CN117457519A - Method for detecting thickness of damaged layer in silicon single crystal processing - Google Patents
Method for detecting thickness of damaged layer in silicon single crystal processing Download PDFInfo
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- CN117457519A CN117457519A CN202311358865.0A CN202311358865A CN117457519A CN 117457519 A CN117457519 A CN 117457519A CN 202311358865 A CN202311358865 A CN 202311358865A CN 117457519 A CN117457519 A CN 117457519A
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 129
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 129
- 239000010703 silicon Substances 0.000 title claims abstract description 129
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000012545 processing Methods 0.000 title claims abstract description 16
- 239000013078 crystal Substances 0.000 title claims description 26
- 238000001514 detection method Methods 0.000 claims abstract description 49
- 238000004140 cleaning Methods 0.000 claims description 21
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 20
- 230000007797 corrosion Effects 0.000 claims description 15
- 238000005260 corrosion Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 14
- 230000003287 optical effect Effects 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000005259 measurement Methods 0.000 claims description 12
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 claims description 11
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 239000004519 grease Substances 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 239000012459 cleaning agent Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 229910021421 monocrystalline silicon Inorganic materials 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003599 detergent Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
- H01L22/10—Measuring as part of the manufacturing process
- H01L22/12—Measuring as part of the manufacturing process for structural parameters, e.g. thickness, line width, refractive index, temperature, warp, bond strength, defects, optical inspection, electrical measurement of structural dimensions, metallurgic measurement of diffusions
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B11/00—Measuring arrangements characterised by the use of optical techniques
- G01B11/02—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness
- G01B11/06—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B11/00—Measuring arrangements characterised by the use of optical techniques
- G01B11/22—Measuring arrangements characterised by the use of optical techniques for measuring depth
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Testing Or Measuring Of Semiconductors Or The Like (AREA)
Abstract
The invention provides a method for detecting thickness of a silicon monocrystalline processing damaged layer, which relates to the technical field of monocrystalline silicon detection methods.
Description
Technical Field
The invention belongs to the technical field of monocrystalline silicon detection methods, and particularly relates to a method for detecting thickness of a silicon monocrystalline processing damaged layer.
Background
Silicon single crystal is an important semiconductor material, various high-power transistors, rectifiers, integrated circuits, solar cells and the like can be manufactured by utilizing the property of the silicon single crystal, and the silicon single crystal rod to a semiconductor device or a solar cell sheet are required to be subjected to processes such as slicing, grinding, etching, polishing and the like, a mechanical damage layer with a certain thickness is generated on the surface of a silicon wafer in a machining process, and the mechanical damage layer is required to be completely removed when the surface flatness of the silicon wafer is processed in the subsequent processes such as acid-base treatment, physical chemical polishing and the like, and if the damage layer is not completely removed, a large number of unsaturated bonds exist in the damage layer, metal particles are easy to be adsorbed, so that the performance of the semiconductor device is influenced; therefore, the thickness of the damaged layer on the surface of the silicon wafer needs to be known, so that the damaged layer cannot be completely removed in the subsequent process, and the quality of the final product is prevented from being influenced.
In the prior art, the silicon wafer is usually detected by means of an X-ray double-star diffraction method, a scanning electron microscope and the like, but the detection equipment for the detection method is high in price and is not applicable to industrial production detection, so that a new detection method for a damaged layer of the silicon wafer needs to be explored.
Disclosure of Invention
In view of this, the present invention provides a novel method for detecting the thickness of a damaged layer in the processing of silicon single crystals.
The technical scheme adopted for solving the technical problems is as follows:
a method for detecting thickness of damaged layer in silicon single crystal processing comprises the following steps,
s1: cleaning the original silicon wafer to remove grease on the surface of the original silicon wafer and obtain a cleaned silicon wafer;
s2: preparing a detection liquid, putting the cleaned silicon wafer into the detection liquid, and anisotropically corroding the silicon wafer at a preset temperature for a preset time to obtain a corroded silicon wafer containing pits;
s3: rinsing the corrosion silicon wafer containing the pits with weak base to obtain a detection silicon wafer;
s4: and placing the detection silicon wafer under an optical microscope, and measuring the depth of the pit to obtain the thickness of the mechanical damage layer of the detection silicon wafer.
Preferably, in the step S1: the cleaning of the original silicon wafer specifically comprises the following steps: and fully cleaning the original silicon wafer by using an organic cleaning agent to obtain an initial cleaned silicon wafer.
Preferably, in the step S1, the cleaning of the original silicon wafer specifically further includes: and (3) after the alcohol is heated, putting the initially cleaned silicon wafer into alcohol to be boiled, and drying after boiling.
Preferably, the temperature of the alcohol heating is 65 ℃ to 75 ℃.
Preferably, in the step S2: the detection liquid is prepared from chromic acid solution and hydrofluoric acid solution.
Preferably, the volume ratio of the chromic acid solution to the hydrofluoric acid solution is 1-10: 1.
preferably, in the step S2: the preset temperature is 20-35 ℃, and the preset time is 20-25 min.
Preferably, in the step S3, the weak base is one of ammonia water and sodium carbonate.
Preferably, in the step S4, the depth of the measuring pit is specifically: the optical microscope automatically fits the deepest pit for measurement.
Preferably, in the step S4, after the depth of an area is measured by the optical microscope, different positions are adjusted, measurement is repeated, and an average value is obtained to obtain the thickness of the mechanically damaged layer of the detected silicon wafer.
Compared with the prior art, the invention has the beneficial effects that:
according to the method for detecting the thickness of the silicon single crystal processing damaged layer, the original silicon wafer is cleaned to remove grease on the surface of the original silicon wafer to obtain the cleaned silicon wafer, the cleaned silicon wafer is placed into the detection liquid, the silicon wafer is anisotropically corroded at the preset temperature for a preset time, so that the damaged crystal lattice of the cleaned silicon wafer is corroded, the complete crystal lattice is left, the corroded silicon wafer containing pits is obtained, the corroded silicon wafer containing pits is rinsed by weak base to obtain the detected silicon wafer, finally the detected silicon wafer is placed under an optical microscope, the depth of the pits is measured to obtain the thickness of the mechanical damaged layer of the detected silicon wafer, and the thickness of the damaged layer of the silicon wafer is detected through anisotropism preferential corrosion.
Drawings
FIG. 1 is a graph showing the test results of test No. 1 in example one.
FIG. 2 is a graph showing the test results of test No. 2 in example one.
FIG. 3 is a graph showing the test results of test No. 3 in example one.
FIG. 4 is a graph showing the test results of test No. 4 in example one.
FIG. 5 is a graph showing the test results of test No. 5 in example one.
Fig. 6 is a graph of the detection result of comparative example one.
Detailed Description
The technical scheme and technical effects of the embodiments of the present invention are further described in detail below with reference to the accompanying drawings.
A method for detecting thickness of damaged layer in silicon single crystal processing comprises the following steps,
s1: cleaning the original silicon wafer to remove grease on the surface of the original silicon wafer, and reducing subsequent detection errors to obtain a cleaned silicon wafer;
s2: preparing a detection liquid, putting the cleaned silicon wafer into the detection liquid, and anisotropically corroding the silicon wafer at a preset temperature for a preset time to obtain a corroded silicon wafer containing pits;
s3: rinsing the corrosion silicon wafer containing the pits with weak base to obtain a detection silicon wafer;
s4: and placing the detection silicon wafer under an optical microscope, and measuring the depth of the pit to obtain the thickness of the mechanical damage layer of the detection silicon wafer.
Compared with the prior art, the invention has the beneficial effects that:
according to the method for detecting the thickness of the silicon single crystal processing damaged layer, the original silicon wafer is cleaned to remove grease on the surface of the original silicon wafer to obtain the cleaned silicon wafer, the cleaned silicon wafer is placed into the detection liquid, the silicon wafer is anisotropically corroded at the preset temperature for a preset time, so that the damaged crystal lattice of the cleaned silicon wafer is corroded, the complete crystal lattice is left, the corroded silicon wafer containing pits is obtained, the corroded silicon wafer containing pits is rinsed by weak base to obtain the detected silicon wafer, finally the detected silicon wafer is placed under an optical microscope, the depth of the pits is measured to obtain the thickness of the mechanical damaged layer of the detected silicon wafer, the thickness of the damaged layer of the silicon wafer is detected through anisotropism preferential corrosion, the detection method is simple and convenient, and the detection result is accurate.
Further, in the step S1: the cleaning of the original silicon wafer specifically comprises the following steps: and fully cleaning the original silicon wafer by using an organic cleaning agent to obtain an initial cleaned silicon wafer so as to effectively remove organic pollution such as grease on the surface of the silicon wafer.
Specifically, the organic cleaning agent is a detergent or a surfactant and the like.
Further, in the step S1, the cleaning of the original silicon wafer specifically further includes: and (3) after the alcohol is heated, putting the initially cleaned silicon wafer into alcohol to be boiled, and drying after boiling.
Further, the temperature of the heating of the alcohol is 65-75 ℃; and (3) putting the initial cleaning silicon wafer into alcohol to boil for 10min, drying the boiled silicon wafer under hot nitrogen or hot air, carrying out secondary boiling on the dried product for 30s, and drying again, and circulating for 5 times to obtain the cleaning silicon wafer so as to remove a large amount of organic pollutants and reduce detection errors.
Further, in the step S2: the detection solution is prepared from chromic acid solution and hydrofluoric acid solution, the chromic acid solution has extremely strong preference, and the reaction rate is extremely high at the lattice distortion place due to the concentration of stress, and has extremely high rate difference with the complete lattice, so that the complete lattice reaction is almost negligible under the condition of short time, and the damage layer is detected by anisotropic corrosion reaction.
Further, the volume ratio of the chromic acid solution to the hydrofluoric acid solution is 1-10: 1, a stress field is caused in a detection liquid prepared by chromic acid solution and hydrofluoric acid solution for cleaning a damaged layer of a silicon wafer, anisotropic corrosion is carried out, so that the corrosion rate of the damaged layer is accelerated, and a great speed difference is generated between the damaged layer and a complete crystal lattice, so that the complete crystal lattice can be in a convex hillock shape on the surface of the corroded silicon wafer, a damaged part can be corroded into a concave pit shape, the selectivity is amplified to the greatest extent, the thickness of the damaged layer is calculated by measuring the height difference between the mountain top and the pit bottom, and the calculated result is accurate.
Further, in the step S2: the preset temperature is 20-35 ℃, the preset time is 20-25min, the temperature is too low, chromium-containing products can be attached to the surface of a silicon wafer, measurement accuracy is affected, the temperature is too high, the time is too long, transverse corrosion is accelerated, hills are flat, measurement errors are increased, and a damage layer is not completely corroded, so that measurement results are affected.
In the step S3, the weak base is one of ammonia water and sodium carbonate so as to sufficiently remove acid marks on the surface of the etched silicon wafer.
Further, in the step S4, the depth of the measuring pit is specifically: at one measurement position, the optical microscope automatically fits the deepest pit for measurement.
In the step S4, after the optical microscope measures the depth of an area, the different positions are adjusted, the measurement is repeated, the number of measured data samples is greater than 10, and the average value is obtained to obtain the thickness of the mechanically damaged layer of the detected silicon wafer.
Embodiment one:
taking a 0.5-1 inch silicon wafer, fully cleaning an original silicon wafer with a detergent to obtain an initial cleaning silicon wafer, heating the initial cleaning silicon wafer with alcohol at 65-75 ℃, putting the initial cleaning silicon wafer into alcohol to boil for 10min, drying the boiled silicon wafer under hot nitrogen at 90 ℃, boiling the dried product for 30s for a second time, drying again, and circulating for 5 times to obtain a cleaning silicon wafer, preparing a detection solution, mixing the detection solution with a chromic acid solution with the concentration of 5-10% and a hydrofluoric acid solution with the concentration of 40-49% at the concentration of 10-8:4-2, putting the cleaning silicon wafer into the detection solution, and corroding for a preset time at 25 ℃ to obtain a corroded silicon wafer containing pits; rinsing the corrosion silicon wafer containing the pits with 10% -20% ammonia water solution to obtain a detection silicon wafer; and placing the detection silicon wafer under an optical microscope, and then, corroding to form a plurality of hills, wherein the optical microscope can automatically fit the highest hills and the lowest hills in the area, calculate the height difference, adjust different positions, measure for 10 times, and calculate the average value to obtain the thickness of the mechanical damage layer processed by the process.
According to the experimental method, the influence of the constant corrosion temperature on the thickness of the damaged layer, which is numbered 1-5, of the corrosion time of the cleaned silicon wafer in the detection liquid is explored, the corrosion temperature and the corrosion time are shown in the table 1, and the results are shown in fig. 1-5.
TABLE 1
From experiment 1 to experiment 5, the thickness data of the damaged layer is stable or slightly smaller after increasing along with the increase of the reaction time, and the data is maximum and is an optimal value in 20-25 min; experiments 1 and 5 show that the time is too short, the damaged layer is not completely corroded, the measurement result is affected, the time is too long, the transverse corrosion is too much, the hills are flat, and the measurement error is increased.
Comparative example one:
the results of sampling a silicon wafer similar to the examples, sampling an angular section microscopic observation in the united states of america recognized authority test, and obtaining the results are shown in fig. 6.
As can be seen from the comparison of the test numbers 4 in the first comparative example and the first embodiment, the detection method of the invention can accurately detect the thickness of the damaged layer of the silicon wafer, has accurate detection results, provides a basis for the establishment of the subsequent acid-base and physicochemical polishing processes, is simple and quick to operate, has low cost, and is suitable for industrial production.
Comparative example two:
the method is characterized in that a silicon wafer similar to the embodiment is taken, a detection solution is prepared by mixing 1% -5% chromic acid solution and 40% -49% hydrofluoric acid solution according to a volume ratio of 1-2:1, the silicon wafer is corroded for 20-25min at 25 ℃ to detect the thickness of a damaged layer of the silicon wafer with 0.5-1 inch, the detection method is the same as that of the embodiment, the test is carried out for 5 times, and the detection result is shown in table 1.
TABLE 2
Comparative example three:
the silicon wafer similar to the embodiment is taken, the detection liquid is prepared by mixing 20% -30% of chromic acid liquid and 40% -49% of hydrofluoric acid solution according to the volume ratio of 1-2:1, the silicon wafer is corroded for 20-25min at 25 ℃ to detect the thickness of a damaged layer of the silicon wafer of 0.5-1 inch, the detection method is the same as that of the embodiment, the test is carried out for 5 times, and the detection result is shown in table 2.
TABLE 3 Table 3
As can be seen from the comparison of the first embodiment with the second and third embodiments, the detection solution is different, and serious errors exist in the detection result, so that the thickness of the silicon wafer damaged layer cannot be accurately obtained.
The foregoing disclosure is illustrative of the preferred embodiments of the present invention, and is not to be construed as limiting the scope of the invention, as it is understood by those skilled in the art that all or part of the above-described embodiments may be practiced with equivalents thereof, which fall within the scope of the invention as defined by the appended claims.
Claims (10)
1. A method for detecting thickness of a silicon single crystal processing damaged layer is characterized by comprising the following steps: comprises the steps of,
s1: cleaning the original silicon wafer to remove grease on the surface of the original silicon wafer and obtain a cleaned silicon wafer;
s2: preparing a detection liquid, putting the cleaned silicon wafer into the detection liquid, and anisotropically corroding the silicon wafer at a preset temperature for a preset time to obtain a corroded silicon wafer containing pits;
s3: rinsing the corrosion silicon wafer containing the pits with weak base to obtain a detection silicon wafer;
s4: and placing the detection silicon wafer under an optical microscope, and measuring the depth of the pit to obtain the thickness of the mechanical damage layer of the detection silicon wafer.
2. The method for detecting a thickness of a damaged layer in a silicon single crystal processing according to claim 1, wherein: in the step S1: the cleaning of the original silicon wafer specifically comprises the following steps: and fully cleaning the original silicon wafer by using an organic cleaning agent to obtain an initial cleaned silicon wafer.
3. The method for detecting thickness of damaged layer in silicon single crystal processing according to claim 2, wherein: in the step S1, the cleaning of the original silicon wafer specifically further includes: and (3) after the alcohol is heated, putting the initially cleaned silicon wafer into alcohol to be boiled, and drying after boiling.
4. The method for detecting a thickness of a damaged layer in a silicon single crystal process according to claim 3, wherein: the heating temperature of the alcohol is 65-75 ℃.
5. The method for detecting thickness of damaged layer in silicon single crystal processing according to claim 2, wherein: in the step S2: the detection liquid is prepared from chromic acid solution and hydrofluoric acid solution.
6. The method for detecting a thickness of a damaged layer in a silicon single crystal process according to claim 5, wherein: the volume ratio of the chromic acid solution to the hydrofluoric acid solution is 1-10: 1.
7. the method for detecting thickness of damaged layer in silicon single crystal processing according to claim 2, wherein: in the step S2: the preset temperature is 20-35 ℃, and the preset time is 20-25 min.
8. The method for detecting thickness of damaged layer in silicon single crystal processing according to claim 2, wherein: in the step S3, the weak base is one of ammonia water and sodium carbonate.
9. The method for detecting thickness of damaged layer in silicon single crystal processing according to claim 2, wherein: in the step S4, the depth of the measuring pit is specifically: the optical microscope automatically fits the deepest pit for measurement.
10. The method for detecting a thickness of a damaged layer in a silicon single crystal process according to claim 9, wherein: and in the step S4, after the depth of one area is measured by the optical microscope, adjusting different positions, repeating the measurement, and obtaining an average value to obtain the thickness of the mechanical damage layer of the detection silicon wafer.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311358865.0A CN117457519A (en) | 2023-10-19 | 2023-10-19 | Method for detecting thickness of damaged layer in silicon single crystal processing |
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| CN202311358865.0A CN117457519A (en) | 2023-10-19 | 2023-10-19 | Method for detecting thickness of damaged layer in silicon single crystal processing |
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