × 10-5Then mbar adjusts beam voltage to 5kV, amplification
Multiple is 200 times, scans monocrystalline silicon piece specimen surface contaminated area, obtains the microscopic appearance image of monocrystalline contaminated area.
2, beam voltage is adjusted to 20kV, X-ray energy spectrum analyzer collects the X-ray energy spectrum letter of contaminated area
Number, determine that two kinds of elements of C, O are contained in contaminated area.
3, monocrystalline silicon piece sample is transferred on micro ft-ir spectroscopy instrument objective table, acquires the infrared microscopy light of contaminated area
Spectrum, wherein use micro ft-ir spectroscopy test condition are as follows: projecting pattern detection, spectra collection resolution ratio 4cm-1, spectrogram scanning time
Number 64 times, the acquisition diaphragm region of micro ft-ir spectroscopy is 250 μm of 250 μ m.Then by the infrared spectroscopy and mark of contaminated area
Infrared spectroscopy in quasi- sample library is compared, referring to fig. 4.
In conjunction with the microscopic appearance image of contaminated area, the element of contaminated area forms and the comparison chart of pollutant infrared spectroscopy
Comprehensive descision, it is known that the pollutant of the contaminated area is one-component glue.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. the detection method that a kind of silicon chip surface stains, which comprises the steps of:
Constituent analysis is carried out to the contaminated area to form with the element of pollutant in the determination contaminated area；
The infrared spectroscopy for acquiring the contaminated area, by the infrared spectroscopy of the infrared spectroscopy of the contaminated area and standard sample into
Row compares.
2. the detection method that silicon chip surface according to claim 1 stains, which is characterized in that the contaminated area into
It further include scanning silicon chip surface before the step of row constituent analysis is formed with the element of pollutant in the determination contaminated area
The step of microscopic appearance of the contaminated area to obtain the contaminated area.
3. the detection method that silicon chip surface according to claim 2 stains, which is characterized in that in being stained with for scanning silicon chip surface
It is using scanning of scanning electron microscope silicon chip surface in the step of microscopic appearance of the dirty region to obtain the contaminated area
Contaminated area.
4. the detection method that silicon chip surface according to claim 3 stains, which is characterized in that the scanning electron microscope
Amplification factor is 500 times -2000 times when scanning the contaminated area.
5. the detection method that silicon chip surface according to claim 3 stains, which is characterized in that the scanning electron microscope
Beam voltage is 0.1kV-20kV when scanning the contaminated area.
6. the detection method that silicon chip surface according to claim 1-5 stains, which is characterized in that be stained with to described
It further include using red before dirty region carries out the step of constituent analysis is formed with the element of pollutant in the determination contaminated area
Outside line detects the step of contaminated area of the silicon chip surface to determine silicon chip surface.
7. the detection method that silicon chip surface according to claim 1-5 stains, which is characterized in that described in acquisition
It is the micro ft-ir spectroscopy for acquiring the contaminated area in the step of infrared spectroscopy of contaminated area.
8. the detection method that silicon chip surface according to claim 7 stains, which is characterized in that acquiring the contaminated area
Micro ft-ir spectroscopy the step of in, acquisition resolution 1cm-1-4cm-1。
9. the detection method that silicon chip surface according to claim 7 stains, which is characterized in that acquiring the contaminated area
Micro ft-ir spectroscopy the step of in, spectrogram scanning times be 16 times -256 times.
10. the detection method that silicon chip surface according to claim 7 stains, which is characterized in that acquiring the contaminated area
In the step of micro ft-ir spectroscopy in domain, acquisition diaphragm region is 100 μm -500 of 100 μ m, 500 μm of μ m.
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| CN113161253A (en) * | 2021-01-25 | 2021-07-23 | 上海磬采电力科技开发有限公司 | Wafer surface impurity pollution degree detection system |
| CN114295632A (en) * | 2021-11-30 | 2022-04-08 | 国高材高分子材料产业创新中心有限公司 | Method for detecting pollutants on surface of waste plastic |
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Application publication date: 20190521 |