CN116004332B - Method for cleaning adhesive on back of rough polished germanium wafer - Google Patents
Method for cleaning adhesive on back of rough polished germanium wafer Download PDFInfo
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- CN116004332B CN116004332B CN202210078324.1A CN202210078324A CN116004332B CN 116004332 B CN116004332 B CN 116004332B CN 202210078324 A CN202210078324 A CN 202210078324A CN 116004332 B CN116004332 B CN 116004332B
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- 238000004140 cleaning Methods 0.000 title claims abstract description 116
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000000853 adhesive Substances 0.000 title claims description 21
- 230000001070 adhesive effect Effects 0.000 title claims description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 95
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 92
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 14
- 239000007921 spray Substances 0.000 claims description 14
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 12
- 239000012498 ultrapure water Substances 0.000 claims description 12
- 230000005587 bubbling Effects 0.000 claims description 11
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 6
- 238000011010 flushing procedure Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- XTOQOJJNGPEPMM-UHFFFAOYSA-N o-(2-oxo-1,3,2$l^{5}-dioxaphosphinan-2-yl)hydroxylamine Chemical compound NOP1(=O)OCCCO1 XTOQOJJNGPEPMM-UHFFFAOYSA-N 0.000 claims 1
- 235000012431 wafers Nutrition 0.000 abstract description 78
- 229920000297 Rayon Polymers 0.000 abstract description 15
- 239000007788 liquid Substances 0.000 abstract description 13
- 230000007797 corrosion Effects 0.000 abstract description 9
- 238000005260 corrosion Methods 0.000 abstract description 9
- 229910052732 germanium Inorganic materials 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 5
- 238000003763 carbonization Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 239000004065 semiconductor Substances 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 11
- 229910052799 carbon Inorganic materials 0.000 description 11
- 238000005507 spraying Methods 0.000 description 11
- 230000007547 defect Effects 0.000 description 6
- 238000005498 polishing Methods 0.000 description 5
- FDGBQHCDMSYZRC-UHFFFAOYSA-N 2-hydroxy-2-oxo-1,3,2$l^{5}-dioxaphosphinan-4-amine Chemical compound NC1CCOP(O)(=O)O1 FDGBQHCDMSYZRC-UHFFFAOYSA-N 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 229920002120 photoresistant polymer Polymers 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- -1 amino trimethyl phosphate Chemical compound 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000007517 polishing process Methods 0.000 description 2
- IEDVJHCEMCRBQM-UHFFFAOYSA-N trimethoprim Chemical compound COC1=C(OC)C(OC)=CC(CC=2C(=NC(N)=NC=2)N)=C1 IEDVJHCEMCRBQM-UHFFFAOYSA-N 0.000 description 2
- 229960001082 trimethoprim Drugs 0.000 description 2
- AOJJSUZBOXZQNB-VTZDEGQISA-N 4'-epidoxorubicin Chemical compound O([C@H]1C[C@@](O)(CC=2C(O)=C3C(=O)C=4C=CC=C(C=4C(=O)C3=C(O)C=21)OC)C(=O)CO)[C@H]1C[C@H](N)[C@@H](O)[C@H](C)O1 AOJJSUZBOXZQNB-VTZDEGQISA-N 0.000 description 1
- 229920000715 Mucilage Polymers 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- SEOVTRFCIGRIMH-UHFFFAOYSA-N indole-3-acetic acid Chemical compound C1=CC=C2C(CC(=O)O)=CNC2=C1 SEOVTRFCIGRIMH-UHFFFAOYSA-N 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- 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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- Cleaning Or Drying Semiconductors (AREA)
Abstract
The invention relates to a cleaning process for viscose on the back of a rough polished germanium wafer, which belongs to the technical field of semiconductor materials, and specifically comprises the steps of cleaning by using degumming liquid and then cleaning by using concentrated sulfuric acid with different concentrations, wherein the degumming liquid comprises the following components in percentage by volume: the cleaning process of the invention comprises the steps of firstly adopting degumming liquid for cleaning, then using concentrated sulfuric acid for carbonization cleaning, and has the characteristics of thorough removal of viscose on the back surface of the wafer, simple operation, high production efficiency and capability of reducing corrosion of acid liquor on the surface of the rough polished germanium wafer, and the invention realizes the mass, high-efficiency and stable production of (2-6) inch rough polished germanium wafers, which is an important process in the production process of high-end germanium wafers.
Description
Technical Field
The invention relates to a method for cleaning viscose on the back of a rough polished germanium wafer, and belongs to the technical field of semiconductor materials.
Background
The high-purity germanium single crystal has the characteristics of high radiation resistance, high frequency and good photoelectric performance, is widely applied to high-tech fields such as energy sources, photoelectricity, national defense military, aerospace, modern information industry and the like, and the germanium substrate compound semiconductor laminated battery has the advantages of high efficiency, high voltage, good high temperature characteristics and the like, the highest conversion efficiency of the grown III-V compound thin film solar battery of the germanium substrate reaches 35% -36.7%, the highest light concentration reaches 40% -44.6%, and is the substrate material with the highest current efficiency, and the high-purity germanium single crystal can be developed rapidly in a quite long period in the future.
In the rough polishing process of the high-end germanium wafer, the time is generally longer and reaches 50-60 minutes, and damage can be caused to the back surface of the germanium wafer, including but not limited to the defects of scratches, specks and the like; therefore, before rough polishing of the germanium wafer, a film needs to be adhered to the back surface of the germanium wafer to avoid damage to the back surface of the germanium wafer in the rough polishing process, but after the rough polishing is finished, the solidified adhesive on the back surface of the wafer needs to be removed. In order not to affect the subsequent cleaning of the germanium wafer, to meet the standards of open-box and ready-to-use, the back-side cured glue needs to be removed before the germanium wafer is finally cleaned. In the prior art, after the film is uncovered, concentrated sulfuric acid is directly used for cleaning and degumming, but aiming at partial products of the company, after the wafer is chamfered, the viscose at the chamfer position is not thoroughly removed, the viscose at the back of the wafer can be furthest removed only by increasing the cleaning time of the concentrated sulfuric acid, but the defects of oxidation corrosion, rough surface and the like can be generated on the front of the wafer by increasing the cleaning time of the concentrated sulfuric acid.
Disclosure of Invention
In view of the prior art, the invention provides a method for cleaning the back side adhesive of a rough polished germanium wafer, which aims at the problem of the back side adhesive of the rough polished germanium wafer.
In order to achieve the above object, the present invention provides the following technical solutions:
the degumming liquid for cleaning the viscose on the back of the rough polished germanium wafer comprises the following components in percentage by volume: 50-90% of aminotrimethylene phosphate, 1-10% of perchloric acid, 1-5% of EDTA-2Na and the balance of pure water.
The invention selects the amino trimethyl phosphate as the main viscose dissolving agent, so that part of viscose on the germanium wafer can be quickly and effectively dissolved; EDTA-2Na is added as an accelerator, and 2 carboxyl groups H + in the EDTA-2Na are transferred to amino N in an aqueous solution to form bipolar ions, so that the EDTA-2Na has wide coordination performance, almost forms stable chelate with all metal ions, promotes the dissolution of viscose and simultaneously removes pollutants such as greasy dirt, dust, oxide layers, metal impurity ions and the like; the invention obtains the degumming liquid proportion through a large number of experiments, and can effectively remove the mucilage on the germanium wafer.
Further, the invention provides a method for cleaning the back adhesive of a rough polished germanium wafer, which comprises the following steps:
(1) Placing the roughly polished and torn germanium wafer into the degumming liquid of claim 1 at 40-60 ℃ to be cleaned for 10-300s, and washing with pure water for 10-60s to be dried;
(2) After the cleaning (1) is finished, the mixture is quickly put into sulfuric acid with the temperature of 35-75 ℃ to be cleaned for 10-280s;
(3) After the cleaning (2) is finished, the mixture is quickly put into sulfuric acid with the temperature of 15-45 ℃ for cleaning for 10-260s;
(4) After the washing (3) is finished, the washing is performed by pure water.
Preferably, in the step (4), the specific step of pure water flushing is as follows:
s1, after sulfuric acid cleaning, rapidly placing the wafer into an overflow tank filled with pure water, and sequentially performing rapid discharge and spray cleaning for 10-240S, and spray washing the wafer for 10-200S;
S2: and S1, after cleaning, rapidly placing the water into a new overflow tank filled with pure water, sequentially performing rapid drainage, spray cleaning for 10-250S, spray cleaning for 10-350S, water injection, bubbling cleaning for 10-200S, and finally rapidly draining and spin-drying.
The quick drainage means that the water in the overflow groove is drained quickly after the wafer is immersed in the overflow groove filled with water, and the main purpose is to dilute and take away the residual concentrated sulfuric acid on the surface of the wafer at the fastest speed, so as to prevent the concentrated sulfuric acid from generating uneven and excessive corrosion on the surface of the wafer; the purpose of the bubbling flush is to increase the activity of metal ions and impurity particles attached to the wafer surface in water, so that the impurities are stained and fall off under the strong bubble flushing.
Preferably, the sulfuric acid used in step (2) and step (3) is UP grade.
Preferably, the pure water is ultrapure water, the resistivity is more than or equal to 18.25 omega-m, the total organic carbon TOC in the water is less than 100, and the water temperature is 10-20 ℃.
Preferably, the water pressure of the spraying is 0.1-1.5MPa, and the rapid drainage rate is 0.1-3L/s.
Preferably, in the step S2, nitrogen is introduced into the bottom of the overflow tank for bubbling, and the flow rate of the nitrogen is 0.2-5L/S.
The cleaning process of the invention firstly adopts degumming liquid for cleaning, and then uses concentrated sulfuric acid for carbonization cleaning, has the characteristics of thorough removal of viscose on the back surface of the wafer, simple operation, high production efficiency and capability of reducing corrosion of acid liquor on the surface of the rough polished germanium wafer, realizes batch, efficient and stable production of (2-6) inch rough polished germanium wafers, and is a process with important significance in the production process of high-end germanium wafers.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a view showing that the front surface of a wafer is subjected to oxidation corrosion and has rough surface defects which are amplified by 50 times by directly adopting concentrated sulfuric acid for cleaning, wherein (a) is the front surface of the wafer close to the edge position and (b) is the front surface central position of the wafer;
FIG. 3 is a view showing the wafer backside wafer with 50-fold enlarged scale of incomplete wafer backside photoresist removal for reducing the acid cleaning time by directly using concentrated sulfuric acid, wherein (a), (b), and (c) are wafer backside edge positions and (d) is wafer backside center position;
FIG. 4 is a view showing the effect of the adhesive cleaning on the back surface of a rough polished germanium wafer of the present invention, which is enlarged 50 times, wherein (a) is the edge position of the back surface of the wafer and (b) is the center position of the back surface of the wafer.
Detailed Description
The present invention will be described in further detail with reference to specific examples, wherein the chemical reagents used in the present invention, as specifically described, are all chemically pure and commercially available, and the apparatus used in steps (4) and (5) in all examples is the cleaning apparatus described in patent 202123342641X.
Example 1
The back side adhesive of the 6-inch rough polished germanium wafer is cleaned, and as shown in fig. 1, the cleaning process is as follows:
(1) Placing the germanium wafer after rough polishing and film tearing into degumming liquid (comprising 70% of aminotrimethylene phosphate, 5% of perchloric acid, 5% of EDTA-2Na 4% and the balance of pure water in percentage by volume) at 50 ℃ for cleaning for 80-150 s, continuously floating up and down and rotating left and right in the degumming liquid in the cleaning process, taking out, and cleaning for 10-60s by using pure water for spin-drying;
(2) After the cleaning (1) is finished, the wafer is quickly put into sulfuric acid at 40 ℃, the sulfuric acid is of UP level and has 96 percent of concentration, the cleaning time is 120-180 seconds, and the wafer is continuously floated UP and down and rotated left and right in the sulfuric acid in the cleaning process;
(3) After the cleaning (2) is finished, the wafer is quickly put into sulfuric acid at 25 ℃, the sulfuric acid is of UP level and has the concentration of 96 percent, the wafer is cleaned for 100 to 150 seconds, and the wafer is continuously floated UP and down and rotated left and right in the sulfuric acid in the cleaning process;
(4) After the cleaning (3) is finished, the wafer is quickly placed into an overflow tank 1 filled with water to be sequentially subjected to quick discharge and spray cleaning for 10-240s, the wafer is sprayed and washed for 10-200s, the resistivity of ultrapure water is more than or equal to 18.25 Ω & m, the total organic carbon TOC in the water is less than 100, the water temperature is 10-20 ℃, the water pressure of spraying is 0.1-1.5MPa, and the quick water discharge rate is 0.1-3L/s;
(5) And (3) after the cleaning (4) is finished, the water is quickly placed into an overflow tank 2 filled with water to be quickly discharged, sprayed and cleaned for 10-250s, sprayed, watered and cleaned for 10-350s, watered and cleaned for 10-200s, the resistivity of the ultrapure water used is more than or equal to 18.25 Ω & m, the total organic carbon TOC in the water is less than 100, the spraying water pressure is 0.1-1.5MPa, the quick water discharge rate is 0.1-3L/s, the nitrogen bubbling flow is 0.2-5L/s, and finally the water is quickly discharged and dried.
The apparatus used in the above steps (4) and (5) is a cleaning apparatus described in patent 202123342641X.
Example 2
The back adhesive of the 6-inch rough polished germanium wafer is cleaned, and the cleaning process is as follows:
(1) Placing the roughly polished and torn germanium wafer into a degumming solution (comprising 90% of aminotrimethylene phosphate, 1% of perchloric acid, 1% of EDTA-2Na and the balance of pure water in percentage by volume) at 60 ℃ to be cleaned for 150-250 s, continuously floating up and down and rotating left and right in the degumming solution during the cleaning process, taking out, and cleaning with pure water for 10-60s to spin-dry;
(2) Putting the wafer into sulfuric acid with the temperature of 75 ℃ after the cleaning (1) is finished, wherein the sulfuric acid is of UP level and the concentration is 96%, the cleaning time is 10-15 s, and the wafer is continuously floated UP and down and rotated left and right in the sulfuric acid in the cleaning process;
(3) After the cleaning (2) is finished, the wafer is quickly put into sulfuric acid with the temperature of 30 ℃, the sulfuric acid is of UP level and the concentration is 96 percent, the wafer is cleaned for 50 to 100 seconds, and the wafer is continuously floated UP and down and rotated left and right in the sulfuric acid in the cleaning process;
(4) After the cleaning (3) is finished, the wafer is quickly placed into an overflow tank 1 filled with water to be sequentially subjected to quick discharge and spray cleaning for 10-240s, the wafer is sprayed and washed for 10-200s, the resistivity of ultrapure water is more than or equal to 18.25 Ω & m, the total organic carbon TOC in the water is less than 100, the water temperature is 10-20 ℃, the water pressure of spraying is 0.1-1.5MPa, and the quick water discharge rate is 0.1-3L/s;
(5) And (3) after the cleaning (4) is finished, the water is quickly placed into an overflow tank 2 filled with water to be quickly discharged, sprayed and cleaned for 10-250s, sprayed, watered and cleaned for 10-350s, watered and cleaned for 10-200s, the resistivity of the ultrapure water used is more than or equal to 18.25 Ω & m, the total organic carbon TOC in the water is less than 100, the spraying water pressure is 0.1-1.5MPa, the quick water discharge rate is 0.1-3L/s, the nitrogen bubbling flow is 0.2-5L/s, and finally the water is quickly discharged and dried.
The apparatus used in the above steps (4) and (5) is a cleaning apparatus described in patent 202123342641X.
Example 3
The back adhesive of the 6-inch rough polished germanium wafer is cleaned, and the cleaning process is as follows:
(1) Placing the roughly polished and torn germanium wafer into a degumming solution (comprising 50% of aminotrimethylene phosphate, 10% of perchloric acid, 5% of EDTA-2Na and the balance of pure water in percentage by volume) at 60 ℃ for cleaning for 200-300 s, continuously floating up and down and rotating left and right in the degumming solution during the cleaning process, taking out, and cleaning for 10-60s by using pure water for spin-drying;
(2) After the cleaning (1) is finished, the wafer is quickly put into sulfuric acid at 35 ℃, the sulfuric acid is of UP level and has the concentration of 96 percent, the cleaning time is 200-280 s, and the wafer is continuously floated UP and down and rotated left and right in the sulfuric acid in the cleaning process;
(3) After the cleaning (2) is finished, the wafer is quickly put into sulfuric acid at 45 ℃, the sulfuric acid is of UP level and the concentration is 96 percent, the wafer is cleaned for 10 to 100 seconds, and the wafer is continuously floated UP and down and rotated left and right in the sulfuric acid in the cleaning process;
(4) After the cleaning (3) is finished, the wafer is quickly placed into an overflow tank 1 filled with water to be sequentially subjected to quick discharge and spray cleaning for 10-240s, the wafer is sprayed and washed for 10-200s, the resistivity of ultrapure water is more than or equal to 18.25 Ω & m, the total organic carbon TOC in the water is less than 100, the water temperature is 10-20 ℃, the water pressure of spraying is 0.1-1.5MPa, and the quick water discharge rate is 0.1-3L/s;
(5) And (3) after the cleaning (4) is finished, the water is quickly placed into an overflow tank 2 filled with water to be quickly discharged, sprayed and cleaned for 10-250s, sprayed, watered and cleaned for 10-350s, watered and cleaned for 10-200s, the resistivity of the ultrapure water used is more than or equal to 18.25 Ω & m, the total organic carbon TOC in the water is less than 100, the spraying water pressure is 0.1-1.5MPa, the quick water discharge rate is 0.1-3L/s, the nitrogen bubbling flow is 0.2-5L/s, and finally the water is quickly discharged and dried.
Example 4
The back adhesive of the 6-inch rough polished germanium wafer is cleaned, and the cleaning process is as follows:
(1) Placing the roughly polished and torn germanium wafer into a degumming liquid (comprising 80% of amino trimethoprim acid, 6% of perchloric acid, 4% of EDTA-2Na and the balance of pure water in percentage by volume) at 40 ℃ for cleaning for 10-100 s, continuously floating up and down in the degumming liquid and rotating left and right in the cleaning process, taking out, and cleaning with pure water for 10-60s for spin-drying;
(2) After the cleaning (1) is finished, the wafer is quickly put into sulfuric acid at 40 ℃, the sulfuric acid is of UP level and has 96 percent of concentration, the cleaning time is 120-180 seconds, and the wafer is continuously floated UP and down and rotated left and right in the sulfuric acid in the cleaning process;
(3) After the cleaning (2) is finished, the wafer is quickly put into sulfuric acid at 25 ℃, the sulfuric acid is of UP level and has the concentration of 96 percent, the wafer is cleaned for 100 to 150 seconds, and the wafer is continuously floated UP and down and rotated left and right in the sulfuric acid in the cleaning process;
(4) After the cleaning (3) is finished, the wafer is quickly placed into an overflow tank 1 filled with water to be sequentially subjected to quick discharge and spray cleaning for 10-240s, the wafer is sprayed and washed for 10-200s, the resistivity of ultrapure water is more than or equal to 18.25 Ω & m, the total organic carbon TOC in the water is less than 100, the water temperature is 10-20 ℃, the water pressure of spraying is 0.1-1.5MPa, and the quick water discharge rate is 0.1-3L/s;
(5) And (3) after the cleaning (4) is finished, the water is quickly placed into an overflow tank 2 filled with water to be quickly discharged, sprayed and cleaned for 10-250s, sprayed, watered and cleaned for 10-350s, watered and cleaned for 10-200s, the resistivity of the ultrapure water used is more than or equal to 18.25 Ω & m, the total organic carbon TOC in the water is less than 100, the water pressure of the spraying is 0.1-1.5MPa, the quick water discharge rate is 0.1-3L/s, the nitrogen bubbling flow is 0.2-5L/s, and finally the water is quickly discharged and dried.
Example 5
The back adhesive of the 6-inch rough polished germanium wafer is cleaned, and the cleaning process is as follows:
(1) Placing the germanium wafer after rough polishing and film tearing into degumming liquid (comprising 80% of amino trimethoprim acid, 8% of perchloric acid, 3% of EDTA-2Na and the balance of pure water in percentage by volume) at 45 ℃ for cleaning for 10-100 s, continuously floating up and down in the degumming liquid and rotating left and right in the cleaning process, taking out, and cleaning with pure water for 10-60s for spin-drying;
(2) After the cleaning (1) is finished, the wafer is quickly put into sulfuric acid with the temperature of 50 ℃, the sulfuric acid is of UP level and the concentration is 96 percent, the cleaning time is 100-150 s, and the wafer is continuously floated UP and down and rotated left and right in the sulfuric acid in the cleaning process;
(3) After the cleaning (2) is finished, the wafer is quickly put into sulfuric acid at 15 ℃, the sulfuric acid is of UP level and the concentration is 96 percent, the wafer is cleaned for 1050-260 seconds, and the wafer is continuously floated UP and down and rotated left and right in the sulfuric acid in the cleaning process;
(4) After the cleaning (3) is finished, the wafer is quickly placed into an overflow tank 1 filled with water to be sequentially subjected to quick discharge and spray cleaning for 10-240s, the wafer is sprayed and washed for 10-200s, the resistivity of ultrapure water is more than or equal to 18.25 Ω & m, the total organic carbon TOC in the water is less than 100, the water temperature is 10-20 ℃, the water pressure of spraying is 0.1-1.5MPa, and the quick water discharge rate is 0.1-3L/s;
(5) And (3) after the cleaning (4) is finished, the water is quickly placed into an overflow tank 2 filled with water to be quickly discharged, sprayed and cleaned for 10-250s, sprayed, watered and cleaned for 10-350s, watered and cleaned for 10-200s, the resistivity of the ultrapure water used is more than or equal to 18.25 Ω & m, the total organic carbon TOC in the water is less than 100, the water pressure of the spraying is 0.1-1.5MPa, the quick water discharge rate is 0.1-3L/s, the nitrogen bubbling flow is 0.2-5L/s, and finally the water is quickly discharged and dried.
Aiming at partial products of the company, after direct use of concentrated sulfuric acid for cleaning experiments, the viscose is found to be difficult to remove at the positions of wafer chamfer and gap, so that the viscose is firstly subjected to preliminary cleaning by adopting a degumming agent, a large amount of viscose is washed off, then concentrated sulfuric acid is used for further carbonization cleaning, the intractable viscose on the back surface of the wafer and in the gap of the chamfer can be effectively removed from the experimental surface, fine carbonized substances are adhered to the wafer chamfer and gap after carbonization cleaning of the concentrated sulfuric acid, and therefore bubbling cleaning is adopted, so that the activity of carbide adhered to the surface of the wafer is increased, and the carbide is dropped.
Specifically, concentrated sulfuric acid is directly used for cleaning, the concentrated sulfuric acid cleaning time is increased to remove the viscose on the back surface of the wafer to the greatest extent, but the concentrated sulfuric acid cleaning time is increased, the front surface of the wafer can generate defects of oxidation corrosion, rough surface and the like, and the pure concentrated sulfuric acid cleaning in the embodiment 1 is adopted as shown in fig. 2 (a) and (b): in the figure, the bright spots are peracid corrosion spots, polishing stress of the wafer, defects of the wafer, and the like can cause inconsistent corrosion rate of the wafer in acid liquor, and the wafer is characterized by rough surface.
Further, as shown in fig. 3 (a) and (b), the wafer back edge adhesive is not cleaned, concentrated sulfuric acid is directly used for cleaning, defects such as oxidation corrosion and rough surface are generated on the front surface, the acid cleaning time is shortened, but the wafer back adhesive is not thoroughly removed, as shown in fig. 3 (c) and (d), the wafer back edge adhesive is not cleaned, the adhesive is carbonized, but the adhesive in the gap close to the edge is not carbonized, so that the adhesive is not dropped, and the adhesive in the center of the wafer back is not cleaned.
The wafer photoresist rinse with the rough polish germanium cleaned in example 1 was as follows: as shown in fig. 4 (a) and (b), the wafer is cleaned by photoresist removal at the edge and center of the back surface, respectively, and it can be seen from the figure that the photoresist is thoroughly removed from the edge and center of the wafer cleaned by concentrated sulfuric acid.
Claims (1)
1. The method for cleaning the adhesive on the back of the rough polished germanium wafer is characterized by comprising the following steps of:
(1) Placing the roughly polished and torn germanium wafer into a degumming solution at 40-60 ℃ for cleaning for 10-300s, washing with pure water for 10-60s, and spin-drying, wherein the degumming solution contains 50-90% of amino trimethylene phosphate, 1-10% of perchloric acid, 1-5% of EDTA-2Na and the balance of pure water in percentage by volume;
(2) After the cleaning (1) is finished, the mixture is quickly put into sulfuric acid with the temperature of 35-75 ℃ to be cleaned for 10-280s;
(3) After the cleaning (2) is finished, the mixture is quickly put into sulfuric acid with the temperature of 15-45 ℃ for cleaning for 10-260s;
(4) After the cleaning (3) is finished, pure water is used for flushing;
The specific steps of pure water flushing are as follows:
s1, after sulfuric acid cleaning, rapidly placing the wafer into an overflow tank filled with pure water, and sequentially performing rapid discharge and spray cleaning for 10-240S, and spray washing the wafer for 10-200S;
S2: s1, after cleaning, rapidly placing the water into a new overflow tank filled with pure water, sequentially performing rapid drainage, spray cleaning for 10-250S, spray cleaning for 10-350S, water injection, bubbling cleaning for 10-200S, and finally rapidly draining and spin-drying;
The sulfuric acid used in the step (2) and the step (3) is of UP grade, and the concentration is 95% -99%;
The pure water is ultrapure water, the resistivity is more than or equal to 18.25 omega-m, the TOC of total organic matters in the water is less than 100, and the water temperature is 10-20 ℃;
the water pressure of the spray is 0.1-1.5MPa, and the rapid drainage rate is 0.1-3L/s;
in the step S2, nitrogen is introduced into the bottom of the overflow tank for bubbling, and the flow rate of the nitrogen is 0.2-5L/S.
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