CN109277359B - Cleaning process of germanium single crystal double-sided polishing sheet for infrared lens - Google Patents
Cleaning process of germanium single crystal double-sided polishing sheet for infrared lens Download PDFInfo
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- CN109277359B CN109277359B CN201811148475.XA CN201811148475A CN109277359B CN 109277359 B CN109277359 B CN 109277359B CN 201811148475 A CN201811148475 A CN 201811148475A CN 109277359 B CN109277359 B CN 109277359B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/02—Cleaning by the force of jets or sprays
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Cleaning Or Drying Semiconductors (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a cleaning process of a germanium single crystal double-sided polishing sheet for an infrared lens. The process adopts a wax-free process to polish the two sides of the germanium sheet, uses a diluted hydrofluoric acid solution to soak and remove surface polishing solution, uses a diluted detergent to remove surface contamination by ultrasonic, and uses a diluted ammonia solution to perform megasonic cleaning to further remove surface particles, thereby achieving the purpose of cleaning-free surface. The invention adopts the mode of combining the high-purity cleaning agent and the HF solution and is matched with ultrasonic cleaning, so that the surface contamination of the double-sided polished germanium sheet is effectively removed, the cleaning-free surface requirement is met, and the surface quality of the infrared double-sided polished sheet is greatly improved. The method is simple to operate and easy to realize, reduces the cleaning difficulty of the double-sided polished germanium sheet, and is easy to realize batch production.
Description
Technical Field
The invention relates to a semiconductor material processing technology, in particular to a cleaning process of a germanium single crystal double-sided polishing sheet for an infrared lens.
Background
The germanium single crystal has good mechanical property and heat conduction property, has a transmission spectrum range of 2-12 mu m, and is widely applied to infrared optical lenses and infrared optical windows for protecting the infrared optical lenses. More than 60% of the middle-low end infrared optical lenses are made of germanium single crystals, and more than 50% of the high end infrared optical lenses are made of germanium single crystals. In addition, germanium has a small absorption at 10.6 μm, is an ideal material for laser lenses, windows, and output coupling mirrors, and is also used as a base material for various infrared filters. The high-end germanium single crystal polished wafer which meets the domestic infrared optical requirement at present is an N-type 2-6 inch double-sided polished wafer, and the thickness of the polished wafer is within the range of 300-600 microns. Generally, manufacturers adopt a mechanical grinding method to process, mechanical stress and submicron damaged layers still exist on a processing surface, and the processing surface is difficult to compare with the international level. The germanium sheet processed by the CMP polishing process is mainly used for the ultrathin germanium substrate for the solar cell, and the processing process and the double polishing process are not universal. In addition, germanium polishing pad cleaning cannot employ conventional RCA cleaning processes, which would otherwise cause surface oxidation and severe corrosion.
In the processing of a high-end germanium double-sided polishing sheet, a CPM polishing mode is adopted, if the surface meets the requirement of a cleaning-free process, only a single-sheet cleaning process can be adopted, organic contamination and fingerprints are removed by adopting a cleaning mode of soaking in hot sulfuric acid and cold sulfuric acid, and then surface contamination and particles are removed by low-temperature No. 1 liquid, so that the cleaning process is complicated, the efficiency is low, and the safety is poor. Therefore, by improving the cleaning process and adopting the process flow and the general equipment which are similar to those of the IC-grade silicon polished wafer, the surface of the infrared germanium single crystal polished wafer can meet the cleaning-free requirement, and the method has very important practical significance.
Disclosure of Invention
In view of the prior art, the invention provides a cleaning process of a germanium single crystal double-sided polishing sheet for an infrared lens, aiming at the problem of cleaning the germanium double-sided polishing sheet. High quality polished wafer surface requirements: has no fog, contamination, fingerprint, corrosion, spot and polishing liquid, and has surface size of 0.3 μm or more and no more than 10 particles. The process adopts a wax-free process to polish the two sides of the germanium sheet, uses a diluted hydrofluoric acid solution to soak and remove surface polishing solution after polishing, uses a diluted 101 high-purity detergent solution to remove surface stains and fingerprints by ultrasonic, and uses a diluted ammonia solution to perform megasonic cleaning to further remove surface particles, thereby achieving the purpose of cleaning-free surface.
The technical scheme adopted by the invention is as follows: a cleaning process of a germanium single crystal double-sided polishing sheet for an infrared lens is characterized by comprising the following steps: after the double-sided polishing of the germanium sheet is carried out by adopting a wax-free process, a diluted hydrofluoric acid solution is adopted for soaking to remove surface polishing solution, a diluted detergent is adopted for ultrasonically removing surface contamination, and diluted ammonia water solution is adopted for megasonic cleaning to further remove surface particles, so that a cleaning-free surface is achieved, and the process comprises the following steps:
(1) and putting the germanium sheet with one polished surface into a PFA flower basket, soaking in a diluted hydrofluoric acid solution for 5min, and then washing with pure water.
(2) And putting the germanium sheet into a diluted cleaning agent, performing ultrasonic treatment for 5min, controlling the ultrasonic temperature at 50-60 ℃, and then performing pure water washing.
(3) And soaking the germanium sheet with the polished second surface in a diluted hydrofluoric acid solution for 5min, and then washing with pure water.
(4) Sequentially putting the germanium sheet into two cups of diluted detergent solution, controlling the ultrasonic temperature at 50-60 ℃, carrying out ultrasonic treatment for 5min in each cup, then carrying out ultrasonic treatment for 2min in pure water in the 3 rd cup, and then carrying out pure water washing.
(5) And putting the cleaned germanium wafer into a diluted ammonia water solution for megasonic cleaning for 10min, wherein the cleaning temperature is 20-25 ℃, and carrying out spin-drying and inspection after spray rinsing.
The volume ratio of the diluted hydrofluoric acid solution is hydrofluoric acid: pure water =1:10, hydrofluoric acid concentration 49%.
The detergent of the invention is KILALA CLEAN101 detergent, the volume ratio of the diluted detergent solution is KILALA CLEAN101 detergent: pure water =1: 10.
The volume ratio of the diluted ammonia water solution is ammonia water: pure water =1:50, ammonia concentration 25%.
The invention has the advantages and beneficial effects that: by adopting the process, the mechanical automatic cleaning of the germanium single crystal double-sided polished wafer can be realized, the risks of low single wafer cleaning efficiency and safety accidents caused by sulfuric acid cleaning are avoided, and the consistency and stability of the cleaning effect of the polished wafer are ensured. A single-chip cleaning process is adopted, only 10 polished wafers can be cleaned per hour, and the one-time cleaning yield is closely related to the proficiency of operators; by adopting the process for cleaning, 75 germanium wafers can be cleaned every hour, the efficiency is improved by 7.5 times, and the once cleaning qualified rate is stabilized to be more than 90%. The method has important significance for reducing the production cost and improving the productivity and seizing the market share.
Detailed Description
The invention is further illustrated by the following examples:
example (b): a germanium single crystal wafer: antimony doped N-type <111>, resistivity: 1-40 Ω · cm, diameter: 100mm, thickness: 500 +/-20 microns, and double-side polishing. The specific implementation steps are as follows:
1. preparing a cleaning solution: preparing a hydrofluoric acid solution: 49% hydrofluoric acid: pure water =1:10, hydrofluoric acid concentration 49%; dilution 101 high-purity detergent: KILALA CLEAN101 detergent, pure water =1:20, KILALA CLEAN101 high-purity detergent, mainly comprising diethanolamine, and tetramethylammonium hydroxide; preparing an ammonia solution: 25% ammonia water: pure water =1:50, ammonia concentration 25%.
2. The double-side polishing process comprises the following steps: front-back-front, the operator wears clean latex gloves, after the first front polishing, the operator soaks in hydrofluoric acid solution for 5min, and starts to polish the back after washing.
3. The polished back germanium sheet was loaded into a 25-piece PFA basket, soaked in hydrofluoric acid solution for 5min, and then rinsed with pure water.
4. Putting the germanium sheet into a diluted 101 high-purity detergent solution, performing ultrasonic treatment for 5min, controlling the ultrasonic temperature at 50 ℃, and then performing pure water washing.
5. And carrying out secondary front polishing for less than 5min, soaking in hydrofluoric acid solution for 5min after polishing, and then washing with pure water.
6. Putting the germanium sheet into two cups of diluted detergent solution in sequence, controlling the ultrasonic temperature at 50 ℃, performing ultrasonic treatment for 5min in each cup, performing ultrasonic treatment for 2min in the 3 rd cup of pure water, and washing with pure water.
7. And (3) putting the cleaned germanium wafer into an ammonia water solution, carrying out megasonic cleaning for 10min at the cleaning temperature of 22 ℃, carrying out spray rinsing, spin-drying and inspecting.
And (3) technical effect inspection: the germanium single crystal double-sided polished wafer is cleaned by the process, after cleaning, the surface is free of fog, contamination, fingerprints, corrosion, spots and polishing solution under a strong light inspection, the number of particles on the surface is less than 10, the number of particles is 0.3 micrometer and more, the one-time cleaning yield reaches 90%, and the daily yield reaches 1000 wafers.
The test results show that: by adopting the process, the mechanical automatic cleaning of the germanium polished wafer can be realized on the same cleaning equipment as the IC-grade silicon single crystal polished wafer, the process is stable, and the efficiency is high.
The invention adopts a mode of combining the 101 high-purity cleaning agent and the HF solution, and is matched with ultrasonic cleaning, so that the surface contamination of the double-sided polished germanium sheet is effectively removed, the cleaning-free surface requirement is met, and the surface quality of the germanium single crystal double-sided polished sheet for the infrared lens is greatly improved. The process is simple to operate and easy to realize, reduces the cleaning difficulty of the double-sided polished germanium sheet, and is easy to realize batch production.
Claims (1)
1. A cleaning process of a germanium single crystal double-sided polishing sheet for an infrared lens is characterized by comprising the following steps: after the double-sided polishing of the germanium sheet is carried out by adopting a wax-free process, a diluted hydrofluoric acid solution is adopted for soaking to remove surface polishing solution, a diluted detergent is adopted for ultrasonically removing surface contamination, and diluted ammonia water solution is adopted for megasonic cleaning to further remove surface particles, so that a cleaning-free surface is achieved, and the process comprises the following steps:
(1) placing the germanium sheet with one polished surface into a PFA flower basket, soaking in a diluted hydrofluoric acid solution for 5min, and then washing with pure water;
(2) putting the germanium sheet into a diluted cleaning agent, performing ultrasonic treatment for 5min, controlling the ultrasonic temperature at 50-60 ℃, and then performing pure water washing;
(3) soaking the polished germanium sheet on the second surface in a diluted hydrofluoric acid solution for 5min, and then washing with pure water;
(4) sequentially putting the germanium sheet into two cups of diluted detergent solution, controlling the ultrasonic temperature at 50-60 ℃, carrying out ultrasonic treatment for 5min in each cup, then carrying out ultrasonic treatment for 2min in 3 rd cup of pure water, and then carrying out pure water washing;
(5) putting the cleaned germanium wafer into a diluted ammonia water solution, cleaning for 10min at 20-25 ℃ with megasonic, drying after spray rinsing, and inspecting;
the volume ratio of the diluted hydrofluoric acid solution is hydrofluoric acid: pure water =1:10, hydrofluoric acid concentration 49%;
the cleaning agent is KILALA CLEAN101 cleaning agent, KILALA CLEAN101 cleaning agent is diethanolamine, and tetramethylammonium hydroxide;
the volume ratio of the diluted detergent solution was KILALA CLEAN101 detergent: pure water =1: 10;
the volume ratio of the diluted ammonia solution is ammonia: pure water =1:50, ammonia concentration 25%.
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| CN201811148475.XA CN109277359B (en) | 2018-09-29 | 2018-09-29 | Cleaning process of germanium single crystal double-sided polishing sheet for infrared lens |
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| CN201811148475.XA CN109277359B (en) | 2018-09-29 | 2018-09-29 | Cleaning process of germanium single crystal double-sided polishing sheet for infrared lens |
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| CN109277359B true CN109277359B (en) | 2021-08-31 |
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| CN103343060A (en) * | 2013-07-17 | 2013-10-09 | 常熟奥首光电材料有限公司 | Sapphire substrate wafer cleaning solution as well as preparation method, application and cleaning method thereof |
| JP5606180B2 (en) * | 2010-06-30 | 2014-10-15 | Ｈｏｙａ株式会社 | Measuring method of silica fine particles |
| CN104377119A (en) * | 2014-10-23 | 2015-02-25 | 中国电子科技集团公司第四十六研究所 | Method for cleaning germanium single crystal polished wafer |
| CN106057645A (en) * | 2016-06-20 | 2016-10-26 | 云南中科鑫圆晶体材料有限公司 | Cleaning method for germanium single crystal polished wafer |
| CN107470266A (en) * | 2017-09-25 | 2017-12-15 | 北京半导体专用设备研究所（中国电子科技集团公司第四十五研究所） | The rear cleaning method of oxide wafer in a kind of CMP process |
| CN108010833A (en) * | 2017-12-01 | 2018-05-08 | 山东理工大学 | For the mixed acid of diode cleaning, production method, diode cleaning method |
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2018
- 2018-09-29 CN CN201811148475.XA patent/CN109277359B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5606180B2 (en) * | 2010-06-30 | 2014-10-15 | Ｈｏｙａ株式会社 | Measuring method of silica fine particles |
| CN102179390A (en) * | 2010-11-25 | 2011-09-14 | 西安北方捷瑞光电科技有限公司 | Method for cleaning ultra-smooth surface |
| CN103029026A (en) * | 2012-12-13 | 2013-04-10 | 天津中环领先材料技术有限公司 | Monocrystalline silicon wafer cleaning method with ultrahigh cleaning capacity |
| CN103343060A (en) * | 2013-07-17 | 2013-10-09 | 常熟奥首光电材料有限公司 | Sapphire substrate wafer cleaning solution as well as preparation method, application and cleaning method thereof |
| CN104377119A (en) * | 2014-10-23 | 2015-02-25 | 中国电子科技集团公司第四十六研究所 | Method for cleaning germanium single crystal polished wafer |
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| CN107470266A (en) * | 2017-09-25 | 2017-12-15 | 北京半导体专用设备研究所（中国电子科技集团公司第四十五研究所） | The rear cleaning method of oxide wafer in a kind of CMP process |
| CN108010833A (en) * | 2017-12-01 | 2018-05-08 | 山东理工大学 | For the mixed acid of diode cleaning, production method, diode cleaning method |
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