CN114184622B - Method for detecting damage depth of surface of zone-melting polycrystalline silicon - Google Patents
Method for detecting damage depth of surface of zone-melting polycrystalline silicon Download PDFInfo
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 204
- 238000004857 zone melting Methods 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000005520 cutting process Methods 0.000 claims abstract description 24
- 238000005530 etching Methods 0.000 claims abstract description 22
- 229920005591 polysilicon Polymers 0.000 claims description 38
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 26
- 229940117975 chromium trioxide Drugs 0.000 claims description 19
- WGLPBDUCMAPZCE-UHFFFAOYSA-N chromium trioxide Inorganic materials O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 19
- GAMDZJFZMJECOS-UHFFFAOYSA-N chromium(6+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Cr+6] GAMDZJFZMJECOS-UHFFFAOYSA-N 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000005553 drilling Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 21
- 239000004065 semiconductor Substances 0.000 abstract description 2
- 235000012431 wafers Nutrition 0.000 description 59
- 238000005498 polishing Methods 0.000 description 14
- 238000001514 detection method Methods 0.000 description 7
- 229910003460 diamond Inorganic materials 0.000 description 7
- 239000010432 diamond Substances 0.000 description 7
- 238000000227 grinding Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 238000011282 treatment Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000003754 machining Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000003517 fume Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 238000012952 Resampling Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000003902 lesion Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
- G01N21/88—Investigating the presence of flaws or contamination
- G01N21/95—Investigating the presence of flaws or contamination characterised by the material or shape of the object to be examined
- G01N21/9501—Semiconductor wafers
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
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- Life Sciences & Earth Sciences (AREA)
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- General Health & Medical Sciences (AREA)
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- Testing Or Measuring Of Semiconductors Or The Like (AREA)
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Abstract
The invention discloses a method for detecting the damage depth of the surface of zone-melting polycrystalline silicon, and relates to the technical field of semiconductor manufacturing. One embodiment of the method comprises the following steps: cutting a next section of polycrystalline silicon rod from the machined zone-melting polycrystalline silicon rod; obtaining a polycrystalline silicon wafer from the outer edge of the polycrystalline silicon rod; etching the polycrystalline silicon wafer by adopting an etchant; and acquiring a damage image of the etched surface of the polycrystalline silicon wafer by adopting a microscope, so as to detect the damage depth of the surface of the zone-melting polycrystalline silicon. The embodiment can solve the technical problem that no method for detecting the surface damage depth of the zone-melting polycrystalline silicon is available at present.
Description
Technical Field
The invention relates to the technical field of semiconductor manufacturing, in particular to a method for detecting the damage depth of the surface of zone-melting polycrystalline silicon.
Background
At present, in the related patent literature, a detection method of the damage depth of the surface of the zone-melting polycrystalline silicon is not found, but in the patent application of CN113267521A, a detection method and an automatic detection system of the damage depth of the surface processing of a silicon product are disclosed, and the damage depth reflected by equipment X-rays is controlled; CN104034568B discloses a method for measuring the damage depth of the wafer surface, and the surface morphology of the etched wafer sample is obtained through a microscope; and the surface damage depth of the wafer sample is measured.
In the process of implementing the present invention, the inventor finds that at least the following problems exist in the prior art:
the defects of the prior art are that ultrathin and fragile silicon wafer test samples are prepared, and the processes and parameter settings of sample preparation such as grinding, polishing, corrosion treatment and the like are different, and are only limited to analysis of wafers. Therefore, no method for detecting the damage depth of the surface of the fused polysilicon is available at present.
Disclosure of Invention
In view of the above, the embodiment of the invention provides a method for detecting the surface damage depth of zone-melting polycrystalline silicon, so as to solve the technical problem that the method for detecting the surface damage depth of zone-melting polycrystalline silicon is not available at present.
In order to achieve the above object, according to an embodiment of the present invention, there is provided a method for detecting a damaged depth of a surface of a fused polysilicon, including:
cutting a next section of polycrystalline silicon rod from the machined zone-melting polycrystalline silicon rod;
obtaining a polycrystalline silicon wafer from the outer edge of the polycrystalline silicon rod;
etching the polycrystalline silicon wafer by adopting an etchant;
and acquiring a damage image of the etched surface of the polycrystalline silicon wafer by adopting a microscope, so as to detect the damage depth of the surface of the zone-melting polycrystalline silicon.
Optionally, cutting a next section of the polysilicon rod from the machined section of molten polysilicon rod, comprising:
dividing the machined zone-melting polycrystalline silicon into three zone-melting polycrystalline silicon sections with equal length;
and cutting a section of polycrystalline silicon rod from the zone-melted polycrystalline silicon section close to the bridge.
Optionally, the length of the polysilicon rod is 100mm-150mm.
Optionally, obtaining a polysilicon wafer from an outer edge of the polysilicon rod comprises:
drilling a polycrystalline silicon sample from the outer edge of the polycrystalline silicon rod by adopting a drill along the length direction of the polycrystalline silicon rod;
and cutting the polycrystalline silicon wafer at the middle position of the polycrystalline silicon sample by adopting a cutting machine along the radial direction of the polycrystalline silicon sample.
Optionally, the diameter of the polysilicon sample is 10mm-20mm.
Optionally, the thickness of the polycrystalline silicon wafer is 1.0mm-4mm.
Optionally, the thickness of the polycrystalline silicon wafer is 1.8mm-2.2mm.
Optionally, etching the polysilicon wafer with an etchant, including:
immersing the polycrystalline silicon wafer in an etchant, and etching for 5-10 seconds;
and cleaning the etched polycrystalline silicon wafer by adopting deionized water, and drying the polycrystalline silicon wafer by adopting nitrogen.
Optionally, the etchant is prepared by the following method:
dissolving chromium trioxide in deionized water to obtain 0.1-2 mol/L chromium trioxide solution;
the chromium trioxide solution is mixed with hydrofluoric acid to obtain an etchant.
Optionally, the volume ratio of the chromium trioxide solution to the hydrofluoric acid is 1:1-5:1.
One embodiment of the above invention has the following advantages or benefits: the embodiment of the invention can visually observe the surface damage depth of the polycrystalline silicon rod after machining by a microscope, and provides a detection method for the downstream production chain pulling single crystal silicon rod.
Further effects of the above-described non-conventional alternatives are described below in connection with the embodiments.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art. Wherein:
FIG. 1 is a schematic diagram of the main flow of a method for detecting the damage depth of a fused polysilicon surface according to an embodiment of the present invention;
FIG. 2 is a schematic view of a structure of a zone-melted polysilicon rod according to an embodiment of the present invention;
FIG. 3 is a schematic diagram according to an embodiment of the invention;
fig. 4a and 4b are schematic diagrams of an image of a lesion according to an embodiment of the present invention.
Detailed Description
Exemplary embodiments of the present invention will now be described with reference to the accompanying drawings, in which various details of the embodiments of the present invention are included to facilitate understanding, and are to be considered merely exemplary. Accordingly, those of ordinary skill in the art will recognize that various changes and modifications of the embodiments described herein can be made without departing from the scope and spirit of the invention. Also, descriptions of well-known functions and constructions are omitted in the following description for clarity and conciseness.
The surface damage depth refers to the damage depth of the surface of the silicon rod caused by external force in the processes of lathe, grinding and the like when the polycrystalline silicon rod is processed, and can be reflected on a polycrystalline silicon wafer.
The surface damage depth of the zone-melting polycrystalline silicon is mainly found in the machining process of the zone-melting polycrystalline silicon, and when a single crystal silicon rod is pulled downstream, the crystal line is broken or the crystal form is misplaced due to the large damage depth, so that the single crystal yield is greatly reduced, and therefore, the surface damage depth of the zone-melting polycrystalline silicon is very necessary to be detected.
In order to solve the technical problems in the prior art, the embodiment of the invention provides a method for detecting the surface damage depth of zone-melting polycrystalline silicon, which is mainly used for detecting the surface damage depth of zone-melting polycrystalline silicon after mechanical processing.
Fig. 1 is a schematic diagram of the main flow of a method for detecting the damage depth of a fused polysilicon surface according to an embodiment of the present invention. As an embodiment of the present invention, as shown in fig. 1, the method for detecting the damage depth of the surface of the zone-melted polysilicon may include:
and 101, cutting a section of polycrystalline silicon rod from the machined zone-melting polycrystalline silicon rod.
And 102, obtaining the polycrystalline silicon chip from the outer edge of the polycrystalline silicon rod.
And step 103, etching the polycrystalline silicon wafer by adopting an etchant.
And 104, acquiring a damage image of the surface of the etched polycrystalline silicon wafer by adopting a microscope, so as to detect the damage depth of the surface of the fused polycrystalline silicon.
The embodiment of the invention can visually observe the surface damage depth of the polycrystalline silicon rod after machining by a microscope, and provides a detection method for the downstream production chain pulling single crystal silicon rod.
Optionally, step 101 may include: dividing the machined zone-melting polycrystalline silicon into three zone-melting polycrystalline silicon sections with equal length; and cutting a section of polycrystalline silicon rod from the zone-melted polycrystalline silicon section close to the bridge. As shown in FIG. 2, the bridge end where the silicon rod grows is started to be an end A, the electrode end is a C end, the middle is a section B, and the zone-melting polycrystalline silicon can be divided into three zone-melting polycrystalline silicon sections with equal length, namely an A section polycrystalline silicon rod, a B section polycrystalline silicon rod and a C section polycrystalline silicon rod.
Optionally, the length of the polycrystalline silicon rod cut is 100mm-150mm, on one hand, to adapt to the length of the cutting tool and on the other hand, to reduce damage caused by stress in the tool during the sample preparation process. Of these, the lengths of the polysilicon rods are typically, but not limited to, preferably 100mm, 120mm, 125mm, 136mm, 147mm and 150mm, and in these embodiments, the damage caused by the cutters during the sample preparation process can be effectively reduced.
Optionally, step 102 may include: drilling a polycrystalline silicon sample from the outer edge of the polycrystalline silicon rod by adopting a drill along the length direction of the polycrystalline silicon rod; and cutting the polycrystalline silicon wafer at the middle position of the polycrystalline silicon sample by adopting a cutting machine along the radial direction of the polycrystalline silicon sample. As shown in fig. 3, a 15mm drill is used to drill a polysilicon sample from the outer edge of the polysilicon rod along the length direction of the polysilicon rod, and the polysilicon sample is approximately semi-cylindrical since the diameter of the polysilicon rod is much greater than 15 mm. According to the embodiment of the invention, the drill bit is adopted to drill the polycrystalline silicon sample from the outer edge of the polycrystalline silicon rod, so that the damage depth of the zone-melted polycrystalline silicon surface can be observed conveniently.
After the polycrystalline silicon wafer is cut from the middle position of the polycrystalline silicon sample by adopting a cutting machine, the polycrystalline silicon wafer can be further subjected to grinding, polishing and other treatments, so that a polycrystalline silicon sheet with a certain thickness is finally formed, and the image is conveniently collected on a microscope.
Alternatively, the diameter of the polysilicon sample is 10mm-20mm, that is, the diameter of the drill may be 10mm-20mm, and the purpose of the embodiment of the present invention is to detect the edge of polysilicon, if the diameter of the cutter is too large, the edge of polysilicon may be damaged, thereby affecting the detection result. Of these, the diameters of the polysilicon samples are typically, but not limited to, preferably 10mm, 12mm, 15mm, 16mm, and 20mm, and in these embodiments damage to the polysilicon edges may be avoided.
Optionally, the thickness of the polycrystalline silicon wafer is 1.0mm-4mm, so that polishing is facilitated, and images are conveniently acquired on a microscope. Among them, the thickness of the polycrystalline silicon wafer is typically, but not limited to, preferably 1.0mm, 1.5mm, 2mm, 2.2mm, 3.1mm, 3.8mm and 4mm. Preferably, the thickness of the polycrystalline silicon wafer is 1.8mm-2.2mm, and the polycrystalline silicon wafer within the thickness range is more suitable for observation and image acquisition by a microscope.
Optionally, step 103 may include: immersing the polycrystalline silicon wafer in an etchant, and etching for 5-10 seconds; and cleaning the etched polycrystalline silicon wafer by adopting deionized water, and drying the polycrystalline silicon wafer by adopting nitrogen. The embodiment of the invention controls the etching time within 5-10 seconds, so that the etchant can be ensured to only etch the surface of the polycrystalline silicon slice, thereby being beneficial to detecting the damage depth of the surface. Wherein immersion times of the polysilicon wafer in the etchant are typically, but not limited to, preferably 5 seconds, 6 seconds, 8 seconds, 10 seconds, etc., in these embodiments, it is ensured that the etchant etches only the surface of the polysilicon wafer.
Optionally, the etchant is prepared by the following method: dissolving chromium trioxide in deionized water to obtain 0.1-2 mol/L chromium trioxide solution; and mixing the chromium trioxide solution with hydrofluoric acid to obtain an etchant, and etching the surface of the polycrystalline silicon wafer by using the etchant, so that the damage depth of the surface of the polycrystalline silicon wafer can be detected under a microscope. Among them, chromium trioxide solutions are typically, but not limited to, preferably 0.1mol/L, 0.28mol/L, 0.5mol/L, 1.0mol/L, 1.3mol/L, 1.75mol/L, and 2.0mol/L, and in these embodiments, etching with these etchants all help to detect the depth of damage to the surface of a polycrystalline silicon wafer under a microscope.
Optionally, the volume ratio of the chromium trioxide solution to the hydrofluoric acid is 1:1-8:1, and the etchant prepared by the method is used for etching the surface of the polycrystalline silicon wafer, so that the damage depth of the surface of the polycrystalline silicon wafer can be detected under a microscope. Wherein the volume ratio of the chromium trioxide solution to the hydrofluoric acid is typically, but not limited to, preferably 1:1, 2:1, 2.5:1, 3:1, 5:1, 6:1 and 8:1, and the etchant thus configured is used for etching the surface of the polycrystalline silicon wafer, thereby facilitating the detection of the damage depth of the surface of the polycrystalline silicon wafer under a microscope.
To aid in understanding the scheme of the present invention, several specific processes for detecting the depth of damage to the surface of the zone-melted polysilicon are given below.
Example 1
The main equipment and the raw materials are as follows:
fume hood Fisher PP CL-PVC custom-built fume hood with acid removal function, electron microscope with 500 times magnification, etching basket, chromium trioxide (CrO 3 ) 48% hydrofluoric acid, zone-melting grade polycrystalline silicon rod, cutting machine, grinding machine, polishing machine and deionized water: all of the water should be deionized water, 3 μm diamond paste or slurry of type E-1 or other equivalent quality as described in ASTM D5127.
Step 1) dividing the polycrystalline silicon rod into three sections on a grown zone-melting polycrystalline silicon rod, taking a bridge end of the growth of the polycrystalline silicon rod as an end A, taking an electrode end as an end C and taking the middle as a section B, dividing the zone-melting polycrystalline silicon into three equal-length zone-melting polycrystalline silicon sections, cutting a section of polycrystalline silicon rod with the length of 100mm from the zone-melting polycrystalline silicon section (the section A shown in fig. 2) close to the bridge, taking a silicon core as the center, selecting two symmetrical positions, using a drill with the diameter of 15mm, drilling polycrystalline silicon samples with the diameter of 15mm on the outer edge of the polycrystalline silicon rod by adopting a pressureless drill, obtaining two semi-cylindrical polycrystalline silicon samples with the diameter of 15mm, taking one sample as a reserved sample, respectively performing appearance inspection, checking whether the machined surface of each polycrystalline silicon sample has drill damage, and packaging the number. If the polysilicon sample is damaged, resampling is required.
Step 2) taking the polycrystalline silicon sample out of the sample bag, cutting a polycrystalline silicon wafer with the thickness of 2.8mm at the middle position of the polycrystalline silicon sample by using a cutting machine, polishing the polycrystalline silicon wafer on one side of the 3 mu m diamond polishing paste after the polishing treatment of the diamond thorn to obtain the polycrystalline silicon wafer with the thickness of 2.0mm, and visually checking whether the machining edge of the polycrystalline silicon wafer is damaged by polishing. If damaged, the sample lot is reworked and marked on the unpolished side.
Step 3) weighing 1gCrO 3 Dissolving in 1L deionized water to obtain 1 mol.L -1 Is then subjected to the oxidationThe chromium solution and hydrofluoric acid are mixed according to the volume ratio of 5:1 to obtain the etchant.
And 4) placing the polycrystalline silicon wafer into an etching basket, engraving a character face upwards, pouring the prepared etchant into a digestion tank, keeping the wafer completely immersed in the etchant, rapidly transferring the etching basket into an overflow deionized water tank after etching for 5 seconds, flushing the polycrystalline silicon wafer with flowing deionized water for at least 5 minutes, taking out the polycrystalline silicon wafer, and drying the polycrystalline silicon wafer by using nitrogen.
And 5) opening the electron microscope, adjusting the magnification to 500 times, placing the wafer on a microscope stage, polishing the surface upwards, and adjusting the stage to align the lens to the edge of the growth layer of the polycrystalline silicon wafer. The magnification of the microscope may be selected and adjusted as necessary according to the apparatus.
Step 6) adjusting the focal length of the microscope so that the focal point is aligned with the surface of the polycrystalline silicon wafer, and after the depth of damage is found, adding the measured value (recording only the depth of damage measured from the outer growth layer direction) and counting as shown in fig. 4a and 4 b.
Example 2
Which differs from the manufacturing method of example 1 in that: in step 1), a section of 120mm length polysilicon rod is cut from the section of zone-melted polysilicon adjacent to the bridge.
Example 3
Which differs from the manufacturing method of example 1 in that: in step 1), a length of 150mm of polysilicon rod is cut from the section of zone-melted polysilicon close to the bridge.
Example 4
Which differs from the manufacturing method of example 1 in that: in step 1), a section of polycrystalline silicon rod with a length of 135mm is cut from the section of zone-melted polycrystalline silicon near the bridge.
Example 5
Which differs from the manufacturing method of example 1 in that: in step 1), a length of 150mm of polysilicon rod is cut from the section of zone-melted polysilicon close to the bridge.
Example 6
Which differs from the manufacturing method of example 1 in that: in step 1), a drill with the diameter of 10mm is used, a pressureless drill is used for drilling a polycrystalline silicon sample with the diameter of 10mm on the outer edge of a polycrystalline silicon rod, two semicylindrical polycrystalline silicon samples with the diameter of 10mm are obtained,
example 7
Which differs from the manufacturing method of example 1 in that: in step 1), a drill bit with the diameter of 13mm is used, a pressureless drill bit is used for drilling a polycrystalline silicon sample with the diameter of 13mm on the outer edge of a polycrystalline silicon rod, two semicylindrical polycrystalline silicon samples with the diameter of 13mm are obtained,
example 8
Which differs from the manufacturing method of example 1 in that: in step 1), a drill with the diameter of 20mm is used, a pressureless drill is used for drilling a polycrystalline silicon sample with the diameter of 20mm on the outer edge of a polycrystalline silicon rod, two semicylindrical polycrystalline silicon samples with the diameter of 20mm are obtained,
example 9
Which differs from the manufacturing method of example 1 in that: in step 1), a drill bit with the diameter of 18mm is used, a pressureless drill bit is used for drilling a polycrystalline silicon sample with the diameter of 18mm on the outer edge of a polycrystalline silicon rod, two semicylindrical polycrystalline silicon samples with the diameter of 18mm are obtained,
example 10
Which differs from the manufacturing method of example 1 in that: in the step 2), a polycrystalline silicon wafer with the thickness of 3.0mm is cut at the middle position of the polycrystalline silicon sample by a cutting machine, and after the diamond is subjected to grinding treatment, the polycrystalline silicon wafer with the thickness of 1.8mm is obtained by single-sided polishing on the 3 mu m diamond polishing paste.
Example 11
Which differs from the manufacturing method of example 1 in that: in the step 2), a polycrystalline silicon wafer with the thickness of 3.5mm is cut at the middle position of the polycrystalline silicon sample by a cutting machine, and after the diamond is subjected to grinding treatment, the polycrystalline silicon wafer with the thickness of 2.2mm is obtained by single-sided polishing on the 3 mu m diamond polishing paste.
Example 12
Which differs from the manufacturing method of example 1 in that: in step 3)Weighing 0.1g CrO 3 Dissolving in 1L deionized water to obtain 0.1 mol.L -1 And then mixing the chromium trioxide solution with hydrofluoric acid according to a volume ratio of 4:1 to obtain the etchant.
Example 13
Which differs from the manufacturing method of example 1 in that: in step 3), 0.5g of CrO is weighed 3 Dissolving in 1L deionized water to obtain 0.5 mol.L -1 And then mixing the chromium trioxide solution with hydrofluoric acid according to a volume ratio of 3:1 to obtain the etchant.
Example 14
Which differs from the manufacturing method of example 1 in that: in step 3), 1g of CrO is weighed 3 Dissolving in 1L deionized water to obtain 1 mol.L -1 And then mixing the chromium trioxide solution with hydrofluoric acid according to a volume ratio of 6:1 to obtain the etchant.
Example 15
Which differs from the manufacturing method of example 1 in that: in step 3), 2g of CrO are weighed 3 Dissolving in 1L deionized water to obtain 2mol.L -1 And then mixing the chromium trioxide solution with hydrofluoric acid according to a volume ratio of 1:1 to obtain the etchant.
Example 16
Which differs from the manufacturing method of example 1 in that: in step 4), the wafer is kept completely immersed in the etchant for etching for 6 seconds.
Example 17
Which differs from the manufacturing method of example 1 in that: in step 4), the wafer is kept completely immersed in the etchant for etching for 10 seconds.
Example 18
Which differs from the manufacturing method of example 1 in that: in step 4), the wafer is kept completely immersed in the etchant for etching for 8 seconds.
Therefore, the polycrystalline silicon wafer for detecting the surface damage depth is obtained by cutting, grinding, polishing, etching and other processes on the zone-melting polycrystalline silicon rod, and the polycrystalline silicon wafer is placed under an electron microscope to measure the surface damage depth. The method can be used for detecting the damage depth of the surface of the zone-melting polycrystalline silicon and visually observing the sub-microcrack of the growth of the zone-melting polycrystalline silicon, and has the main advantages of simple operation, stable process and low equipment requirement.
The above embodiments do not limit the scope of the present invention. It will be apparent to those skilled in the art that various modifications, combinations, sub-combinations and alternatives can occur depending upon design requirements and other factors. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the scope of the present invention.
Claims (8)
1. The method for detecting the damage depth of the surface of the zone-melting polycrystalline silicon is characterized by comprising the following steps of:
cutting a next section of polycrystalline silicon rod from the machined zone-melting polycrystalline silicon rod;
obtaining a polycrystalline silicon wafer from the outer edge of the polycrystalline silicon rod;
etching the polycrystalline silicon wafer by adopting an etchant;
acquiring a damage image of the etched surface of the polycrystalline silicon wafer by adopting a microscope, so as to detect the damage depth of the surface of the zone-melting polycrystalline silicon;
cutting a section of polycrystalline silicon rod from the machined zone-melting polycrystalline silicon rod, comprising:
dividing the machined zone-melting polycrystalline silicon into three zone-melting polycrystalline silicon sections with equal length;
cutting a section of polycrystalline silicon rod from the zone-melted polycrystalline silicon section close to the bridge;
obtaining a polycrystalline silicon wafer from the outer edge of the polycrystalline silicon rod comprises the following steps:
drilling a polycrystalline silicon sample from the outer edge of the polycrystalline silicon rod by adopting a drill along the length direction of the polycrystalline silicon rod;
and cutting the polycrystalline silicon wafer at the middle position of the polycrystalline silicon sample by adopting a cutting machine along the radial direction of the polycrystalline silicon sample.
2. The method of claim 1, wherein the length of the polysilicon rod is 100mm-150mm.
3. The method of claim 1, wherein the polysilicon sample has a diameter of 10mm to 20mm.
4. A method according to claim 3, wherein the polycrystalline silicon wafer has a thickness of 1.0mm to 4mm.
5. The method of claim 4, wherein the polysilicon wafer has a thickness of 1.8mm to 2.2mm.
6. The method of claim 1, wherein etching the polysilicon wafer with an etchant comprises:
immersing the polycrystalline silicon wafer in an etchant, and etching for 5-10 seconds;
and cleaning the etched polycrystalline silicon wafer by adopting deionized water, and drying the polycrystalline silicon wafer by adopting nitrogen.
7. The method of claim 6, wherein the etchant is prepared by:
dissolving chromium trioxide in deionized water to obtain 0.1-2 mol/L chromium trioxide solution;
the chromium trioxide solution is mixed with hydrofluoric acid to obtain an etchant.
8. The method according to claim 7, wherein the volume ratio of the chromium trioxide solution to the hydrofluoric acid is 1:1-8:1.
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