CN103521474B - Method for cleaning surfaces of sapphire substrate materials by using polishing to replace washing - Google Patents
Method for cleaning surfaces of sapphire substrate materials by using polishing to replace washing Download PDFInfo
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- CN103521474B CN103521474B CN201310362887.4A CN201310362887A CN103521474B CN 103521474 B CN103521474 B CN 103521474B CN 201310362887 A CN201310362887 A CN 201310362887A CN 103521474 B CN103521474 B CN 103521474B
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- polishing
- cleaning
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- cleaning method
- surface cleaning
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02082—Cleaning product to be cleaned
-
- 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
-
- 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
Abstract
The invention relates to a method for cleaning surfaces of sapphire substrate materials by using polishing to replace washing. Firstly, oxidation liquid is added for cleaning organic matter, then mixed cleaning liquid of active agents and chelating agents are added for removing particles and metal ions, and finally deionized water is added for conducting cleaning. According to the method, the cleaning liquid does not contain strong acid and strong base components, is environmentally friendly and free of pollution, and has no harm to technical operators; after cleaning is finished, the quantity of dirt on the surfaces is lower than 300 required by the industry and reaches or exceeds the required level in the industry; cleaning efficiency is high and can reach more than 98%, cleaning time is saved, cleaning equipment is prevented from being used, industrial production capacity is enhanced, and production cost is reduced.
Description
Technical field
The invention belongs to the clean technology of wafer surface after CMP, particularly relate to a kind of to throw the saphire substrate material surface cleaning method that generation washes.
Background technology
As the GaN of the third generation semi-conducting material after Si, GaAs, become the milestone in LED chip manufacturing industry development process undoubtedly, greatly developing gallium nitride based LED luminescent material at present has become the trend and emphasis that develop into the Lighting Industry over year.Because GaN is difficult to prepare body material, must 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, and comprise sapphire, carborundum, silicon, magnesia, zinc oxide etc., in numerous material, saphire substrate material becomes the preferred material of cost and technological feasibility.At present along with the proposition again of energy-saving and emission-reduction and green energy resource, be processed into the focus of people's research as the sapphire wafer making luminescent device substrate.
Sapphire substrate wafer material is converted into smooth LED reverse mounting type by initial alundum (Al2O3) particle, in whole process through long crystalline substance, draw tens procedures such as rod, section, annealing, grinding, polishing, often through the processing of an operation, sapphire substrate wafer has all carried out time processing pollution, need to clean after each procedure of therefore sapphire substrate wafer material, and the wash result often walked 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 current Sapphire Substrate batch production, wafer surface energy is high, surface tension large, remaining slurry skewness, phenomenon such as contamination metal ion and residual grains etc. all occur.Thus reduce the yield rate of sapphire substrate wafer, and then affect the processing of subsequent device.
After chemically mechanical polishing, the pollution of Sapphire wafer surface mainly contains several large pollutions such as remaining slurry, 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 current Sapphire Substrate has a lot, as traditional RCA cleaning, ultrasonic cleaning, million sound cleanings, mechanical scrub and rotary spray cleaning, plasma clean, laser beam cleaning etc.Development for Cleaning Technique so far, but be usually applicable to industrial or conventional solution soak and clean, general step is many, consume chemicals and deionized water also many, and the use of strong acid, highly basic, strong oxidizer not only operational hazards, and volatilely cause environmental pollution, and operating personnel's health is damaged.
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, clean through removing mega sonic wave in the organic solvent of the saphire substrate material after organic impurities, the cleaning of inorganic metal impurity at electronic pure, with electronic grade ultrapure water cleaning, with the mixed liquor cleaning of ammoniacal liquor, hydrogen peroxide, water composition, clean with strong acid.Its weak point is, consumes chemicals and deionized water is many in cleaning method used, and the use of strong acid not only operational hazards and volatilely cause environmental pollution.
Summary of the invention
The object of the invention is to solve existing sapphire cleaning technique step many; consume chemicals and deionized water many; and the use of strong acid, highly basic, strong oxidizer not only operational hazards; and volatilely cause environmental pollution, and the defect that operating personnel's health is damaged and a kind of environmental protection is provided, reduce costs, protect operating personnel to throw the saphire substrate material surface cleaning method that generation washes.
To achieve these goals, the present invention is by the following technical solutions:
To throw the saphire substrate material surface cleaning method for washing, described surface cleaning method comprises the following steps:
A) saphire substrate material is after polishing process terminates polishing, oxidation solution is passed into polishing machine and carries out second polishing, and pressure is 0.05-0.1MPa, flow 500-700mL/min, and polishing time is 120-150s; Active ingredient in described oxidation solution is the anode Strong oxdiative liquid of electrolyzing gold diamond film gained;
B) again the cleaning fluid that chelating agent becomes with surfactant formulatory is passed into polishing machine and carry out polishing again, pressure is 0.05-0.1MPa, and flow is 500-700mL/min, and polishing time is 120-150s;
C) finally pass into deionized water and carry out water throwing, pressure is 0.04-0.06MPa, and flow is 900-1200mL/min, time 120-180s;
D) saphire substrate material cleaned is taken out in polishing machine, in drier, pass into nitrogen dry, dry up.
In the technical program, after a polish the polishing fluid that passes into is stopped, changing to and pass into oxidation solution and cleaning fluid, change the cleaning that corresponding pressure, rotating speed and oxidation solution and cleaning fluid flow can carry out sapphire wafer after polishing simultaneously.Mainly because if abrasive concentration during sapphire wafer polishing is higher, after polishing, polishing fluid is residual serious, and clean again after shelving the long period after polishing, polishing fluid abrasive material and polishing fluid component residue can be caused in wafer surface, and the form being converted into chemisorbed by physical absorption is adsorbed on surface, cleaning difficulty is increased.It should be noted that polishing fluid the pipeline that leads to and oxidation solution or cleaning fluid the pipeline that leads to separate, independently to use.
Pass into oxidation solution cleaning organic matter, pass into mixing cleaning fluid removal particle and metal ion that activating agent adds chelating agent again, because surfactant is a kind of organic solvent, and concentration is lower in cleaning fluid, therefore in the dynamic cleaning process of polishing, dissolve completely, new organic contamination can't be caused to Sapphire wafer surface.Rely on the contact of wafer and polishing cloth, apply pressure, rotating speed carrys out spin friction, rely on the strong oxidation of oxidation solution in cleaning fluid simultaneously, the infiltration of surfactant, soak the effect of grade, and the complexing of metal ion effect of chelating agent, respectively oxidation operation can be decomposed, particle parsing and remaining slurry are departed from from surface, metal ion-chelant becomes water-soluble chelate products, these reacted products all can be thrown out along with the rotary course of ramming head and polishing disk, reach the object of cleaning, improve cleaning efficiency, also improve sapphire substrate wafer surface quality.
As preferably, in step a) oxidation solution used, the volume fraction of the anode Strong oxdiative liquid of electrolyzing gold diamond film gained is 10-20%.In the technical program, the active ingredient of oxidation solution is the anode Strong oxdiative liquid of electrolyzing gold diamond film gained, inorganic phosphate is added at anode electrolytic tank in electrolytic process, anode can occur oxidation reaction and generate pyrophosphate peroxide, the oxidisability of solution is strengthened greatly, make most organic pollutants can be broken down into carbon dioxide and water, the removal of this oxidation solution to metal impurities also has certain effect, this is because the pyrophosphate that pyrophosphate peroxide is reduced into has very strong complexing power, it can with the complexing of metal ion such as copper, can timely along with the process rotated be thrown out after organic substance decomposing in cleaning process, avoid causing secondary pollution.
As preferably, in step b), chelating agent shared volume fraction in cleaning fluid is 1-1.5 ‰, and surfactant shared volume fraction in cleaning fluid is 1.5-2 ‰, and solvent is deionized water.In the technical program, surfactant can not add too much, too much has a large amount of foam and occurs, be unfavorable for cleaning so on the contrary, therefore surfactant shared volume fraction in cleaning fluid is 1.5-2 ‰; Chelating agent mainly removes metal ion, because be flowing cleaning in polishing process, does not need to add too much, therefore chelating agent shared volume fraction in cleaning fluid is 1-1.5 ‰.
As preferably, surfactant is AEO.In the technical program; AEO is non-ionic surface active agent; can be very fast in polishing process be uniformly distributed in wafer surface; and can osmosis be easily passed through; particle and wafer surface are resolved, and forms fine and close diaphragm by wetting action, prevent particle from again adsorbing; and this surfactant can make chelating agent in cleaning fluid more even to the microcorrosion effect of material surface, reduces 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 first passes into oxidation solution cleaning organic matter, then passes into the mixing cleaning fluid that activating agent adds chelating agent and remove particle and metal ion, improves cleaning efficiency, also improves sapphire substrate wafer surface quality;
2) the present invention passes into deionized water and cleans, and fully combine the action effect of mechanical scrub and deionized water rinsing, wherein deionized water is electronic grade ultrapure water, and can remove product after cleaning further, avoid polluting, cleaning efficiency significantly improves;
3) in cleaning method cleaning fluid provided by the present invention not containing strong acid and highly basic composition, environmental protection, pollution-free, to technical operation personnel also without endangering, cleaning the dirty quantity in rear surface lower than within require in the industry 300, meeting or exceeding and require level in the industry; Cleaning efficiency is higher, can reach more than 98%, has saved scavenging period, also eliminates the use of cleaning equipment, improves suitability for industrialized production ability and reduces production cost.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further explained:
The present invention's chelating agent used is commercially available FA/O type chelating agent; Surfactant is commercially available nonionic surface active agent;
Embodiment 1
To throw the saphire substrate material surface cleaning method for washing, described surface cleaning method comprises the following steps:
A) saphire substrate material is after polishing process terminates polishing, oxidation solution is passed into polishing machine and carries out second polishing, and pressure is 0.05MPa, flow 500mL/min, and polishing time is 150s; Active ingredient in described oxidation solution is the anode Strong oxdiative liquid of electrolyzing gold diamond film gained, and the volume fraction of anode Strong oxdiative liquid in oxidation solution is 10%;
B) again the cleaning fluid that FA/O type chelating agent and nonionic surface active agent AEO are mixed with is passed into polishing machine and carry out polishing again, pressure is 0.05MPa, and flow is 500mL/min, and polishing time is 150s; FA/O type chelating agent shared volume fraction in cleaning fluid is 1 ‰, and nonionic surface active agent AEO shared volume fraction in cleaning fluid is 1.5 ‰;
C) finally pass into deionized water and carry out water throwing, pressure is 0.04MPa, and flow is 900mL/min, time 150s;
D) saphire substrate material cleaned is taken out in polishing machine, in drier, pass into nitrogen dry, dry up.
Embodiment 2
To throw the saphire substrate material surface cleaning method for washing, described surface cleaning method comprises the following steps:
A) saphire substrate material is after polishing process terminates polishing, oxidation solution is passed into polishing machine and carries out second polishing, and pressure is 0.08MPa, flow 600mL/min, and polishing time is 130s; Active ingredient in described oxidation solution is the anode Strong oxdiative liquid of electrolyzing gold diamond film gained, and the volume fraction of anode Strong oxdiative liquid in oxidation solution is 15%;
B) again the cleaning fluid that FA/O type chelating agent and nonionic surface active agent AEO are mixed with is passed into polishing machine and carry out polishing again, pressure is 0.08MPa, and flow is 600mL/min, and polishing time is 130s; FA/O type chelating agent shared volume fraction in cleaning fluid is 1.2 ‰, and nonionic surface active agent AEO shared volume fraction in cleaning fluid is 1.8 ‰;
C) finally pass into deionized water and carry out water throwing, pressure is 0.05MPa, and flow is 1000mL/min, time 120s;
D) saphire substrate material cleaned is taken out in polishing machine, in drier, pass into nitrogen dry, dry up.
Embodiment 3
To throw the saphire substrate material surface cleaning method for washing, described surface cleaning method comprises the following steps:
A) saphire substrate material is after polishing process terminates polishing, oxidation solution is passed into polishing machine and carries out second polishing, and pressure is 0.1MPa, flow 700mL/min, and polishing time is 120s; Active ingredient in described oxidation solution is the anode Strong oxdiative liquid of electrolyzing gold diamond film gained, and the volume fraction of anode Strong oxdiative liquid in oxidation solution is 20%;
B) again the cleaning fluid that FA/O type chelating agent and nonionic surface active agent AEO are mixed with is passed into polishing machine and carry out polishing again, pressure is 0.1MPa, and flow is 700mL/min, and polishing time is 120s; FA/O type chelating agent shared volume fraction in cleaning fluid is 1.5 ‰, and nonionic surface active agent AEO shared volume fraction in cleaning fluid is 2 ‰;
C) finally pass into deionized water and carry out water throwing, pressure is 0.06MPa, and flow is 1200mL/min, time 180s;
D) saphire substrate material cleaned is taken out in polishing machine, in drier, pass into nitrogen dry, dry up.
By cleaning method of the present invention, the difficulty of cleaning is reduced, and the Be very effective of cleaning increase; Cleaning fluid composition is gentle, and the surface roughness therefore after cleaning is low, can reach below 0.2nm, occur without corrosion figure; And not containing strong acid and highly basic composition in cleaning fluid, environmental protection, pollution-free, to technical operation personnel also without endangering, cleaning the dirty quantity in rear surface lower than within require in the industry 300, meeting or exceeding and require level in the industry; Cleaning efficiency is higher, can reach more than 98%, has saved scavenging period, also eliminates the use of cleaning equipment, improves suitability for industrialized production ability and reduces production cost.
Claims (6)
1., to throw the saphire substrate material surface cleaning method for washing, it is characterized in that, described surface cleaning method comprises the following steps:
A) saphire substrate material is after polishing process terminates polishing, oxidation solution is passed into polishing machine and carries out second polishing, and pressure is 0.05-0.1MPa, flow 500-700mL/min, and polishing time is 120-150s; Active ingredient in described oxidation solution is the anode Strong oxdiative liquid of electrolyzing gold diamond film gained;
B) again the cleaning fluid that chelating agent becomes with surfactant formulatory is passed into polishing machine and carry out polishing again, pressure is 0.05-0.1MPa, and flow is 500-700mL/min, and polishing time is 120-150s;
C) finally pass into deionized water and carry out water throwing, pressure is 0.04-0.06MPa, and flow is 900-1200mL/min, time 120-180s;
D) saphire substrate material cleaned is taken out in polishing machine, in drier, pass into nitrogen dry, dry up.
2. according to claim 1 a kind of with the saphire substrate material surface cleaning method thrown for washing, it is characterized in that, in step a) oxidation solution used, the volume fraction of the anode Strong oxdiative liquid of electrolyzing gold diamond film gained is 10-20%.
3. according to claim 1 a kind of with the saphire substrate material surface cleaning method thrown for washing, it is characterized in that, in step b), chelating agent shared volume fraction in cleaning fluid is 1-1.5 ‰, surfactant shared volume fraction in cleaning fluid is 1.5-2 ‰, and solvent is deionized water.
4. a kind of to throw the saphire substrate material surface cleaning method washed of generation according to claim 1 or 3, it is characterized in that, surfactant is AEO.
5. a kind of to throw the saphire substrate material surface cleaning method washed of generation according to claim 1 or 3, it is characterized in that, chelating agent is commercially available FA/O type chelating agent.
6. a kind of to throw the saphire substrate material surface cleaning method washed of generation according to claim 1 or 2 or 3, it is characterized in that, deionized water is electronic grade ultrapure water.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104440495B (en) * | 2014-11-03 | 2016-11-16 | 佛山市思特四通化工有限公司 | A kind of quartz polishing coating film production line |
| CN104440496B (en) * | 2014-11-07 | 2017-04-05 | 江苏吉星新材料有限公司 | A kind of cleaning of sapphire wafer |
| CN108857860A (en) * | 2018-06-12 | 2018-11-23 | 宁波江丰电子材料股份有限公司 | Grinding method, wafer orientation ring and its application of wafer orientation ring and chemical mechanical polishing apparatus |
| CN110712119B (en) * | 2019-11-15 | 2021-04-13 | 河北工业大学 | Method for post-cleaning silicon wafer by utilizing CMP (chemical mechanical polishing) equipment |
| CN112404026B (en) * | 2020-09-11 | 2022-03-01 | 上海金堂轻纺新材料科技有限公司 | Process for recycling degreasing wastewater |
| CN114425534B (en) * | 2021-12-13 | 2024-04-16 | 金华博蓝特新材料有限公司 | Method for cleaning sapphire substrate after copper polishing |
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| JP3329593B2 (en) * | 1994-09-28 | 2002-09-30 | 有限会社遠野精器 | Method for manufacturing sapphire dummy wafer |
| CN101892510A (en) * | 2010-07-21 | 2010-11-24 | 河北工业大学 | Cleaning method for removing surface metal impurities on polished silicon substrate material |
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Effective date of registration: 20160119 Address after: 698 No. 330095 Jiangxi city of Nanchang Province, high tech Industrial Development Zone, North Road Patentee after: Zeng Xiqiang Address before: 314300 Salt Road 12, Wuyuan industrial area, Haiyan County, Zhejiang, Jiaxing Patentee before: Zeng Xiqiang |
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Denomination of invention: Method for cleaning surfaces of sapphire substrate materials by using polishing to replace washing Effective date of registration: 20190619 Granted publication date: 20150722 Pledgee: Jiangxi Weijia Creative Development Enterprise Management Co., Ltd. Pledgor: Zeng Xiqiang Registration number: 2019360000018 |
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Effective date of registration: 20200921 Address after: 330000 Room 908, Building A, Madison Square Commercial Office Building, 228 Jinggangshan Avenue, Qingyunpu District, Nanchang City, Jiangxi Province (9th floor) Patentee after: JIANGXI WEIJIA CHUANGZHAN ENTERPRISE MANAGEMENT Co.,Ltd. Address before: 698 No. 330095 Jiangxi city of Nanchang Province, high tech Industrial Development Zone, North Road Patentee before: JIANGXI EAST OCEAN SAPPHIRE OPTOELECTRONICS TECHNOLOGY Co.,Ltd. |