CN116259533A - Method for cleaning phosphoric acid etching residues, silicon wafer, processing method thereof and chip - Google Patents
Method for cleaning phosphoric acid etching residues, silicon wafer, processing method thereof and chip Download PDFInfo
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- CN116259533A CN116259533A CN202310533405.0A CN202310533405A CN116259533A CN 116259533 A CN116259533 A CN 116259533A CN 202310533405 A CN202310533405 A CN 202310533405A CN 116259533 A CN116259533 A CN 116259533A
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- 238000004140 cleaning Methods 0.000 title claims abstract description 183
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 147
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 77
- 239000010703 silicon Substances 0.000 title claims abstract description 77
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 63
- 238000005530 etching Methods 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 49
- 238000003672 processing method Methods 0.000 title abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 177
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 177
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 68
- 238000004380 ashing Methods 0.000 claims abstract description 46
- 238000001035 drying Methods 0.000 claims abstract description 43
- 239000000243 solution Substances 0.000 claims description 51
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 239000012530 fluid Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 229910000831 Steel Inorganic materials 0.000 claims 1
- 239000010959 steel Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 35
- 235000012431 wafers Nutrition 0.000 description 69
- 230000007547 defect Effects 0.000 description 14
- 239000012535 impurity Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 13
- 229910052581 Si3N4 Inorganic materials 0.000 description 12
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 12
- 238000010586 diagram Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02057—Cleaning during device manufacture
- H01L21/0206—Cleaning during device manufacture during, before or after processing of insulating layers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/16—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only elements of Group IV of the Periodic Table
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- 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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- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Manufacturing & Machinery (AREA)
- Ceramic Engineering (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
The application relates to a cleaning method of phosphoric acid etching residues, a silicon wafer, a processing method of the silicon wafer and a chip. The method for cleaning the phosphoric acid etching residues comprises the following steps: carrying out first washing on the sample subjected to phosphoric acid etching, wherein the temperature of the first washing is 55-70 ℃; carrying out SC1 cleaning solution cleaning on the sample subjected to the first water washing, wherein the temperature of the SC1 cleaning solution cleaning is 60-70 ℃; carrying out second water washing on the sample cleaned by the SC1 cleaning solution, wherein the temperature of the second water washing is 55-70 ℃; IPA drying is carried out on the sample after the second water washing; ashing the sample after IPA drying; and (3) carrying out high-temperature sulfuric acid cleaning on the ashed sample, wherein the temperature of the high-temperature sulfuric acid cleaning is 110-120 ℃. The method for cleaning the phosphoric acid etching residues has good effect on removing the phosphoric acid residues, can reduce the amount of the phosphoric acid residues on the surface of the sample, and can reduce the occurrence of water marks on the surface of the sample.
Description
Technical Field
The present disclosure relates to the field of chip manufacturing technologies, and in particular, to a method for cleaning phosphoric acid etching residues, a silicon wafer, a processing method thereof, and a chip.
Background
During the fabrication of the chip, the silicon nitride of the operable region needs to be etched. In this etching step, a phosphoric acid etching solution is generally used to etch silicon nitride. Phosphoric acid etching liquid is easy to remain on the surface of a sample due to the viscous physical property. Therefore, after etching of silicon nitride is completed, the phosphoric acid residue on the sample surface needs to be cleaned. However, the conventional method for cleaning the phosphoric acid etching residues has poor cleaning effect on the phosphoric acid residues, which results in a large amount of the phosphoric acid residues on the sample surface, thereby causing defects on the sample surface. Meanwhile, if the sample after phosphoric acid etching is subjected to hot water cleaning for a long time, water marks on the surface of the sample are easily caused.
Disclosure of Invention
Accordingly, it is necessary to provide a method for cleaning the phosphoric acid etching residues, a silicon wafer, a method for processing the silicon wafer, and a chip. The method for cleaning the phosphoric acid etching residues has a good cleaning effect on the phosphoric acid residues, can reduce the amount of the phosphoric acid residues on the surface of a sample, and can reduce the occurrence of water marks on the surface of the sample.
In a first aspect, the present application provides a method for cleaning a phosphoric acid etching residue, comprising:
carrying out first washing on the sample subjected to phosphoric acid etching, wherein the temperature of the first washing is 55-70 ℃;
carrying out SC1 cleaning fluid cleaning on the sample after the first water cleaning, wherein the temperature of the SC1 cleaning fluid cleaning is 60-70 ℃, and the SC1 cleaning fluid comprises NH 4 OH、H 2 O 2 And H 2 O, where NH 4 OH、H 2 O 2 And H 2 The mass ratio of O is 1:2:50-1:1:200;
performing second water washing on the sample cleaned by the SC1 cleaning solution, wherein the temperature of the second water washing is 55-70 ℃;
IPA drying is carried out on the sample after the second water washing;
ashing the sample dried by IPA;
and carrying out high-temperature sulfuric acid cleaning on the ashed sample, wherein the temperature of the high-temperature sulfuric acid cleaning is 110-120 ℃.
In some embodiments, the SC1 cleaning time is 200s to 300s.
In some embodiments, the first water washing time is 200s to 300s.
In some embodiments, the second water washing time is 200s to 300s.
In some embodiments, the IPA is dried for 320s to 480s.
In some embodiments, the IPA drying temperature is 40℃to 60 ℃.
In some embodiments, the ashing process has an oxygen flow rate of 8000sccm to 12000sccm.
In some embodiments, the nitrogen flow rate of the ashing process is 800sccm to 1000sccm.
In some embodiments, the ashing process is performed at a power of 2000 watts to 4500 watts.
In some embodiments, the high temperature sulfuric acid wash is with H 2 SO 4 And H 2 O 2 Is washed.
In some embodiments, the H 2 SO 4 The mass fraction of (2) is 90% -98%.
In some embodiments, the H 2 O 2 The mass fraction of the (C) is 20% -40%.
In some embodiments, the SC1 cleaning solution further comprises a third water washing step for the sample after the first water washing step, wherein the temperature of the third water washing step is 25 ℃ to 35 ℃.
In some embodiments, the method further comprises performing a fourth water washing on the sample after the second water washing, wherein the temperature of the fourth water washing is 25-35 ℃.
In some embodiments, the third water washing time is 200s to 300s.
In some embodiments, the fourth water washing time is 200s to 300s.
In a second aspect, the present application provides a method for processing a silicon wafer, including:
etching the silicon wafer using phosphoric acid;
the silicon wafer is cleaned using any of the above-described cleaning methods of the phosphoric acid etching residues.
In a third aspect, the present application provides a silicon wafer processed by any one of the above-described processing methods for a silicon wafer.
In a fourth aspect, the present application provides a chip comprising the silicon wafer described above.
The method for cleaning the phosphoric acid etching residues comprises the steps of sequentially performing first water washing, SC1 cleaning liquid cleaning, second water washing, IPA drying, ashing treatment and high-temperature sulfuric acid cleaning on the sample after phosphoric acid etching. Wherein the temperature of the first water washing is 55-70 ℃, the temperature of the SC1 cleaning liquid is 60-70 ℃, the temperature of the second water washing is 55-70 ℃, and the temperature of the high-temperature sulfuric acid washing is 110-120 ℃. According to the cleaning method, after the sample is etched by phosphoric acid, through the cooperation of the first water washing, the SC1 cleaning solution washing, the second water washing, the IPA drying, the ashing treatment and the high-temperature sulfuric acid cleaning, the cleaning process has a good effect on removing phosphoric acid residues, the amount of the phosphoric acid residues on the surface of the sample can be reduced, and meanwhile, the occurrence of water marks on the surface of the sample can be reduced.
Drawings
FIG. 1 is a schematic flow chart of a method for cleaning a phosphoric acid etching residue according to an embodiment of the present disclosure;
FIG. 2 is a flow chart of a method for cleaning a phosphoric acid etching residue according to another embodiment of the present disclosure;
FIG. 3 is an SEM image of the surface of a silicon wafer provided in comparative example 1 of the present application after 24 hours of placement;
FIG. 4 is an SEM image of the surface defect area of a silicon wafer after 24 hours of placement, provided in comparative example 1 of the present application;
FIG. 5 is a bright field image and dark field image of a surface defect area after 24 hours of placement of a silicon wafer as provided in comparative example 1 of the present application;
FIG. 6 is a graph showing the energy spectrum of surface defects after 24 hours of placement of a silicon wafer according to comparative example 1 of the present application;
fig. 7 is a schematic diagram of elemental analysis of a surface defect area after 24h of placement of a silicon wafer according to comparative example 1 of the present application, wherein fig. 7 (a) is a Si element distribution diagram, fig. 7 (b) is a P element distribution diagram, fig. 7 (c) is an O element distribution diagram, fig. 7 (d) is a Pt element distribution diagram, and fig. 7 (e) is an N element schematic diagram;
fig. 8 is an SEM image of the surface of the silicon wafer provided in comparative example 2 of the present application after being left for 48 hours.
Detailed Description
In order to make the above objects, features and advantages of the present application more comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present application. This application is, however, susceptible of embodiment in many other forms than those described herein and similar modifications can be made by those skilled in the art without departing from the spirit of the application, and therefore the application is not to be limited to the specific embodiments disclosed below.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
An embodiment of the present application provides a method for cleaning a phosphoric acid etching residue, referring to fig. 1, including:
s101: carrying out first washing on the sample subjected to phosphoric acid etching, wherein the temperature of the first washing is 55-70 ℃;
s102: carrying out SC1 cleaning solution cleaning on the sample subjected to the first water washing, wherein the temperature of the SC1 cleaning solution cleaning is 60-70 ℃, and the SC1 cleaning solution comprises NH 4 OH、H 2 O 2 And H 2 O, where NH 4 OH、H 2 O 2 And H 2 The mass ratio of O is 1:2:50-1:1:200;
s103: carrying out second water washing on the sample cleaned by the SC1 cleaning solution, wherein the temperature of the second water washing is 55-70 ℃;
s104: IPA drying is carried out on the sample after the second water washing;
s105: ashing the sample after IPA drying;
s106: and (3) carrying out high-temperature sulfuric acid cleaning on the ashed sample, wherein the temperature of the high-temperature sulfuric acid cleaning is 110-120 ℃. The method for cleaning the phosphoric acid etching residues comprises the steps of sequentially performing first water washing, SC1 cleaning liquid cleaning, second water washing, IPA drying, ashing treatment and high-temperature sulfuric acid cleaning on the sample after phosphoric acid etching. Wherein the temperature of the first water washing is 55-70 ℃, the temperature of the SC1 cleaning liquid is 60-70 ℃, the temperature of the second water washing is 55-70 ℃, and the temperature of the high-temperature sulfuric acid washing is 110-120 ℃. According to the cleaning method, after the sample is etched by phosphoric acid, through the cooperation of the first water washing, the SC1 cleaning solution washing, the second water washing, the IPA drying, the ashing treatment and the high-temperature sulfuric acid cleaning, the cleaning process has a good effect on removing phosphoric acid residues, the amount of the phosphoric acid residues on the surface of the sample can be reduced, and meanwhile, the occurrence of water marks on the surface of the sample can be reduced.
In the temperature range of the SC1 cleaning solution, the cleaning effect on the phosphoric acid etching residues is better, and the effect of reducing the water mark on the surface of the sample is better. Alternatively, the SC1 wash is at a temperature of 60 ℃, 60.5 ℃, 61 ℃, 61.5 ℃, 62 ℃, 62.5 ℃, 63 ℃, 63.5 ℃, 64 ℃, 64.5 ℃, 65 ℃, 65.5 ℃, 66 ℃, 66.5 ℃, 67 ℃, 67.5 ℃, 68 ℃, 68.5 ℃, 69 ℃, 69.5 ℃ or 70 ℃. In the temperature range of the first water washing, the cleaning effect on the phosphoric acid etching residues is good, and the effect of reducing water marks on the surface of the sample is good. Alternatively, the temperature of the first water wash is 55 ℃, 56 ℃, 57 ℃, 58 ℃, 59 ℃, 60 ℃, 61 ℃, 62 ℃, 63 ℃, 64 ℃, 65 ℃, 66 ℃, 67 ℃, 68 ℃, 69 ℃, or 70 ℃. In some embodiments, the temperature of the second water wash is 55 ℃ to 70 ℃. In the temperature range of the second water washing, the cleaning effect on the phosphoric acid etching residues is good, and the effect of reducing water marks on the surface of the sample is good. Optionally, the second water wash is at a temperature of 55 ℃, 56 ℃, 57 ℃, 58 ℃, 59 ℃, 60 ℃, 61 ℃, 62 ℃, 63 ℃, 64 ℃, 65 ℃, 66 ℃, 67 ℃, 68 ℃, 69 ℃, or 70 ℃. In the temperature range of the high-temperature sulfuric acid cleaning, the cleaning effect on the phosphoric acid etching residues is good, and the effect of reducing water marks on the surface of a sample is good. Alternatively, the high temperature sulfuric acid cleaning is performed at a temperature of 110 ℃, 111 ℃, 112 ℃, 113 ℃, 114 ℃, 115 ℃, 116 ℃, 117 ℃, 118 ℃, 119 ℃, or 120 ℃.
In some embodiments, the SC1 rinse is performed for 200s to 300s. In the time range of the SC1 cleaning solution cleaning, the SC1 cleaning solution has better cleaning effect on phosphoric acid residues and better effect on reducing water marks on the surface of a sample. Optionally, the SC1 wash solution is washed for 200s, 205s, 210s, 215s, 220s, 225s, 230s, 235s, 240s, 245s, 250s, 255s, 260s, 265s, 270s, 275s, 280s, 285s, 290s, 295s or 300s.
In some embodiments, the first water wash time is 200s to 300s. In the time range of the first water washing, the cleaning effect on the phosphoric acid residues is good, and the effect of reducing water marks on the surface of the sample is good. Optionally, the first water wash time is 200s, 205s, 210s, 215s, 220s, 225s, 230s, 235s, 240s, 245s, 250s, 255s, 260s, 265s, 270s, 275s, 280s, 285s, 290s, 295s or 300s.
In some embodiments, the second water wash time is 200s to 300s. In the time range of the second water washing, the cleaning effect on the phosphoric acid residues is good, and the effect of reducing the occurrence of water marks on the surface of the sample is good. Optionally, the second water wash is for 200s, 205s, 210s, 215s, 220s, 225s, 230s, 235s, 240s, 245s, 250s, 255s, 260s, 265s, 270s, 275s, 280s, 285s, 290s, 295s or 300s.
In some embodiments, the IPA is dried for 320s to 480s. In this IPA drying time range, the IPA drying effect is good, and the phosphoric acid residue cleaning effect is good. Optionally, the IPA is dried for 320s, 325s, 330s, 335s, 340s, 345s, 350s, 355s, 360s, 365s, 370s, 375s, 380s, 385s, 390s, 395s, 400s, 405s, 410s, 415s, 420s, 425s, 430s, 435s, 440s, 445s, 450s, 455s, 460s, 465s, 470s, 475s or 480s.
In some embodiments, the IPA is dried for a time of 60% -80% of the total time of the first water wash and the second water wash. Optionally, the drying time is 60%, 61%, 62%, 63%, 64%, 65%, 66%, 67%, 68%, 69%, 70%, 71%, 72%, 73%, 74%, 75%, 76%, 77%, 78%, 79% or 80% of the total time of the first and second water washes.
In some embodiments, the temperature of the IPA drying is 40℃to 60 ℃. Alternatively, the IPA drying temperature is 40 ℃, 42 ℃, 44 ℃, 46 ℃, 48 ℃, 50 ℃, 52 ℃, 54 ℃, 56 ℃, 58 ℃ or 60 ℃.
In some embodiments, the oxygen flow rate of the ashing process is in the range of 8000sccm to 12000sccm. In the oxygen flow rate range of the ashing treatment, the effect of the ashing treatment is good. Optionally, the ashing process has an oxygen flow rate of 8000sccm, 8200sccm, 8400sccm, 8600sccm, 8800sccm, 9000sccm, 9200sccm, 9400sccm, 9600sccm, 9800sccm, 10000sccm, 10200sccm, 10400sccm, 10600sccm, 10800sccm, 11000sccm, 11200sccm, 11400sccm, 11600sccm, 11800sccm, or 12000sccm.
In some embodiments, the nitrogen flow rate of the ashing process is 800sccm to 1000sccm. In the nitrogen flow rate range of the ashing treatment, the effect of the ashing treatment is good. Optionally, the nitrogen flow rate of the ashing process is 800sccm, 810sccm, 820sccm, 830sccm, 840sccm, 850sccm, 860sccm, 870sccm, 880sccm, 890sccm, 900sccm, 910sccm, 920sccm, 930sccm, 940sccm, 950sccm, 960sccm, 970sccm, 980sccm, 990sccm, or 1000sccm.
In some embodiments, the ashing process is performed at a power of 2000 watts to 4500 watts. In the power range of the ashing treatment, the effect of the ashing treatment is good. Alternatively, the ashing process has a power of 2000 watts, 2100 watts, 2200 watts, 2300 watts, 2400 watts, 2500 watts, 2600 watts, 2700 watts, 2800 watts, 2900 watts, 3000 watts, 3100 watts, 3200 watts, 3300 watts, 3400 watts, 3500 watts, 3600 watts, 3700 watts, 3800 watts, 3900 watts, 4000 watts, 4100 watts, 4200 watts, 4300 watts, 4400 watts, or 4500 watts.
In some embodiments, the high temperature sulfuric acid rinse is performed using H 2 SO 4 And H 2 O 2 Is washed.
In some embodiments, H 2 SO 4 The mass fraction of (2) is 90% -98%. Alternatively, H 2 SO 4 Is 90%, 91%, 92%, 93%, 94%, 95%, 96%, 97% or 98% by mass.
In some embodiments, H 2 O 2 The mass fraction of the (C) is 20% -40%. Alternatively, H 2 O 2 Is 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39% or 40% by mass.
In some embodiments, the SC1 cleaning solution further comprises a third water washing step of performing a third water washing step on the sample after the first water washing step, wherein the temperature of the third water washing step is 25 ℃ to 35 ℃. In the temperature range of the third water washing, the cleaning effect on the phosphoric acid residues is good, and the effect of reducing water marks on the surface of the sample is good. Optionally, the temperature of the third water wash is 25 ℃, 25.5 ℃, 26 ℃, 26.5 ℃, 27 ℃, 27.5 ℃, 28 ℃, 28.5 ℃, 29 ℃, 29.5 ℃, 30 ℃, 30.5 ℃, 31, 31.5 ℃, 32 ℃, 32.5 ℃, 33 ℃, 33.5 ℃, 34 ℃, 34.5 ℃ or 35 ℃.
In some embodiments, the method further comprises performing a fourth water washing on the sample after the second water washing, wherein the temperature of the fourth water washing is 25-35 ℃. In the temperature range of the fourth water washing, the cleaning effect on the phosphoric acid residues is good, and the effect of reducing water marks on the surface of the sample is good. Optionally, the fourth water wash has a temperature of 25 ℃, 25.5 ℃, 26 ℃, 26.5 ℃, 27 ℃, 27.5 ℃, 28 ℃, 28.5 ℃, 29 ℃, 29.5 ℃, 30 ℃, 30.5 ℃, 31, 31.5 ℃, 32 ℃, 32.5 ℃, 33 ℃, 33.5 ℃, 34 ℃, 34.5 ℃ or 35 ℃.
In some embodiments, the third water wash time is 200s to 300s. In the time range of the third water washing, the cleaning effect on the phosphoric acid residues is good, and the effect of reducing the occurrence of water marks on the surface of the sample is good. Optionally, the third water wash is for 200s, 205s, 210s, 215s, 220s, 225s, 230s, 235s, 240s, 245s, 250s, 255s, 260s, 265s, 270s, 275s, 280s, 285s, 290s, 295s or 300s.
In some embodiments, the fourth water wash time is 200s to 300s. In the time range of the fourth water washing, the cleaning effect on the phosphoric acid residues is good, and the effect of reducing the occurrence of water marks on the surface of the sample is good. Optionally, the fourth water wash time is 200s, 205s, 210s, 215s, 220s, 225s, 230s, 235s, 240s, 245s, 250s, 255s, 260s, 265s, 270s, 275s, 280s, 285s, 290s, 295s or 300s.
In some embodiments, referring to fig. 2, the method of cleaning the phosphoric acid etch residue comprises the steps of:
s201: carrying out first washing on the sample subjected to phosphoric acid etching, wherein the temperature of the first washing is 55-70 ℃, and the time of the first washing is 200-300 s;
s202: carrying out third water washing on the sample after the first water washing, wherein the temperature of the third water washing is 25-35 ℃, and the time of the third water washing is 200-300 s;
s203: carrying out SC1 cleaning solution cleaning on the sample subjected to the third water cleaning, wherein the temperature of the SC1 cleaning solution cleaning is 60-70 ℃, the time of the SC1 cleaning solution cleaning is 200-300 s, and the SC1 cleaning solution comprises NH 4 OH、H 2 O 2 And H 2 O, where NH 4 OH、H 2 O 2 And H 2 The mass ratio of O is 1:2:50-1:1:200;
s204: carrying out second washing on the sample cleaned by the SC1 cleaning solution, wherein the temperature of the second washing is 55-70 ℃, and the time of the second washing is 200-300 s;
s205: carrying out fourth water washing on the sample after the second water washing, wherein the temperature of the fourth water washing is 25-35 ℃, and the time of the fourth water washing is 200-300 s;
s206: performing IPA drying on the sample subjected to the fourth water washing, wherein the time of IPA drying is 320-480 s, and the temperature of IPA drying is 40-60 ℃;
s207: carrying out ashing treatment on the sample subjected to IPA drying, wherein the oxygen flow rate of the ashing treatment is 800-12000 sccm, the nitrogen flow rate of the ashing treatment is 800-1000 sccm, and the power of the ashing treatment is 2000-4500 watts;
s208: carrying out high-temperature sulfuric acid cleaning on the ashed sample, wherein the temperature of the high-temperature sulfuric acid cleaning is 110-120 ℃, and the high-temperature sulfuric acid cleaning is H 2 SO 4 And H 2 O 2 Is washed by the mixed solution of H 2 SO 4 The mass fraction of (2) is 90% -98%, H 2 O 2 The mass fraction of the (C) is 20% -40%.
In one embodiment, the method for cleaning the phosphoric acid etching residues comprises the following steps:
(1) Carrying out first washing on the sample subjected to phosphoric acid etching, wherein the temperature of the first washing is 55-70 ℃, and the time of the first washing is 200-300 s;
(2) Carrying out third water washing on the sample after the first water washing, wherein the temperature of the third water washing is 25-35 ℃, and the time of the third water washing is 200-300 s;
(3) Carrying out SC1 cleaning solution cleaning on the sample subjected to the third water cleaning, wherein the temperature of the SC1 cleaning solution cleaning is 60-70 ℃, the time of the SC1 cleaning solution cleaning is 200-300 s, and the SC1 cleaning solution comprises NH 4 OH、H 2 O 2 And H 2 O, where NH 4 OH、H 2 O 2 And H 2 The mass ratio of O is 1:2:50-1:1:200;
(4) Carrying out second washing on the sample cleaned by the SC1 cleaning solution, wherein the temperature of the second washing is 55-70 ℃, and the time of the second washing is 200-300 s;
(5) Carrying out fourth water washing on the sample after the second water washing, wherein the temperature of the fourth water washing is 25-35 ℃, and the time of the fourth water washing is 200-300 s;
(6) Performing IPA drying on the sample subjected to the fourth water washing, wherein the time of IPA drying is 320-480 s, and the temperature of IPA drying is 40-60 ℃;
(7) Carrying out ashing treatment on the sample subjected to IPA drying, wherein the oxygen flow rate of the ashing treatment is 800-12000 sccm, the nitrogen flow rate of the ashing treatment is 800-1000 sccm, and the power of the ashing treatment is 2000-4500 watts;
(8) Carrying out high-temperature sulfuric acid cleaning on the ashed sample, wherein the temperature of the high-temperature sulfuric acid cleaning is 110-120 ℃, and the high-temperature sulfuric acid cleaning is H 2 SO 4 And H 2 O 2 Is washed by the mixed solution of H 2 SO 4 The mass fraction of (2) is 90% -98%, H 2 O 2 The mass fraction of the (C) is 20% -40%.
Yet another embodiment of the present application provides a method for processing a silicon wafer, including:
etching the silicon wafer using phosphoric acid;
the silicon wafer is cleaned using any of the above-described cleaning methods of the phosphoric acid etching residues.
In some embodiments, the cleaning method using any of the above phosphoric acid etching residues further comprises, prior to cleaning the silicon wafer:
and removing impurities on the surface of the silicon wafer.
In some embodiments, removing the impurities from the surface of the silicon wafer is removing the impurities from the surface of the silicon wafer using dilute hydrofluoric acid (DHF).
In some embodiments, removing impurities from the surface of the silicon wafer further comprises performing a fifth water wash on the silicon wafer, wherein the temperature of the fifth water wash is 25-35 ℃. Optionally, the fifth water wash has a temperature of 25 ℃, 25.5 ℃, 26 ℃, 26.5 ℃, 27 ℃, 27.5 ℃, 28 ℃, 28.5 ℃, 29 ℃, 29.5 ℃, 30 ℃, 30.5 ℃, 31, 31.5 ℃, 32 ℃, 32.5 ℃, 33 ℃, 33.5 ℃, 34 ℃, 34.5 ℃ or 35 ℃.
In some embodiments, the fifth water wash time is 200s to 300s. Optionally, the fifth water wash time is 200s, 205s, 210s, 215s, 220s, 225s, 230s, 235s, 240s, 245s, 250s, 255s, 260s, 265s, 270s, 275s, 280s, 285s, 290s, 295s or 300s.
In some embodiments, the mass concentration of phosphoric acid is 75% -90%. Within the phosphoric acid concentration range, the effect of phosphoric acid on etching silicon nitride on the surface of the silicon wafer is good. Alternatively, the mass concentration of phosphoric acid is 75%, 76%, 77%, 78%, 79%, 80%, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88%, 89%, or 90%.
In some embodiments, the silicon nitride on the surface of the silicon wafer is etched using phosphoric acid at a temperature of 155-165 ℃. The phosphoric acid has a good effect of etching the silicon nitride on the surface of the silicon wafer in the temperature range. Alternatively, the silicon nitride on the surface of the silicon wafer is etched using phosphoric acid at a temperature of 155 ℃, 155.5 ℃, 156 ℃, 156.5 ℃, 157 ℃, 157.5 ℃, 158 ℃, 158.5 ℃, 159 ℃, 159.5 ℃, 160 ℃, 160.5 ℃, 161 ℃, 161.5 ℃, 162 ℃, 162.5 ℃, 163 ℃, 163.5 ℃, 164 ℃, 164.5 ℃ or 165 ℃.
In some embodiments, a method of processing a silicon wafer includes the steps of:
(1) Providing a silicon wafer;
(2) Removing impurities on the surface of the silicon wafer by using DHF;
(3) Carrying out fifth water washing on the silicon wafer with the surface impurities removed, wherein the temperature of the fifth water washing is 25-35 ℃, and the time of the fifth water washing is 200-300 s;
(4) Etching the silicon nitride on the surface of the silicon wafer by using phosphoric acid;
(5) Carrying out first washing on the etched sample, wherein the temperature of the first washing is 55-70 ℃, and the time of the first washing is 200-300 s;
(6) Carrying out third water washing on the sample after the first water washing, wherein the temperature of the third water washing is 25-35 ℃, and the time of the third water washing is 200-300 s;
(7) Carrying out SC1 cleaning solution cleaning on the sample subjected to the third water cleaning, wherein the temperature of the SC1 cleaning solution cleaning is 60-70 ℃, the time of the SC1 cleaning solution cleaning is 200-300 s, and the SC1 cleaning solution comprises NH 4 OH、H 2 O 2 And H 2 O, where NH 4 OH、H 2 O 2 And H 2 The mass ratio of O is 1:2:50-1:1:200;
(8) Carrying out second washing on the sample cleaned by the SC1 cleaning solution, wherein the temperature of the second washing is 55-70 ℃, and the time of the second washing is 200-300 s;
(9) Carrying out fourth water washing on the sample after the second water washing, wherein the temperature of the fourth water washing is 25-35 ℃, and the time of the fourth water washing is 200-300 s;
(10) Performing IPA drying on the sample subjected to the fourth water washing, wherein the time of IPA drying is 320-480 s, and the temperature of IPA drying is 40-60 ℃;
(11) Carrying out ashing treatment on the sample subjected to IPA drying, wherein the oxygen flow rate of the ashing treatment is 800-12000 sccm, the nitrogen flow rate of the ashing treatment is 800-1000 sccm, and the power of the ashing treatment is 2000-4500 watts;
(12) Carrying out high-temperature sulfuric acid cleaning on the ashed sample, wherein the temperature of the high-temperature sulfuric acid cleaning is 110-120 ℃, and the high-temperature sulfuric acid cleaning is H 2 SO 4 And H 2 O 2 Is washed by the mixed solution of H 2 SO 4 The mass fraction of (2) is 90% -98%, H 2 O 2 The mass fraction of the (C) is 20% -40%.
In one embodiment, the method of processing a silicon wafer comprises the steps of:
(1) Providing a silicon wafer;
(2) Removing impurities on the surface of the silicon wafer by using DHF;
(3) Carrying out fifth water washing on the silicon wafer with the surface impurities removed, wherein the temperature of the fifth water washing is 25-35 ℃, and the time of the fifth water washing is 200-300 s;
(4) Etching the silicon nitride on the surface of the silicon wafer by using phosphoric acid;
(5) Carrying out first washing on the etched sample, wherein the temperature of the first washing is 55-70 ℃, and the time of the first washing is 200-300 s;
(6) Carrying out third water washing on the sample after the first water washing, wherein the temperature of the third water washing is 25-35 ℃, and the time of the third water washing is 200-300 s;
(7) Carrying out SC1 cleaning solution cleaning on the sample subjected to the third water cleaning, wherein the temperature of the SC1 cleaning solution cleaning is 60-70 ℃, the time of the SC1 cleaning solution cleaning is 200-300 s, and the SC1 cleaning solution comprises NH 4 OH、H 2 O 2 And H 2 O, where NH 4 OH、H 2 O 2 And H 2 The mass ratio of O is 1:2:50-1:1:200;
(8) Carrying out second washing on the sample cleaned by the SC1 cleaning solution, wherein the temperature of the second washing is 55-70 ℃, and the time of the second washing is 200-300 s;
(9) Carrying out fourth water washing on the sample after the second water washing, wherein the temperature of the fourth water washing is 25-35 ℃, and the time of the fourth water washing is 200-300 s;
(10) Performing IPA drying on the sample subjected to the fourth water washing, wherein the time of IPA drying is 320-480 s, and the temperature of IPA drying is 40-60 ℃;
(11) Carrying out ashing treatment on the sample subjected to IPA drying, wherein the oxygen flow rate of the ashing treatment is 800-12000 sccm, the nitrogen flow rate of the ashing treatment is 800-1000 sccm, and the power of the ashing treatment is 2000-4500 watts;
(12) Carrying out high-temperature sulfuric acid cleaning on the ashed sample, wherein the temperature of the high-temperature sulfuric acid cleaning is 110-120 ℃, and the high-temperature sulfuric acid cleaning is H 2 SO 4 And H 2 O 2 Is washed by the mixed solution of H 2 SO 4 The mass fraction of (2) is 90% -98%, H 2 O 2 The mass fraction of the (C) is 20% -40%.
A further embodiment of the present application provides a silicon wafer processed by any one of the above-described processing methods of a silicon wafer.
Yet another embodiment of the present application provides a chip including the silicon wafer described above.
The following are specific examples.
Example 1
(1) Providing a silicon wafer;
(2) Removing impurities on the surface of the silicon wafer by using DHF;
(3) Carrying out fifth water washing on the silicon wafer with the surface impurities removed, wherein the temperature of the fifth water washing is 25-35 ℃, and the time of the fifth water washing is 200-300 s;
(4) Etching silicon nitride on the surface of a silicon wafer by using phosphoric acid, wherein the mass concentration of the phosphoric acid is 75% -90%, and the etching temperature is 155 ℃ -165 ℃;
(5) Carrying out first washing on the sample subjected to phosphoric acid etching, wherein the temperature of the first washing is 55-70 ℃, and the time of the first washing is 200-300 s;
(6) Carrying out third water washing on the sample after the first water washing, wherein the temperature of the third water washing is 25-35 ℃, and the time of the third water washing is 200-300 s;
(7) Carrying out SC1 cleaning solution cleaning on the sample subjected to the third water cleaning, wherein the temperature of the SC1 cleaning solution cleaning is 60-70 ℃, the time of the SC1 cleaning solution cleaning is 200-300 s, and the SC1 cleaning solution comprises NH 4 OH、H 2 O 2 And H 2 O, where NH 4 OH、H 2 O 2 And H 2 The mass ratio of O is 1:2:50-1:1:200;
(8) Carrying out second washing on the sample cleaned by the SC1 cleaning solution, wherein the temperature of the second washing is 55-70 ℃, and the time of the second washing is 200-300 s;
(9) Carrying out fourth water washing on the sample after the second water washing, wherein the temperature of the fourth water washing is 25-35 ℃, and the time of the fourth water washing is 200-300 s;
(10) Performing IPA drying on the sample subjected to the fourth water washing, wherein the time of IPA drying is 320-480 s, and the temperature of IPA drying is 40-60 ℃;
(11) Carrying out ashing treatment on the sample subjected to IPA drying, wherein the oxygen flow rate of the ashing treatment is 800-12000 sccm, the nitrogen flow rate of the ashing treatment is 800-1000 sccm, and the power of the ashing treatment is 2000-4500 watts;
(12) Carrying out high-temperature sulfuric acid cleaning on the ashed sample, wherein the temperature of the high-temperature sulfuric acid cleaning is 110-120 ℃, and the high-temperature sulfuric acid cleaning is H 2 SO 4 And H 2 O 2 Is washed by the mixed solution of H 2 SO 4 The mass fraction of (2) is 90% -98%, H 2 O 2 The mass fraction of the (C) is 20% -40%.
Comparative example 1
(1) Providing a silicon wafer;
(2) Removing impurities on the surface of the silicon wafer by using DHF;
(3) Carrying out fifth water washing on the silicon wafer with the surface impurities removed, wherein the temperature of the fifth water washing is 25-35 ℃, and the time of the fifth water washing is 200-300 s;
(4) Etching silicon nitride on the surface of a silicon wafer by using phosphoric acid, wherein the mass concentration of the phosphoric acid is 75% -90%, and the etching temperature is 155 ℃ -165 ℃;
(5) Carrying out first washing on the etched silicon wafer, wherein the temperature of the first washing is 55-70 ℃, and the time of the first washing is 200-300 s;
(6) Performing third water washing on the silicon wafer subjected to the first water washing, wherein the temperature of the third water washing is 25-35 ℃, and the time of the third water washing is 200-300 s;
(7) Carrying out SC1 cleaning solution cleaning on the sample subjected to the third water cleaning, wherein the temperature of the SC1 cleaning solution cleaning is 30-40 ℃, the time of the SC1 cleaning solution cleaning is 200-300 s, and the SC1 cleaning solution comprises NH 4 OH、H 2 O 2 And H 2 O, where NH 4 OH、H 2 O 2 And H 2 The mass ratio of O is 1:2:50-1:1:200;
(8) And (3) performing IPA drying on the silicon wafer cleaned by the SC1 cleaning solution, wherein the IPA drying time is 240s, and the temperature of the IPA drying is 40-60 ℃.
Comparative example 2
(1) Providing a silicon wafer;
(2) Removing impurities on the surface of the silicon wafer by using DHF;
(3) Carrying out fifth water washing on the silicon wafer with the surface impurities removed, wherein the temperature of the fifth water washing is 25-35 ℃, and the time of the fifth water washing is 200-300 s;
(4) Etching silicon nitride on the surface of a silicon wafer by using phosphoric acid, wherein the mass concentration of the phosphoric acid is 75% -90%, and the etching temperature is 155 ℃ -165 ℃;
(5) Performing first water washing on the silicon wafer, wherein the temperature of the first water washing is 55-70 ℃, and the time of the first water washing is 450-600 s;
(6) Performing third water washing on the silicon wafer subjected to the first water washing, wherein the temperature of the third water washing is 25-35 ℃, and the time of the third water washing is 200-300 s;
(7) Carrying out SC1 cleaning solution cleaning on the sample subjected to the third water cleaning, wherein the temperature of the SC1 cleaning solution cleaning is 30-40 ℃, the time of the SC1 cleaning solution cleaning is 200-300 s, and the SC1 cleaning solution comprises NH 4 OH、H 2 O 2 And H 2 O, where NH 4 OH、H 2 O 2 And H 2 The mass ratio of O is 1:2:50-1:1:200;
(8) And (3) performing IPA drying on the silicon wafer cleaned by the SC1 cleaning solution, wherein the IPA drying time is 320-480 s, and the temperature of the IPA drying is 40-60 ℃.
The surface defect state of the silicon wafers processed in example 1 and comparative examples 1 to 2 was observed after the wafers were left to stand. The silicon wafer obtained in example 1 was left for 72 hours without defects. Referring to fig. 3 to 4, after the silicon wafer obtained in comparative example 1 was left for 24 hours, a circular region defect was generated on the surface, and fig. 5 is a bright field image and a dark field image of the circular defect, wherein BF-S is a bright field image and HAADF is a dark field image. Referring to fig. 6 to 7, elemental analysis of the circular region defect can find that phosphorus remains in the circular region defect. Referring to fig. 8, the silicon wafer obtained in comparative example 2 gradually developed defects similar to those of comparative example 1 in which phosphorus remained after being left for 48 hours, and the surface of the silicon wafer additionally developed water film defects. Compared with comparative examples 1 and 2, the removal effect of phosphoric acid residue in example 1 is better, the amount of phosphoric acid residue in the obtained silicon wafer is smaller, the silicon wafer can not generate the defect of phosphorus residue in a longer time, and the subsequent processing of the silicon wafer is convenient.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples merely represent a few embodiments of the present application, which are described in more detail and are not to be construed as limiting the scope of the invention. It should be noted that it would be apparent to those skilled in the art that various modifications and improvements could be made without departing from the spirit of the present application, which would be within the scope of the present application. The scope of the patent is therefore intended to be covered by the appended claims, and the description and drawings may be interpreted as illustrative of the contents of the claims.
Claims (10)
1. A method for cleaning a phosphoric acid etching residue, comprising:
carrying out first washing on the sample subjected to phosphoric acid etching, wherein the temperature of the first washing is 55-70 ℃;
carrying out SC1 cleaning fluid cleaning on the sample after the first water cleaning, wherein the temperature of the SC1 cleaning fluid cleaning is 60-70 ℃, and the SC1 cleaning fluid comprises NH 4 OH、H 2 O 2 And H 2 O, where NH 4 OH、H 2 O 2 And H 2 The mass ratio of O is 1:2:50-1:1:200;
performing second water washing on the sample cleaned by the SC1 cleaning solution, wherein the temperature of the second water washing is 55-70 ℃;
IPA drying is carried out on the sample after the second water washing;
ashing the sample dried by IPA;
and carrying out high-temperature sulfuric acid cleaning on the ashed sample, wherein the temperature of the high-temperature sulfuric acid cleaning is 110-120 ℃.
2. The method for cleaning phosphoric acid etching residues according to claim 1, wherein the time for cleaning the SC1 is 200s to 300s;
and/or the time of the first water washing is 200 s-300 s;
and/or the second water washing time is 200 s-300 s.
3. The method of claim 1, wherein the IPA is dried for 320s to 480s;
and/or the IPA drying temperature is 40-60 ℃.
4. The method for cleaning a phosphoric acid etching residue according to claim 1, wherein,
the oxygen flow rate of the ashing treatment is 8000-12000 sccm;
and/or the flow rate of the nitrogen in the ashing treatment is 800 sccm-1000 sccm;
and/or the ashing treatment power is 2000-4500 watts.
5. The method of cleaning a phosphoric acid etching residue according to claim 1, wherein the high-temperature sulfuric acid cleaning is performed using H 2 SO 4 And H 2 O 2 Wherein the H is a mixed solution of the components 2 SO 4 The mass fraction of (2) is 90% -98%, and/or the H is the same as that of the steel 2 O 2 The mass fraction of the (C) is 20% -40%.
6. The method for cleaning a phosphoric acid etching residue according to any one of claims 1 to 5, wherein the step of cleaning the SC1 cleaning solution further comprises a step of performing a third water-washing on the sample after the first water-washing, wherein the temperature of the third water-washing is 25 ℃ to 35 ℃;
and/or, further comprising performing a fourth water washing on the sample after the second water washing, wherein the temperature of the fourth water washing is 25-35 ℃.
7. The method of cleaning a phosphoric acid etching residue according to claim 6, wherein the third water washing time is 200s to 300s;
and/or the fourth water washing time is 200 s-300 s.
8. A method for processing a silicon wafer, comprising:
etching the silicon wafer using phosphoric acid;
the silicon wafer is cleaned by the cleaning method of the phosphoric acid etching residues according to any one of claims 1 to 7.
9. A silicon wafer obtained by the method for processing a silicon wafer according to claim 8.
10. A chip comprising the silicon wafer of claim 9.
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