CN103537453A - Method for ultrasonic cleaning of polished sapphire substrate wafer - Google Patents
Method for ultrasonic cleaning of polished sapphire substrate wafer Download PDFInfo
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- 238000004506 ultrasonic cleaning Methods 0.000 title claims abstract description 72
- 239000000758 substrate Substances 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 38
- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 28
- 239000010980 sapphire Substances 0.000 title claims abstract description 28
- 238000004140 cleaning Methods 0.000 claims abstract description 87
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 40
- 230000003647 oxidation Effects 0.000 claims abstract description 38
- 239000004094 surface-active agent Substances 0.000 claims abstract description 23
- 239000002738 chelating agent Substances 0.000 claims abstract description 21
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 15
- 239000010432 diamond Substances 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims description 43
- MUJOIMFVNIBMKC-UHFFFAOYSA-N fludioxonil Chemical compound C=12OC(F)(F)OC2=CC=CC=1C1=CNC=C1C#N MUJOIMFVNIBMKC-UHFFFAOYSA-N 0.000 claims description 32
- 239000012530 fluid Substances 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 239000008367 deionised water Substances 0.000 claims description 26
- 229910021641 deionized water Inorganic materials 0.000 claims description 26
- 238000005498 polishing Methods 0.000 claims description 23
- -1 alkyl alcohol ethers Chemical group 0.000 claims description 20
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 14
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 12
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 12
- 229910052737 gold Inorganic materials 0.000 claims description 12
- 239000010931 gold Substances 0.000 claims description 12
- 125000005233 alkylalcohol group Chemical group 0.000 claims description 7
- 239000004480 active ingredient Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 4
- 239000012498 ultrapure water Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 abstract description 14
- 239000012535 impurity Substances 0.000 abstract description 8
- 239000002184 metal Substances 0.000 abstract description 7
- 229910052751 metal Inorganic materials 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 6
- 229910021645 metal ion Inorganic materials 0.000 abstract description 6
- 239000007788 liquid Substances 0.000 abstract description 5
- 238000004377 microelectronic Methods 0.000 abstract description 3
- 238000005868 electrolysis reaction Methods 0.000 abstract description 2
- 238000002604 ultrasonography Methods 0.000 abstract 2
- 239000000243 solution Substances 0.000 description 33
- 239000002253 acid Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 229910002601 GaN Inorganic materials 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000005416 organic matter Substances 0.000 description 5
- 235000011180 diphosphates Nutrition 0.000 description 4
- 238000003912 environmental pollution Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 230000002000 scavenging effect Effects 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000006061 abrasive grain Substances 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
The invention relates to a method for ultrasonic cleaning of a polished sapphire substrate wafer and provides a method for conducting cleaning through ultrasound and a solution to remove particles and metal ions and then conducting cleaning through ultrasound and oxidation liquid to remove organic matters. According to removal of the particles and the metal ions, an FA/O type chelating agent and two kinds of non-ionic surface active agents including JFC and AEO are selected and prepared to mixed liquid in proportion and the ultrasonic action is added so that cleaning can be conducted; anodic oxidation liquid obtained through electrolysis of a diamond film (BDD) is selected to remove organic pollution, the oxidation liquid is high in oxidation function, and therefore most organic matters are resolved. According to the method, comprehensive cleaning of the particles, the organic matters and metal impurities is conducted, the number of steps is small, operation is simple, and the method can satisfy the requirement of the new-period micro-electronic cleaning technology.
Description
Technical field
The clean technology that the invention belongs to wafer surface after CMP, relates in particular to the ultrasonic cleaning method after a kind of Sapphire Substrate wafer polishing.
Background technology
As the GaN of the third generation semi-conducting material after Si, GaAs, become undoubtedly the milestone in LED chip manufacturing industry development process, greatly develop at present gallium nitride based LED luminescent material become into year over trend and the emphasis of Lighting Industry development.Because GaN is difficult to prepare body material, must be on other backing material growing film, therefore, for the manufacture of the LED chip of GaN base, the selection of substrate is the factor of overriding concern.The backing material of GaN has multiple, comprises sapphire, carborundum, silicon, magnesia, zinc oxide etc., and in numerous materials, saphire substrate material becomes the preferred material of cost and technological feasibility.Along with the proposition again of energy-saving and emission-reduction and green energy resource, as the sapphire wafer of making luminescent device substrate, be processed into the focus of people's research at present.
Sapphire Substrate wafer material is to be converted into smooth LED reverse mounting type by initial alundum (Al2O3) particle, in whole process through long crystalline substance, draw rod, section, annealing, grinding, polishing etc. tens procedures, every processing through an operation, Sapphire Substrate wafer has all carried out time processing pollution, therefore after each procedure of Sapphire Substrate wafer material, need to clean, and the wash result of every step all directly affects the difficulty of next step manufacturing procedure, affect the raising of product quality.Especially the surface of polished clean technology as one of process for treating surface is even more important.After at present Sapphire Substrate batch production, wafer surface energy is high, surface tension is large, residual polishing fluid skewness, stain the phenomenons such as metal ion and residual grains and all occur.Thereby reduced the yield rate of Sapphire Substrate wafer, and then affected the processing of subsequent device.
After chemically mechanical polishing, the pollution on sapphire wafer surface mainly contains several large pollutions such as residual polishing fluid, abrasive grain and other particle, organic matter and metal ion pollution, so the cleaning after sapphire substrate material polishing is generally undertaken by above three major types.
The cleaning method of Sapphire Substrate has much at present, as traditional RCA cleaning, ultrasonic cleaning, million sound cleanings, mechanical scrub and rotary spray cleaning, plasma clean, laser beam clean etc.Development for Cleaning Technique so far, but being conventionally applicable to industrial or traditional solution soaks to clean, general step is many, consume chemicals and deionized water also many, and the use of strong acid, highly basic, strong oxidizer is operational hazards not only, and volatilely cause environmental pollution, and operating personnel's actual bodily harm etc.
Chinese patent publication No. CN102632055A, date of publication on August 15th, 2012, name is called a kind of cleaning method of Sapphire Substrate, this application case discloses a kind of cleaning method of Sapphire Substrate, saphire substrate material mega sonic wave in the organic solvent of electronic pure after cleaning except organic impurities, inorganic metal impurity is cleaned, with electronic grade ultrapure water, clean, with the mixed liquor that ammoniacal liquor, hydrogen peroxide, water form, clean, with strong acid, clean.Its weak point is, consumes chemicals and deionized water is many in cleaning method used, and the use of strong acid operational hazards and volatilely cause environmental pollution not only.
Summary of the invention
The object of the invention is in order to solve existing sapphire cleaning technique step many, consume chemicals and deionized water many, and the use of strong acid, highly basic, strong oxidizer is operational hazards not only, and volatilely cause environmental pollution, and the defect of operating personnel's actual bodily harm and a kind of use of avoiding strong acid and strong base is provided, reduced environmental pollution, the ultrasonic cleaning method after the high Sapphire Substrate wafer polishing of cleaning efficiency.
To achieve these goals, the present invention is by the following technical solutions:
A ultrasonic cleaning method after Sapphire Substrate wafer polishing, described ultrasonic cleaning method comprises the following steps:
A), at 45-55 ℃, the saphire substrate material after polishing is immersed to be equipped with in the supersonic cleaning machine that mixes cleaning fluid and carry out ultrasonic cleaning, time 10-20min, ultrasonic power 1.5-2kw, frequency 35-50 KHz, then carries out twice ultrasonic cleaning with the frequency of 80-100KHz, time 5-10min; After twice ultrasonic cleans, standing 5-10min, then carry out ultrasonic cleaning for the third time, time 2-5min with the frequency of 35-50KHz; Wherein, mixing cleaning fluid is formulated by chelating agent and surfactant;
B) under room temperature, by the saphire substrate material deionized water rinsing after step a) ultrasonic cleaning, time 5-10min;
C) saphire substrate material after step b) cleaning is immersed in the ultrasonic cleaning that oxidation solution is housed and carries out ultrasonic cleaning, temperature is 60-80 ℃, time 10-20min, ultrasonic power 2-2.5kw, frequency 70-90KHz, then with the frequency of 30-40 KHz, carry out twice ultrasonic cleaning, time 5-10min; After twice ultrasonic cleans, standing 5-10min, then carry out ultrasonic cleaning for the third time, time 2-5min with the frequency of 35-50KHz; Wherein, the active ingredient in oxidation solution is the strong oxidation solution of anode of electrolyzing gold diamond film gained;
D) under room temperature, with deionized water rinsing step c) saphire substrate material after ultrasonic cleaning, time 5-10min;
E) saphire substrate material after step d) cleaning is immersed in the supersonic cleaning machine that deionized water is housed and carries out overflow ultrasonic cleaning, temperature is 30-50 ℃, time 10-20min, ultrasonic power 1.5-2kw, frequency 75-105KHz;
F) saphire substrate material after step e) cleaning is dried, dried up.
In the technical program, adopt the strong oxidation solution of electrolysis gained to carry out organic removal, oxidation solution is the strong oxidation solution of anode of electrolyzing gold diamond film gained, principle is for to add inorganic electrolyte at anode electrolytic tank,, because the overpotential for oxygen evolution of diamond film is very high, on anode, can there is oxidation reaction and generate pyrophosphate peroxide in phosphate, the oxidisability of solution is strengthened greatly, is mainly peroxide pyrophosphate ion (P
2o
8 4-) oxidation-reduction potential be 2.07V, and Organic Pollution oxidizing potential is generally in about 1.2 ~ 2V, so most organic pollutants can be broken down into carbon dioxide and water.Electrochemical oxidation liquid not only can effectively be removed surperficial organic contamination, and can effectively remove the organic contaminations such as carbon that the non-ionic surface active agent that cleaned by the first step is introduced, this oxidation solution also has certain effect to the removal of metal impurities, this is because the pyrophosphate that is reduced into of pyrophosphate peroxide has very strong complexing power, it can with the complexing of metal ion such as copper; Ultrasonic+Aqueous Solution Cleaning Technology is removed particle, metal impurities, then removes organic matter with oxidation solution, can complete the comprehensive cleaning to particle, organic matter and metal impurities, and step is few, simple to operate, meets the requirement of new period microelectronics cleaning technique.
The present invention uses the repeated ultrasonic that upper frequency is combined with lower frequency to clean, and improves cleaning performance and cleaning efficiency.
As preferably, in step a), chelating agent shared volume fraction in mixing cleaning fluid is 1 ~ 2%, and surfactant shared volume fraction in mixing cleaning fluid is 1 ~ 1.5 ‰, and solvent is deionized water.In the technical program, surfactant can not add too much, too much has a large amount of foams and occurs, is unfavorable for so on the contrary cleaning, therefore surfactant shared volume fraction in cleaning fluid is 1 ~ 1.5 ‰; Chelating agent is mainly to remove metal ion, therefore chelating agent shared volume fraction in cleaning fluid is 1 ~ 2%.
As preferably, in step c) oxidation solution used, the volume fraction of the strong oxidation solution of anode of electrolyzing gold diamond film gained is 50-70%.
As preferably, surfactant used is mixed by two kinds of AEO and the secondary alkyl alcohol ethers of polyoxyethylene, and AEO is 1:1-3 with the mass ratio of the polyoxyethylene alkyl alcohol ether second month in a season.In the technical program; AEO is non-ionic surface active agent; the secondary alkyl alcohol ether of polyoxyethylene is bleeding agent; this surfactant can be very soon under ultrasonic effect and is passed through easily osmosis; particle and wafer surface are resolved, and form fine and close diaphragm by wetting action, prevent that particle from adsorbing again; and this surfactant can make in cleaning fluid chelating agent more even to the microcorrosion effect of material surface, has reduced surface roughness.
As preferably, chelating agent is commercially available FA/O type chelating agent.
As preferably, deionized water is electronic grade ultrapure water.
The invention has the beneficial effects as follows:
1) the present invention adopts oxidation solution to carry out organic removal, oxidation solution is the strong oxidation solution of anode of electrolyzing gold diamond film gained, principle is for to add inorganic electrolyte at anode electrolytic tank, phosphate, because the overpotential for oxygen evolution of diamond film is very high, on anode, can there is oxidation reaction and generate pyrophosphate peroxide, the oxidisability of solution is strengthened greatly;
2) activating agent that in the present invention, the removal of particle is used is non-ionic surface active agent, particle and wafer surface are resolved, and form fine and close diaphragm by wetting action, prevent that particle from adsorbing again, make in cleaning fluid chelating agent more even to the microcorrosion effect of material surface, reduced surface roughness;
3) the present invention first removes particle, metal impurities with ultrasonic cleaning and Aqueous Solution Cleaning Technology, with oxidation solution, remove organic matter again, can complete the comprehensive cleaning to particle, organic matter and metal impurities, step is few, simple to operate, meet the requirement of new period microelectronics cleaning technique;
4) in cleaning method cleaning fluid provided by the present invention containing strong acid and highly basic composition, environmental protection, pollution-free, to technical operation personnel also without harm, clean rear surface stolen goods dirt quantity lower than requirement in the industry 300 in, meet or exceed and require in the industry level; Cleaning efficiency is higher, can reach more than 98%, has saved scavenging period, has also removed the use of cleaning equipment from, has improved suitability for industrialized production ability and has reduced production cost.
The specific embodiment
Below, by specific embodiment, the present invention will be further explained:
The present invention's chelating agent used is commercially available FA/O type chelating agent; The secondary alkyl alcohol ether of polyoxyethylene is commercially available product, model JFC; AEO is commercially available product, model AEO; Deionized water is electronic grade ultrapure water.
Embodiment 1
A ultrasonic cleaning method after Sapphire Substrate wafer polishing, described ultrasonic cleaning method comprises the following steps:
A), at 45 ℃, the saphire substrate material after polishing is immersed to be equipped with in the supersonic cleaning machine that mixes cleaning fluid and carry out ultrasonic cleaning, time 10min, ultrasonic power 1.5kw, frequency 50 KHz, then carry out twice ultrasonic cleaning with the frequency of 100KHz, time 10min; After twice ultrasonic cleans, standing 10min, then carry out ultrasonic cleaning for the third time, time 5min with the frequency of 35KHz; Wherein, mixing cleaning fluid is formulated by FA/O type chelating agent and surfactant; FA/O type chelating agent shared volume fraction in mixing cleaning fluid is 1%, and surfactant shared volume fraction in mixing cleaning fluid is 1 ‰, and solvent is deionized water; Surfactant used is mixed by two kinds of the secondary alkyl alcohol ethers of AEO and polyoxyethylene, and AEO is 1:1 with the mass ratio of the polyoxyethylene alkyl alcohol ether second month in a season;
B) under room temperature, by the saphire substrate material deionized water rinsing after step a) ultrasonic cleaning, time 5min;
C) saphire substrate material after step b) cleaning is immersed in the ultrasonic cleaning that oxidation solution is housed and carries out ultrasonic cleaning, temperature is 60 ℃, time 15min, ultrasonic power 1.5kw, frequency 100KHz, then carries out twice ultrasonic cleaning with the frequency of 45KHz, time 10min; After twice ultrasonic cleans, standing 10min, then carry out ultrasonic cleaning for the third time, time 5min with the frequency of 35KHz; Wherein, the active ingredient in oxidation solution is the strong oxidation solution of anode of electrolyzing gold diamond film gained; In oxidation solution used, the volume fraction of the strong oxidation solution of anode of electrolyzing gold diamond film gained is 50%.
D) under room temperature, with deionized water rinsing step c) saphire substrate material after ultrasonic cleaning, time 5min;
E) saphire substrate material after step d) cleaning is immersed in the supersonic cleaning machine that deionized water is housed and carries out overflow ultrasonic cleaning, temperature is 30 ℃, time 10min, ultrasonic power 1.5kw, frequency 100KHz;
F) saphire substrate material after step e) cleaning is dried, dried up.
Embodiment 2
A ultrasonic cleaning method after Sapphire Substrate wafer polishing, described ultrasonic cleaning method comprises the following steps:
A), at 50 ℃, the saphire substrate material after polishing is immersed to be equipped with in the supersonic cleaning machine that mixes cleaning fluid and carry out ultrasonic cleaning, time 12min, ultrasonic power 1.8kw, frequency 40 KHz, then carry out twice ultrasonic cleaning with the frequency of 90KHz, time 8min; After twice ultrasonic cleans, standing 8min, then carry out ultrasonic cleaning for the third time, time 3min with the frequency of 45KHz; Wherein, mixing cleaning fluid is formulated by FA/O type chelating agent and surfactant; FA/O type chelating agent shared volume fraction in mixing cleaning fluid is 1.5%, and surfactant shared volume fraction in mixing cleaning fluid is 1.2 ‰, and solvent is deionized water; Surfactant used is mixed by two kinds of the secondary alkyl alcohol ethers of AEO and polyoxyethylene, and AEO is 1:2 with the mass ratio of the polyoxyethylene alkyl alcohol ether second month in a season;
B) under room temperature, by the saphire substrate material deionized water rinsing after step a) ultrasonic cleaning, time 8min;
C) saphire substrate material after step b) cleaning is immersed in the ultrasonic cleaning that oxidation solution is housed and carries out ultrasonic cleaning, temperature is 70 ℃, time 15min, ultrasonic power 2.3kw, frequency 80KHz, then carries out twice ultrasonic cleaning with the frequency of 35KHz, time 8min; After twice ultrasonic cleans, standing 8min, then carry out ultrasonic cleaning for the third time, time 3min with the frequency of 45KHz; Wherein, the active ingredient in oxidation solution is the strong oxidation solution of anode of electrolyzing gold diamond film gained; In oxidation solution used, the volume fraction of the strong oxidation solution of anode of electrolyzing gold diamond film gained is 60%
D) under room temperature, with deionized water rinsing step c) saphire substrate material after ultrasonic cleaning, time 8min;
E) saphire substrate material after step d) cleaning is immersed in the supersonic cleaning machine that deionized water is housed and carries out overflow ultrasonic cleaning, temperature is 40 ℃, time 15min, ultrasonic power 1.8kw, frequency 95KHz;
F) saphire substrate material after step e) cleaning is dried, dried up.
Embodiment 3
A ultrasonic cleaning method after Sapphire Substrate wafer polishing, described ultrasonic cleaning method comprises the following steps:
A) at 55 ℃, the saphire substrate material after polishing is immersed to be equipped with in the supersonic cleaning machine that mixes cleaning fluid and carry out ultrasonic cleaning, time 20min, ultrasonic power 2kw, frequency 35KHz, then carries out twice ultrasonic cleaning with the frequency of 80 KHz, time 5min; After twice ultrasonic cleans, standing 5min, then carry out ultrasonic cleaning for the third time, time 2min with the frequency of 50KHz; Wherein, mixing cleaning fluid is formulated by FA/O type chelating agent and surfactant; FA/O type chelating agent shared volume fraction in mixing cleaning fluid is 2%, and surfactant shared volume fraction in mixing cleaning fluid is 1.5 ‰, and solvent is deionized water; Surfactant used is mixed by two kinds of the secondary alkyl alcohol ethers of AEO and polyoxyethylene, and AEO is 1:3 with the mass ratio of the polyoxyethylene alkyl alcohol ether second month in a season;
B) under room temperature, by the saphire substrate material deionized water rinsing after step a) ultrasonic cleaning, time 10min;
C) saphire substrate material after step b) cleaning is immersed in the ultrasonic cleaning that oxidation solution is housed and carries out ultrasonic cleaning, temperature is 80 ℃, time 10min, ultrasonic power 2kw, frequency 80KHz, then carries out twice ultrasonic cleaning with the frequency of 30 KHz, time 5min; After twice ultrasonic cleans, standing 5min, then carry out ultrasonic cleaning for the third time, time 2min with the frequency of 50KHz; Wherein, the active ingredient in oxidation solution is the strong oxidation solution of anode of electrolyzing gold diamond film gained; In oxidation solution used, the volume fraction of the strong oxidation solution of anode of electrolyzing gold diamond film gained is 70%;
D) under room temperature, with deionized water rinsing step c) saphire substrate material after ultrasonic cleaning, time 10min;
E) saphire substrate material after step d) cleaning is immersed in the supersonic cleaning machine that deionized water is housed and carries out overflow ultrasonic cleaning, temperature is 50 ℃, time 20min, ultrasonic power 2kw, frequency 105KHz;
F) saphire substrate material after step e) cleaning is dried, dried up.
By cleaning method of the present invention, the difficulty of cleaning is reduced, and the effect of cleaning significantly increase; Cleaning fluid composition is gentle, and the surface roughness after therefore cleaning is low, can reach below 0.2nm, without corrosion figure, occurs; And in cleaning fluid containing strong acid and highly basic composition, environmental protection, pollution-free, to technical operation personnel also without harm, clean rear surface stolen goods dirt quantity lower than requirement in the industry 300 in, meet or exceed and require in the industry level; Cleaning efficiency is higher, can reach more than 98%, has saved scavenging period, has also removed the use of cleaning equipment from, has improved suitability for industrialized production ability and has reduced production cost.
Claims (6)
1. the ultrasonic cleaning method after Sapphire Substrate wafer polishing, is characterized in that, described ultrasonic cleaning method comprises the following steps:
A), at 45-55 ℃, the saphire substrate material after polishing is immersed to be equipped with in the supersonic cleaning machine that mixes cleaning fluid and carry out ultrasonic cleaning, time 10-20min, ultrasonic power 1.5-2kw, frequency 35-50 KHz, then carries out twice ultrasonic cleaning with the frequency of 80-100KHz, time 5-10min; After twice ultrasonic cleans, standing 5-10min, then carry out ultrasonic cleaning for the third time, time 2-5min with the frequency of 35-50KHz; Wherein, mixing cleaning fluid is formulated by chelating agent and surfactant;
B) under room temperature, by the saphire substrate material deionized water rinsing after step a) ultrasonic cleaning, time 5-10min;
C) saphire substrate material after step b) cleaning is immersed in the ultrasonic cleaning that oxidation solution is housed and carries out ultrasonic cleaning, temperature is 60-80 ℃, time 10-20min, ultrasonic power 2-2.5kw, frequency 70-90KHz, then with the frequency of 30-40 KHz, carry out twice ultrasonic cleaning, time 5-10min; After twice ultrasonic cleans, standing 5-10min, then carry out ultrasonic cleaning for the third time, time 2-5min with the frequency of 35-50KHz; Wherein, the active ingredient in oxidation solution is the strong oxidation solution of anode of electrolyzing gold diamond film gained;
D) under room temperature, with deionized water rinsing step c) saphire substrate material after ultrasonic cleaning, time 5-10min;
E) saphire substrate material after step d) cleaning is immersed in the supersonic cleaning machine that deionized water is housed and carries out overflow ultrasonic cleaning, temperature is 30-50 ℃, time 10-20min, ultrasonic power 1.5-2kw, frequency 75-105KHz;
F) saphire substrate material after step e) cleaning is dried, dried up.
2. the ultrasonic cleaning method after a kind of Sapphire Substrate wafer polishing according to claim 1, it is characterized in that, in step a), chelating agent shared volume fraction in mixing cleaning fluid is 1 ~ 2%, surfactant shared volume fraction in mixing cleaning fluid is 1 ~ 1.5 ‰, and solvent is deionized water.
3. the ultrasonic cleaning method after a kind of Sapphire Substrate wafer polishing according to claim 1, is characterized in that, in step c) oxidation solution used, the volume fraction of the strong oxidation solution of anode of electrolyzing gold diamond film gained is 50-70%.
4. the ultrasonic cleaning method after a kind of Sapphire Substrate wafer polishing according to claim 1 and 2, it is characterized in that, surfactant used is mixed by two kinds of the secondary alkyl alcohol ethers of AEO and polyoxyethylene, and AEO is 1:1-3 with the mass ratio of the polyoxyethylene alkyl alcohol ether second month in a season.
5. the ultrasonic cleaning method after a kind of Sapphire Substrate wafer polishing according to claim 1 and 2, is characterized in that, chelating agent is commercially available FA/O type chelating agent.
6. according to the ultrasonic cleaning method after a kind of Sapphire Substrate wafer polishing described in claim 1 or 2 or 3, it is characterized in that, deionized water is electronic grade ultrapure water.
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| CN105903694A (en) * | 2016-04-27 | 2016-08-31 | 上海超硅半导体有限公司 | Cleaning method and back-side defect reworking method for large-size sapphire substrate before annealing |
| US9812371B2 (en) | 2015-03-24 | 2017-11-07 | Soitec | Methods for reducing metal contamination on a surface of a sapphire substrate by plasma treatment |
| CN107717640A (en) * | 2016-08-10 | 2018-02-23 | 云南民族大学 | A kind of method of ultrasonic assistant grinding and polishing |
| CN109755106A (en) * | 2019-01-11 | 2019-05-14 | 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） | A kind of method for cleaning wafer |
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| CN104259132A (en) * | 2014-07-29 | 2015-01-07 | 蓝思科技股份有限公司 | Technology for cleaning sapphire wafer |
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| CN112871849A (en) * | 2020-12-29 | 2021-06-01 | 北京天科合达半导体股份有限公司 | Cleaning method for removing particles on surface of silicon carbide wafer |
| WO2023202192A1 (en) * | 2022-04-19 | 2023-10-26 | 天通控股股份有限公司 | Method for cleaning single-side-polished lithium niobate wafer |
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