CN109277359A - A kind of cleaning process of infrared lens germanium single crystal twin polishing piece - Google Patents

A kind of cleaning process of infrared lens germanium single crystal twin polishing piece Download PDF

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Publication number
CN109277359A
CN109277359A CN201811148475.XA CN201811148475A CN109277359A CN 109277359 A CN109277359 A CN 109277359A CN 201811148475 A CN201811148475 A CN 201811148475A CN 109277359 A CN109277359 A CN 109277359A
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China
Prior art keywords
cleaning
diluted
twin polishing
pure water
germanium
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CN201811148475.XA
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CN109277359B (en
Inventor
王云彪
武永超
吕菲
陈亚楠
张贺强
杨召杰
耿莉
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CETC 46 Research Institute
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CETC 46 Research Institute
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04Cleaning involving contact with liquid
    • B08B3/08Cleaning involving contact with liquid the liquid having chemical or dissolving effect
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/02Cleaning by the force of jets or sprays
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04Cleaning involving contact with liquid
    • B08B3/10Cleaning 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
    • B08B3/12Cleaning 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 kind of infrared lens cleaning processes of germanium single crystal twin polishing piece.After this technique carries out germanium wafer twin polishing using no ceroplastic, removal surface polishing liquid is impregnated using diluted hydrofluoric acid solution, surface contamination is removed using diluted remover ultrasound, surface particles are further removed using diluted ammonia spirit megasonic cleaning, reach surface free of cleaning.Present invention employs the modes that high purity detergent and HF solution combine, and cooperate ultrasonic cleaning, have effectively removed the surface contamination of twin polishing germanium wafer, reached surface requirements free of cleaning, greatly improved the infrared surface quality with twin polishing piece.Operation of the present invention is simple, is easily achieved, and reduces the cleaning difficulty of twin polishing germanium wafer, it is easy to accomplish mass production.

Description

A kind of cleaning process of infrared lens germanium single crystal twin polishing piece
Technical field
The present invention relates to semiconductor material processing technologies, more particularly to a kind of infrared lens germanium single crystal twin polishing piece Cleaning process.
Background technique
Germanium single crystal has good mechanical performance and heating conduction, its transmitted spectrum range is 2-12 μm, is widely applied In infrared optical lens and the infrared optical window of protection infrared optical lens.60% or more low and middle-end infrared optical lens For germanium single crystal manufacture, 50% or more high-end infrared optical lens are germanium single crystal manufacture.In addition, absorption of the germanium at 10.6 μm is very It is small, it is the ideal material of laser lens, window and output coupling mirror, is also act as the base material of various infrared filters.Mesh The high-end germanium single crystal polished silicon wafer of preceding country's infrared optics demand is N-type 2-6 inches of twin polishing piece, and thickness is at 300-600 microns Range.Usual producer is processed using the method for mechanical lapping, and machined surface still has mechanical stress and sub-micron damaging layer, it is difficult to Compared with world level.And the germanium wafer of CMP planarization technique processing is used to be mainly used for ultra-thin germanium substrate used for solar batteries, add Work technique and double throwing techniques are not general.In addition, otherwise the cleaning of germanium polished silicon wafer cannot will cause using conventional RCA cleaning process Surface oxidation and heavy corrosion.
In the processing of high-end germanium twin polishing piece, using the polishing mode of CPM, if thinking, surface reaches technique free of cleaning and wants It asks, monolithic cleaning process can only be used, the cleaning way removal organic contaminations and hand impregnated by using hot sulfuric acid+cold sulfuric acid Print, then remove surface contamination and particle by low temperature 1# liquid, cleaning process is cumbersome, low efficiency, safety are poor.Therefore, by changing Into cleaning process, using with process flow and common apparatus similar in IC grades of silicon polished productions, make infrared to be polished with germanium single crystal Piece surface reaches requirement free of cleaning, is of great practical significance.
Summary of the invention
In view of prior art situation, for the cleaning problem of germanium twin polishing piece, the present invention provides a kind of infrared lens use The cleaning process of germanium single crystal twin polishing piece.The polished silicon wafer surface requirements of high quality: it is fogless, without stain, without impression of the hand, it is corrosion-free, It is not more than 10 without spot, without polishing fluid, 0.3 micron of surface and the above particle.So this technique carries out germanium using no ceroplastic Piece twin polishing impregnates removal surface polishing liquid using diluted hydrofluoric acid solution after polishing, high-purity clean using diluted 101 Agent solution ultrasound removes surface contamination and impression of the hand, further removes surface particles using diluted ammonia spirit megasonic cleaning, reaches To the purpose on surface free of cleaning.
The technical solution adopted by the present invention is that: a kind of cleaning process of infrared lens germanium single crystal twin polishing piece, it is special Sign is: after carrying out germanium wafer twin polishing using no ceroplastic, impregnating removal surface polishing liquid using diluted hydrofluoric acid solution, adopts Surface contamination is removed with diluted remover ultrasound, surface particles are further removed using diluted ammonia spirit megasonic cleaning, Reach surface free of cleaning, processing step is as follows:
(1), the polished germanium wafer of one side is fitted into the PFA gaily decorated basket, 5min is impregnated in diluted hydrofluoric acid solution, is then carried out Pure water rinsing.
(2), germanium wafer is put into ultrasound 5min in diluted remover, ultrasonic temperature is controlled at 50-60 DEG C, then carried out pure Water rinses.
(3), the polished germanium wafer in the second face is impregnated into diluted hydrofluoric acid solution 5min, then carries out pure water punching It washes.
(4), germanium wafer is sequentially placed into two cups has in diluted clean agent solution, and ultrasonic temperature is controlled at 50-60 DEG C, often Cup ultrasound 5min, then has ultrasound 2min in pure water in the 3rd cup, then carry out pure water rinsing.
(5), the germanium wafer after cleaning is put into megasonic cleaning 10min in diluted ammonia spirit, cleaning temperature 20-25 DEG C, it dries, examine after spray irrigation.
The volume ratio of diluted hydrofluoric acid solution of the present invention is hydrofluoric acid: pure water=1:10, hydrofluoric acid concentration 49%.
Remover of the present invention is KILALA CLEAN101 remover, the volume ratio of the diluted clean agent solution For KILALA CLEAN101 remover: pure water=1:10.
The volume ratio of diluted ammonia spirit of the present invention is ammonium hydroxide: pure water=1:50, ammonia concn 25%.
The present invention has the advantage that is with beneficial effect: using this technique, the machine of germanium single crystal twin polishing piece may be implemented Toolization is cleaned automatically, is avoided that monolithic cleaning efficiency is low, washes sulfuric acid and is easy to happen the risk of safety accident, ensure that polished silicon wafer is clear Wash the consistency and stability of effect.Using monolithic cleaning process, 10 polished silicon wafers can only be cleaned per hour, and primary cleaning at Product rate and operator's proficiency are closely related;It is cleaned using this technique, cleaning germanium wafer 75 may be implemented per hour, efficiency mentions 7.5 times are risen, primary qualification rate of cleaning is stablized 90% or more.This improves production capacity, from seizing market for reducing production cost Share is of great significance.
Specific embodiment
The invention will be further described with reference to embodiments:
Embodiment: single germanium wafer: N-type<111>mixes antimony, resistivity are as follows: 1-40 Ω ㎝, diameter: 100mm, thickness: 500 ± 20 μ M, twin polishing.Specific implementation step is as follows:
1, it prepares cleaning solution: preparing hydrofluoric acid solution: 49% hydrofluoric acid: pure water=1:10, hydrofluoric acid concentration 49%;It is high to dilute 101 Pure remover: 101 remover of KILALA CLEAN: pure water=1:20,101 high purity detergent main component of KILALA CLEAN For diethanol amine, tetramethylphosphonihydroxide hydroxide base amine;Prepare ammonia spirit: 25% ammonium hydroxide: pure water=1:50, ammonia concn 25%.
2, twin polishing process are as follows: the front-back side-front, operator wear clean emgloves, and front is thrown for the first time After light, 5min is impregnated in a solution of hydrofluoric acid, starts polished back face after flushing.
3, the germanium wafer at the polished back side is fitted into 25 PFA gailys decorated basket, impregnates 5min in a solution of hydrofluoric acid, then into Row pure water rinsing.
4, germanium wafer is put into ultrasound 5min in diluted 101 high purity detergent solution, at 50 DEG C, then ultrasonic temperature controls Carry out pure water rinsing.
5, second of front polishing is carried out, polishing time is less than 5min, impregnates 5min after polishing in a solution of hydrofluoric acid, so After carry out pure water rinsing.
6, germanium wafer is sequentially placed into two cups has in diluted clean agent solution, and at 50 DEG C, every glass super for ultrasonic temperature control Then sound 5min has ultrasound 2min in pure water in the 3rd cup, then carries out pure water rinsing.
7, the germanium wafer after cleaning is put into megasonic cleaning 10min in ammonia spirit, cleaning temperature is 22 DEG C, after spray irrigation Drying is examined.
Technical effect is examined: germanium single crystal twin polishing piece is cleaned using this technique, is cleaned under rear surface major light and is examined nothing Mist, without stain, without impression of the hand, it is corrosion-free, without spot, without polishing fluid, 0.3 micron of surface and the above particle are primary clear less than 10 It washes yield rate and reaches 90%, the daily output reaches 1000.
The inspection result shows: this technique is used, it can be real on cleaning equipment identical with IC grade silicon polished silicon wafer The mechanization of existing germanium polished silicon wafer is cleaned automatically, and process stabilizing is high-efficient.
Present invention employs the modes that 101 high purity detergents and HF solution combine, and cooperate ultrasonic cleaning, effectively remove The surface contamination of twin polishing germanium wafer, has reached surface requirements free of cleaning, and it is double to greatly improve infrared lens germanium single crystal The surface quality of face polished silicon wafer.This technological operation is simple, is easily achieved, and reduces the cleaning difficulty of twin polishing germanium wafer, is easy to Realize mass production.

Claims (4)

1. a kind of infrared lens cleaning process of germanium single crystal twin polishing piece, it is characterized in that: carrying out germanium wafer using no ceroplastic After twin polishing, removal surface polishing liquid is impregnated using diluted hydrofluoric acid solution, table is removed using diluted remover ultrasound Face is stain, and is further removed surface particles using diluted ammonia spirit megasonic cleaning, is reached surface free of cleaning, processing step It is as follows:
(1), the polished germanium wafer of one side is fitted into the PFA gaily decorated basket, 5min is impregnated in diluted hydrofluoric acid solution, is then carried out Pure water rinsing;
(2), germanium wafer is put into ultrasound 5min in diluted remover, ultrasonic temperature is controlled at 50-60 DEG C, then carries out pure water punching It washes;
(3), the polished germanium wafer in the second face is impregnated into diluted hydrofluoric acid solution 5min, then carries out pure water rinsing;
(4), germanium wafer is sequentially placed into two cups has in diluted clean agent solution, and at 50-60 DEG C, every glass super for ultrasonic temperature control Then sound 5min has ultrasound 2min in pure water in the 3rd cup, then carries out pure water rinsing;
(5), the germanium wafer after cleaning is put into megasonic cleaning 10min in diluted ammonia spirit, cleaning temperature is 20-25 DEG C, spray Drying, inspection after leaching is rinsed.
2. the cleaning process of a kind of infrared lens germanium single crystal twin polishing piece according to claim 1, it is characterized in that: institute The volume ratio for stating diluted hydrofluoric acid solution is hydrofluoric acid: pure water=1:10, hydrofluoric acid concentration 49%.
3. the cleaning process of a kind of infrared lens germanium single crystal twin polishing piece according to claim 1, it is characterized in that: washing Net agent is 101 remover of KILALA CLEAN, and the volume ratio of the diluted clean agent solution is that KILALA CLEAN 101 is washed Net agent: pure water=1:10.
4. the cleaning process of a kind of infrared lens germanium single crystal twin polishing piece according to claim 1, it is characterized in that: institute The volume ratio for stating diluted ammonia spirit is ammonium hydroxide: pure water=1:50, ammonia concn 25%.
CN201811148475.XA 2018-09-29 2018-09-29 Cleaning process of germanium single crystal double-sided polishing sheet for infrared lens Active CN109277359B (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
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

Patent Citations (8)

* Cited by examiner, † Cited by third party
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
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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